EPA/540/5-89/005a
February 1990
Technology Evaluation Report:
SITE Program Demonstration Test
Soliditech, Inc.
Solidification/Stabilization Process
Volume I
Risk Reduction Engineering Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, OH 45268
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NOTICE
This information in this document has been funded by the U.S. Environmental
Protection Agency under Contract No. 68-03-3484 and the Superfund Innovative
Technology Evaluation (SITE) program. It has been subjected to the Agency's
peer review and administrative review and it has been approved for publication as
a U.S. EPA document. Mention of trade names or commercial products does not
constitute and endorsement or recommendation for use.
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FOREWORD
The Superfund Innovative Technology Evaluation (SITE) Program was authorized in the
1986 Superfund amendments. The program is a joint effort between EPA's Office of Research
and Development (ORD) and Office of Solid Waste and Emergency Response (OSWER). The
purpose of the program is to assist the development of hazardous waste treatment technologies
necessary to implement new cleanup standards which require greater reliance on permanent
remedies. This is accomplished through technology demonstrations which are designed to provide
engineering and cost data on selected technologies.
This project is a field demonstration under the SITE program and designed to analyze the
Soliditech, Inc. solidification/stabilization technology. The technology demonstration took place
at a former oil recycling facility in Morganville, New Jersey. The demonstration effort was
directed at obtaining information on the performance and cost of the technology for assessing its
use at this as well as other uncontrolled hazardous waste sites. Documentation will consist of two
reports: (1) a Technology Evaluation Report that describes the field activities and laboratory
results; and (2) an Applications Analysis Report that provides an interpretation of the data, and
discusses the potential applicability of the technology.
Additional copies of this report may be obtained at no charge from EPA's Center for
Environmental Research Information, 26 West Martin Luther King Drive, Cincinnati, Ohio,
45268, using the EPA document number found on the report's front cover. Once this supply is
exhausted, copies can be purchased from the National Technical Information Service,
Ravensworth Bldg., Springfield, Virginia, 22161, (702) 487-4600. Reference copies will be
available at EPA libraries in their Hazardous Waste Collection. You can also call the SITE
Clearinghouse hotline at 1-800-424-9346 or (202) 382-3000 in Washington, D.C., to inquire about
the availability of otier reports.
E. Timothy Oppelt, Director
Risk Reduction Engineering Laboratory
111
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ABSTRACT
The primary objective of the Soliditech, Inc., solidification/stabilization demonstration
was to develop reliable performance and cost information. The demonstration took place at the
Imperial Oil Company/Champion Chemical Company Superfund site in Morganville, New Jersey.
Contamination at this site includes PCBs, various metals, and oil and grease. The Soliditech
process mixes the waste material with Urrichem, a proprietary reagent; proprietary additives;
pozzolanic materials or cement (cement was used for the demonstration); and water; in an open-
top concrete mixer.
i
The technical criteria used to evaluate the effectiveness of the Soliditech process were
contaminant mobility, based upon leaching and permeability tests; and the structural integrity of
the solidified material, based upon physical and morphological tests.
The treated wastes had significant structural integrity, low permeability, and higher bulk
density than the untreated wastes. pH values of the treated wastes were highly influenced by
alkalinity of the Portland cement added during treatment. Treatment resulted in significantly
reduced concentrations of arsenic, lead and zinc in (1) extracts from TCLP, EP Toxicity, and
BET procedures; and (2) leachates from intact cast cylinders subjected to ANS 16.1 and WILT
procedures. PCBs could not be detected in any extracts or leachates from treated wastes.
IV
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VOLUME I
TABLE OF CONTENTS
Page
NOTICE ii
FOREWORD . iii
ABSTRACT iv
ABBREVIATIONS xii
CONVERSION OF CUSTOMARY UNITS TO METRIC UNITS xiv
ACKNOWLEDGEMENT xv
1.0 EXECUTIVE SUMMARY 1
1.1 INTRODUCTION 1
1.2 PROCESS DESCRIPTION 2
1.3 SAMPLING AND ANALYSIS PROGRAM 3
1.4 FIELD OBSERVATIONS 4
1.5 ANALYTICAL RESULTS . , 4
2.0 INTRODUCTION 8
2.1 BACKGROUND 8
2.1.1 SITE Program 8
2.1.2 Soliditech Technology 9
2.1.3 Site Background . . . 9
2.2 TECHNOLOGY DEMONSTRATION PROGRAM OBJECTIVES 11
2.3 TECHNOLOGY EVALUATION CRITERIA 11
2.4 DESCRIPTION OF OPERATIONS 14
2.5 PROJECT ORGANIZATION . . . 15
3.0 CONCLUSIONS 16
3.1 SUMMARY OF PERFORMANCE DATA . 16
3.2 SUMMARY OF MAJOR PROBLEMS 20
3.3 ADVANTAGES AND LIMITATIONS OF THE SOLIDITECH PROCESS ... 20
3.3.1 Advantages of the Soliditech Process 20
3.3.2 Limitations of the Soliditech Process 27
4.0 SOLIDITECH PROCESS 29
4.1 PROCESS DESCRIPTION 29
4.2 PROCESS SCHEMATIC 29
4.3 EQUIPMENT SPECIFICATIONS 32
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TABLE OF CONTENTS
Section Page
5.0 DEMONSTRATION PROCEDURES 35
5.1 SITE DESCRIPTION 35
5.2 WASTE CHARACTERISTICS 36
5.3 DEMONSTRATION PREPARATION 38
5.4 SAMPLING PROGRAM 38
5.4.1 Waste Material Collection Locations 38
5.4.2 Sampling Schedule 38
5.4.2.1 Pretreatment Sampling Methods and Types . . 43
5.4.2.2 Reagent Mix Sampling Methods and Types . . 50
5.4.2.3 Post-Treatment Sampling Methods and Types 50
5.5 PHYSICAL TESTS 51
5.5.1 On-Site Tests . 51
5.5.2 Laboratory Tests 51
5.6 CHEMICAL TESTS 53
5.7 LEACHING TESTS 59
5.8 QUALITY ASSURANCE AND QUALITY CONTROL SUMMARY 61
6.0 FIELD ACTIVITIES 63
6.1 WASTE MATERIAL COLLECTION 63
6.1.1 Summary of Operations * 63
6.1.2 Deviations from the Demonstration Plan 66
6.2 WASTE TREATMENT 66
6.2.1 Summary of Test Runs 67
6.2.2 Deviations from the Demonstration Plan 69
6.3 SAMPLING FOR PROCESS EVALUATION 70
6.3.1 Pretreatment Sampling Procedures 70
6.3.2 Post-Treatment Sampling Procedures 70
6.3.3 Sampling Deviations 75
7.0 PERFORMANCE DATA AND EVALUATION 76
7.1 PHYSICAL TESTS 76
7.1.1 Bulk Density 76
7.1.2 Water Content 76
7.1.3 Particle Size Distribution 78
VI
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TABLE OF CONTENTS
Section
7.1.4 Permeability . 78
7.1.5 Unconfined Compressive Strength ] 78
7.1.6 Wet/Dry Weathering Test ............... 78
7.1.7 Freeze/Thaw Weathering Test . . 79
7.1.8 Loss on Ignition . 78
7.1.9 On-Site Tests .'.I'.'.'.'.'.'.'.'.'.'.'. 79
7.2 CHEMICAL TESTS . . 79
7-2.1 pH 80
7.2.2 Eh , ;;;; — 1%
7.2.3 Metals . go
7.2.4 Polychlorinated Biphenyls 84
7.2.5 Volatile Organic Compounds . . '.'.'.'.'.'.'.'.'.'.'. 84
7.2.6 Semivolatile Organic Compounds . . . . ! 85
7.2.7 Oil and Grease 86
7.2.8 Acid Neutralization Capacity/Neutralization Potential ............ 86
7.3 LEACHING TESTS ... 86
7.3.1 TCLP 87
7.3.1.1 Reagent Mix 87
7.3.1.2 Filter Cake ' " ' 87
7.3.1.3 Filter Cake/Oily Sludge 89
7.3.1.4 Off-Site Area One '.'.'.'.'.'.'.'.'.'.'.'.'. 90
7.3.2 EP Toxicity . . . 91
7.3.2.1 Reagent Mix 01
7.3.2.2 Filter Cake ' " ' 9}
7.3.2.3 Filter Cake/Oily Sludge 93
7.3.2.4 Off-Site Area One ......'.'.'.'.'.'.'.'.'.'.'. 93
7.3.3 BET 94
7.3.3.1 Reagent Mix 94
7.3.3.2 Filter Cake 94
7.3.3.3 Filter Cake/Oily Sludge 99
7.3.3.4 Off-Site Area One .... 100
7J3.4 ANS 16.1 101
7.3.4.1 Filter Cake . 10i
7.3.4.2 Filter Cake/Oily Sludge 105
7.3.4.3 Off-Site Area One ' ' 105
7.4 MORPHOLOGICAL TESTS n<
7.5 LONG-TERM TESTS '.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'.'. 107
7.5.1 v Waste Interface Leaching Test 107
7.5.2 TCLP and EP Extracts of Solidified Waste '.'.'.'.'.'.'.'.'. 108
VII
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TABLE OF CONTENTS
Section
8.0
7.6
Page
7.5.3 PHYSICAL STABILITY OF TREATED WASTE MONOLITHS 110
7.5.3.1 SURFACE SPALLING 110
7.5.3.2 GRAIN EXFOLIATION Ill
7.5.3.3 CRACK AND FISSURE DEVELOPMENT Ill
7.5.3.4 OXIDATIVE DISCOLORATION Ill
7.5.3.5 SALT EFFLORESCENCE 112
7.5.3.6 PORE CHARACTERIZATION 112
MATERIALS BALANCE 112
COST OF DEMONSTRATION 116
8.1 U.S. EPA SITE CONTRACTOR COSTS 116
8.1.1 Phase I: Planning Stage 116
8.1.2 Phase II: Demonstration Stage 117
8.2 DEVELOPER (SOLIDITECH) COSTS 117
REFERENCES 119
Appendices
A LABORATORY DATA FROM THE TECHNOLOGY DEMONSTRATION
B LABORATORY QA/QC RESULTS
C LABORATORY DATA FROM THE TREATABILITY STUDY
D RESULTS OF FIELD EXPERIMENTS
E PRC TRIP REPORT
F SOLIDITECH DOCUMENTATION OF FIELD REPORTS
G PRELIMINARY WILT RESULTS
vni
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LIST OF TABLES
Table Page
1 PHYSICAL PROPERTIES . . 5
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
CHEMICAL PROPERTIES ........ . 6
. . 21
TCLP AND EP TOXICITY LEACHATE RESULTS FOR FILTER CAKE
WASTE .
TCLP AND EP TOXICITY LEACHATE RESULTS FOR FILTER CAKE/OILY
SLUDGE MIXTURE 22
TCLP AND EP TOXICITY LEACHATE RESULTS FOR OFF-SITE AREA ONE
WASTE
23
BET EXTRACT RESULTS FOR FILTER CAKE WASTE 24
BET EXTRACT FOR FILTER CAKE/OILY SLUDGE MIXTURE 25
BET EXTRACT FOR OFF-SITE AREA ONE WASTE 26
SOLIDITECH TREATMENT FORMULATIONS 30
SAMPLING REQUIREMENTS 39
STANDARD METHODS AND PROCEDURES OF SAMPLE ANALYSIS . 44
DIGESTION AND ANALYTICAL TECHNIQUES
FOR ELEMENTAL ANALYSIS 58
SOLIDITECH DEMONSTRATION CHRONOLOGY 64
CHEMICAL AND PHYSICAL ANALYSES OF UNTREATED AND TREATED
WASTE 77
CHEMICAL ANALYSIS OF SAND 81
CHEMICAL ANALYSIS OF PREDEMONSTRATION BLANK 82
CHEMICAL ANALYSES OF TCLP EXTRACT FROM UNTREATED
AND TREATED WASTE MATERIALS
88
CHEMICAL ANALYSES OF EP EXTRACT FROM UNTREATED AND
TREATED WASTE 92
CHEMICAL ANALYSES OF BET EXTRACT FROM UNTREATED AND
TREATED FILTER CAKE WASTE 95
CHEMICAL ANALYSES OF BET EXTRACT FROM UNTREATED AND
TREATED FILTER CAKE/OILY SLUDGE MIXTURE
96
CHEMICAL ANALYSES OF BET EXTRACT FROM UNTREATED AND
TREATED OFF-SITE AREA ONE WASTE 97
IX
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LIST OF TABLES
Table
22 CHEMICAL ANALYSES OF BET EXTRACT FROM REAGENT MIX
Page
98
23 CHEMICAL ANALYSES OF ANS 16.1 LEACH ATE
FROM TREATED FILTER CAKE WASTE . 102
24 CHEMICAL ANALYSES OF ANS 16.1 LEACH ATE
FROM TREATED FILTER CAKE/OILY SLUDGE MIXTURE 103
25 CHEMICAL ANALYSES OF ANS 16.1 LEACHATE
FROM TREATED OFF-SITE AREA ONE WASTE 104
26 WILT TEST RESULTS THROUGH WEEK 16 109
27 MATERIALS BALANCE 113
28 OBSERVED VOLUME AND WEIGHT OF TREATED MATERIAL 114
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LIST OF FIGURES
Figure Page
1 SITE LOCATION MAP . . . . 10
2 IMPERIAL OIL COMPANY/CHAMPION CHEMICALS SITE
WASTE PILE AND ABANDONED STORAGE TANK 12
3 IMPERIAL OIL COMPANY/CHAMPION CHEMICALS SITE
OFF-SITE AREAS 13
4 SOLIDITECH PROCESS SCHEMATIC . . ... 31
5 WASTE CONTAINED IN 10-CUBIC-YARD SOLIDITECH MIXER ............ 65
6 DISCHARGING OF TREATED WASTE INTO PLYWOOD FORMS 68
7 SAMPLES OF TREATED WASTE IN CYLINDRICAL MOLDS 72
8 LARGE MONOLITHS OF TREATED WASTE BEING PREPARED FOR LONG-
TERM STUDY 73
9 STACKING DIAGRAM OF THE
TREATED WASTE MONOLITHS ; 74
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ABBREVIATIONS
AAS
ANS-16.1
ASA
ASTM
BET
C
CERCLA
CFR
cm
CVAAS
EP
EPA
Eh
F
g
gal
GC/ECD
GC/MS
GFAAS
HDPE
hr
ICP
Kg
kwhr
L
Ib
M
mg
mg/Kg
mg/L
min
mL
mm
mv
N
NC
ND
NJDEP
NPL
ORD
OSWER
PCS
PRC
psi
PVC
QA/QC
RCRA
RI/FS
RPM
RSD
SARA
Atomic Absorption Spectroscopy
Leach test used by the American Nuclear Society
American Society of Agronomy
American Society for Testing and Materials
Batch Extraction Test
Celsius
Comprehensive Environmental Response, Compensation, and
Liability Act
Code of Federal Regulations
centimeter
Cold Vapor Atomic Absorption Spectroscopy
Extraction Procedure Toxicity Test
Environmental Protection Agency
Oxidation/Reduction Potential
Fahrenheit
gram
gallon
Gas Chromatography/Electron Capture Detection
Gas Chromatography/Mass Spectrometer
Graphite Furnace Atomic Absorption Spectroscopy
High-Density Polyethylene
hour
Inductively Coupled Argon Plasma Spectroscopy
Kilogram
kilowatt/hour
liter
pound
Molarity
milligram
milligrams per Kilogram
milligrams per Liter
minute
milliliter
millimeter
millivolts
Normality
Not Calculated
Not Detected
New Jersey Department of Environmental Protection
National Priority List
Office of Research and Development
Office of Solid Waste and Emergency Response
Polychlorinated Biphenyl
Planning Research Corporation Environmental Management, Inc.
pounds per square inch
Polyvinyl Chloride
Quality Assurance/Quality Control
Resource Conservation and Recovery Act
Remedial Investigation and Feasibility Study
Revolutions Per Minute
Relative Standard Deviation
Superfund Amendments and Reauthorization Act
XII
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ABBREVIATIONS (Continued)
sec
SEM
SITE
S/L
svoc
TCLP
TDS
TOC
TMSWC
TSCA
UCS
Mg
WI/L
Aim
fJLmho
voc
WES
WILT
wt
XRD
yd
ZHE
second
Scanning Electron Microscope
Superfund Innovative Technology Evaluation
Solid to Liquid Ratio
Semivolatile Organic Compound
Toxicity Characteristics Leaching Procedure
Total Dissolved Solids
Total Organic Carbon
Test Methods for Solidified Waste Characterization
Toxic Substances Control Act
Unconfined Compressive Strength
micrograms
micrograms per Liter
micrometer
units of conductance
Volatile Organic Compound
Waterways Experiment Station
Waste Interface Leaching Test
weight
X-Ray Diffraction
yard
Zero Headspace Extractor
Xlll
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CONVERSION OF CUSTOMARY UNITS TO METRIC UNITS
Length
Volume
Weight
inches
inches
feet
gallons
cubic yards
pounds
short tons
X
X
X
X
X
X
X
2.54
0.0254
0.3048
3.785
0.7646
0.4536
0.9072
= centimeters
meters
= meters
= liters
cubic meters
= kilograms
= metric tons
Temperature
Note:
5/9
X (° Farenheit - 32)
1000 liters
1000 kilograms
1 cubic meter
1 metric ton
0 Celsius
xiv
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ACKNOWLEDGEMENT
This document was prepared under the direction of Dr. Walter E. Grube, Jr., EPA SITE
program manager in the Risk Reduction Engineering Laboratory of Cincinnati, Ohio.
Contributors and reviewers were Dr. Grube, Robert Soboleski of New Jersey Department of
Environmental Protection, Carl Brassow of Soliditech, Inc., George Kulick, Jr. of the Imperial Oil
Company, Paul dePercin, Guy Simes and Steve James of U.S. EPA Risk Reduction Engineering
Laboratory, John Kingscott and John Quander of U.S EPA Office of Solid Waste and Emergency
Response, Mark Bricka and G. Sam Wong of U.S. Army Corps of Engineers Waterways
Experiment Station, Peter Hannak of Canviro Consultants, and Dr. Paul Bishop of University of
Cincinnati.
This report was prepared for the EPA's Superfund Innovative Technology Evaluation
(SITE) Program by Dr. Kenneth Partymiller, Sarah V. Woodland, and Neil F. Morton of PRC
Environmental Management, Inc., and Dr. Danny Jackson and Debra Bisson of Radian
Corporation under Contract No. 68-03-3484. Sampling and analysis activities were conducted by
Radian Corporation.
xv
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1.0 EXECUTIVE SUMMARY
1.1
INTRODUCTION
In response to the Superfund Amendments and Reauthorization Act of 1986 (SARA), U.S.
EPA has established a formal program to accelerate the development, demonstration, and use of
new or innovative technologies that offer permanent, long-term cleanup solutions at Superfund
sites. This program is called the Superfund Innovative Technology Evaluation or SITE program,
and is administered by the Office of Solid Waste and Emergency Response (OSWER) and the
Office of Research and Development (ORD).
The SITE program has four primary goals:
• To identify and remove impediments to the development and commercial use of
alternate technologies.
• To conduct a demonstration of the more promising innovative technologies to
establish reliable performance and cost information for site characterization and
cleanup decision making.
• To develop procedures and policies that encourage the selection of available
alternative treatment remedies at Superfund sites as well as other waste sites and
commercial facilities.
• To structure a development program that nurtures emerging technologies.
In January 1987, U.S. EPA solicited proposals from approximately 400 developers of
innovative waste treatment technologies who had expressed an interest in becoming involved in
the SITE program. U.S. EPA received 29 proposals by the March 13, 1987 due date. In
September 1987, EPA selected 10 technologies for inclusion in the SITE demonstration program
(002). One of these was the solidification/stabilization process developed by Soliditech, Inc., of
Houston, Texas.
The Imperial Oil Company/Champion Chemical Company Superfund site in Morganville,
New Jersey was chosen for the Soliditech demonstration. The chemicals of concern at this site
include metals such as arsenic, beryllium, cadmium, chromium, copper, lead, mercury, nickel,
selenium, thallium, and zinc; and various organic chemicals including polychlorinated biphenyls
(PCBs) and petroleum hydrocarbons. Contamination is present in the soil, in a waste filter cake
pile, and in an abandoned storage tank, as well as in the ground water. Samples of contaminated
material from the soil, the waste filter cake pile, and the abandoned storage tank were treated
during the demonstration.
1
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The four major objectives identified for the Soliditech SITE demonstration were to:
• Determine the effectiveness of the technology to solidify and stabilize waste
materials found at the site.
• Determine whether the solidified material maintains its structural properties and
stabilization effectiveness over a five-year period.
• Determine the volume and mass change of the solidified material due to addition
of pozzolans, water, reagent, and other proprietary additives.
Develop reliable capital and operating costs for the technology that can be used in
the Superfund decision-making process.
To meet these objectives, a SITE Demonstration Plan was prepared (PRC, 1988b). This
plan detailed all sampling and analysis to be performed during the Soliditech demonstration.
Analytical tests were performed on samples of untreated as well as solidified waste material
collected during the demonstration. The results will be used to evaluate the effectiveness of the
treatment process and the structural properties of the resulting solidified material. Soliditech
personnel maintained operating logs to determine the capital and operating expenses associated
with the demonstration. Soliditech and U.S. EPA personnel maintained field logs of the volume
and weight of all ingredients for each test run, as well as the volume and weight of all treated
material. These data are presented in this report and have been analyzed in view of the above
objectives.
1.2
PROCESS DESCRIPTION
Soliditech, Inc. claims that its solidification/stabilization process chemically and physically
immobilizes hazardous constituents in waste material. This immobilization occurs by one or more
of the following processes: encapsulation, adsorption, and incorporation into the crystalline
structure of the solidified material. The Soliditech process uses a proprietary reagent (Urrichem);
proprietary additives; pozzolans (such as fly ash), kiln dust, or cement; and water to solidify
solids and sludge containing organic and inorganic chemicals typically found at hazardous waste
sites.
The chemical reagent and proprietary additives are mixed in a batch process with the
waste material, water, and the pozzolanic materials to solidify the waste materials by chemical
and physical processes. Once thoroughly mixed, the treated waste is discharged from the mixer
and allowed to cure. The final product is claimed to be a monolithic material with measurable
structural strength and significantly reduced leaching potential.
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During the demonstration, waste materials from three site locations were collected,
screened, mixed, and treated by the Soliditech process. In addition, clean sand was treated as a
control. The treated material was placed in small, cylindrical molds for chemical and physical
testing, and in large 1-cubic yard plywood forms for long-term monitoring, and allowed to cure
for 28 days. After curing, the small cast sample cylinders were shipped to the analytical
laboratories where they were analyzed. After the plywood sides of the large forms were
removed, the resulting treated waste monoliths were placed in an enclosed on-site storage area for
long-term monitoring.
1.3
SAMPLING AND ANALYSIS PROGRAM
Samples of waste material from four areas of the site were collected six months prior to
the demonstration (PRG, 1988a). A portion of this material was supplied to Soliditech for testing
to determine the suitability of the waste for treatment. Both raw and treated samples of the
waste material were chemically analyzed to determine levels of contamination in the four areas,
to assess the effectiveness of the Soliditech bench scale tests, and to allow the analytical
laboratory to assess possible analytical problems. Additionally, Toxicity Characteristics Leaching
Procedure (TCLP) tests were performed on the samples of raw and treated waste material and the
leachate was chemically analyzed (Radian, 1988). Three areas containing three distinct waste
types were chosen for treatment during the full-scale field demonstration.
During the SITE demonstration, pretreatment waste samples were collected for each test
parameter from each of the three waste materials to be treated. These samples were analyzed for
chemical constituents, physical characteristics, and ability to withstand leaching/extraction using
both destructive and nondestructive techniques. The results allow a direct comparison of physical
and chemical properties between the treated and untreated waste, and help determine the
effectiveness of the treatment process.
A control run was performed to determine whether the Soliditech proprietary reagent and
proprietary additives were contributing contamination to treated waste samples, and to set
baseline values for some of the physical properties. Samples from the control run are referred to
reagent mix samples. Clean sand was used as a surrogate waste material in the control run.
These samples were analyzed for chemical constituents and physical characteristics.
Treated waste samples were collected immediately after each of the three waste treatment
test runs and analyzed for chemical constituents, physical characteristics, and ability to withstand
leaching/extraction. Samples for long-term testing were also collected. The long-term study
includes a twelve-month, nondestructive leaching experiment, leaching by other leaching
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procedures at various times up to five years after treatment, and petrographic analysis and
observation. These tests will help to assess the long-term stability of the treated material.
1.4
FIELD OBSERVATIONS
Several significant observations were made during the demonstration. These are
summarized below.
A small amount of contaminated waste material was treated during the demonstration.
For this small amount of material, mobilization and demobilization times were found to be
disproportionately long. Additionally, special pre- and post-treatment procedures were followed
to meet the demonstration objectives. During the remediation of a hazardous waste site, the time
expended performing these activities would be insignificant compared to the actual waste
treatment activities.
Measuring the exact weight or volume of wastes that were treated was difficult. This
problem was largely due to the inability to accurately determine the weights of all ingredients.
This should not be a problem in the field, when numerous batches and similar wastes are treated.
The adequacy of mixing of each batch of waste material was determined by the Soliditech
operator, apparently based upon past experience rather than an objective standard. After curing,
the solidified waste was observed to contain small amounts of unmixed material. Skilled
operators or an objective standard are necessary to determine when waste is adequately mixed.
1.5
ANALYTICAL RESULTS
The analyses of the samples collected before, during, and after the Soliditech
demonstration are summarized in Tables 1 and 2. The results are discussed below.
Pretreatment waste from the site consisted of contaminated soil, filter cake, and filter
cake/oily sludge. These wastes contained 2.8 to 17 percent oil and grease with relatively low
levels of other organic compounds. PCB (Aroclors 1242 and 1260) concentrations ranged from 28
to 43 mg/Kg in the pretreatment wastes. Lead concentrations ranged from 650 to 2500 mg/Kg in
the pretreatment wastes.
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Filter Cake
TABLE 1
PHYSICAL PROPERTIES
Filter Cake/Oily
Sludge Mixture
Off-Site Area One
Untreated
Bulk Density 1.14
(g/cm3)
Permeability NA(M
(cm/sec)
Unconfined
Compressive NA
Strength
(psi)
Loss on
Ignition 54
Treated(a) Untreated Treated(a) Untreated Treated(a)
1.43 1.19 1.68 1.26 1.59
4.53 x 10'7 NA 8.93 x 10'9 NA 3.41 x 10'8
390 NA 860 NA 680
41 70 34 36 34
Water Content 28.7
21.0
58.1
14.7
23.5
12.6
Notes:
Treated waste sampled after a 28-day curing period.
NA = Not analyzed.
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TABLE 2
CHEMICAL PROPERTIES
o\
Filler Cake
Leachate Leachale
from from
Chemical Untreated Treated Untreated Treated
Parameter*8* Waste Wasle ND 36 28 16 ND ND
Oil and Grease 170,000 77,000 1.4 . 4.4
Arsenic 26 28 0.005 ND
I*ad 2,200 680 4.3 0.002
Zinc 26 23 0.28 ND
Notes:
8 Analyte concentration units for the untreated and treated waste
b Treated wastes were sampled after a 28-day curing period.
c Leachate values refer to results from TCLP test.
d VOCs = volatile organic compounds.
e ND = not detected.
* These values contain low levels of acetone, melhylene chloride,
' SVOCs = semivolatile organic compounds.
h PCBs = polychlorinated biphenyls.
Filter Cake/Oilv Sludee Mixture Off-Sile Area One
Leachate Leachate Leachate Leachate
from from from from
Untreated Treated Untreated Treated Untreated Treated Untreated Treated
Waste Waste^ Wasle(c) Waste 17
43 15 ND ND 43 40 ND ND
130,000 60,000 1.6 2.4 28,000 46,000 1.9 12
14 40 0.014 ND 94 92 0.19 ND
2,500 850 5.4 0.014 650 480 0.55 0.012
150 54 1.3 ND 120 95 0.63 ND '
are mg/Kg. Analyte concentration units for the leachate from untreated and treated waste are mg/L.
various phthalates, or other analytes which are commonly attributed to sampling or analytical contamination.
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The Soliditech solidification/stabilization process produced solidified waste with
significant structural stability (UCS values ranging from 390 to 860 psi) and low permeability
(10~9 to 10"7 cm/sec). Because of the cement in the Soliditech process, pH values of the
solidified wastes ranged from 11.8 to 12.0. Lead concentrations ranged from 480 to 850 mg/Kg
in the post-treatment wastes. PCB (Aroclors 1242 and 1260) concentrations ranged from
approximately 15 to 41 mg/Kg in the post-treatment wastes. Oil and grease concentrations in the
treated wastes ranged from 4.6 to 7.7 mg/Kg. Low concentrations of phenol (12 and 4.8 mg/Kg)
and p-cresol (14 and 4.4 mg/Kg) were found in solidified filter cake and filter cake/oily waste
samples.
The reagent mixture contained 20 mg/Kg of lead. PCBs, phenols, oil and grease, and
cresols were not detected in the reagent mixture. The Soliditech reagent mix could not be
reliably analyzed for phenol, p-cresol, and o-cresol because of its high alkalinity.
Leaching/extraction tests were performed using both destructive methods (TCLP, EP
Toxicity, and BET) and non-destructive methods (ANS 16.1 and WILT). Destructive methods
crush or grind the samples prior to testing destroying the physical integrity of solidified waste
samples. Non-destructive methods were applied to intact cast cylinders.
Arsenic, lead, and zinc were found in EP, TCLP, and BET leachates from the
pretreatment wastes. TCLP leachate from the pretreatment filter cake waste contained 4.3 mg/L
of lead. These metals were not detected in post-treatment waste leachates produced by the EP,
TCLP, and BET. The high alkalinity of the waste solidified by the Soliditech process neutralized
the acidity of the EP and TCLP procedures. Pretreatment wastes could not be tested by ANS
16.1. Metals were not detected in post-treatment waste leachates produced by the ANS 16.1
method.
The post-treatment TCLP leachates contained phenol (100 to 630 Mg/L), p-cresol (110 to
440 Mg/L), and o-cresol (13 to 88 Mg/L). These compounds were either not found or were found
in lower concentrations in the pre-treatment waste samples.
Oil and grease were generally detected at similar concentrations (ND to 12 mg/L) in the
EP, TCLP and BET leachates of both pretreatment and post-treatment wastes.
Results from the first 16 weeks of leaching by the Waste Interface Leaching Test (WILT)
indicate that potentially toxic metals and organic compounds released by the solidified wastes
were below levels of concern.
-------
2.0 INTRODUCTION
This section provides background information about the Superfund Innovative Technology
Evaluation (SITE) program, the Soliditech, Inc., solidification/stabilization technology, and the
location of the demonstration. It also presents the demonstration program objectives, the
technology evaluation criteria, a description of the field operations, and the project organization.
2.1
BACKGROUND
Past hazardous waste disposal practices and the environmental and human health impacts
of those practices caused Congress to enact the Comprehensive Environmental Response,
Compensation, and Liability Act (CERCLA) of 1980. The original act established a Hazardous
Substance Response Trust Fund to deal with costs incurred in cleanups of hazardous materials;
this fund has become known as the Superfund. U.S. EPA has proceeded to investigate potentially
dangerous hazardous waste sites and to establish national priorities for site cleanups. The
ultimate objective of these investigations is to develop plans for permanent, long-term site
cleanups. The list of potential cleanup sites is known as the National Priorities List (NPL).
Congress expressed concern over the use of land-based disposal and containment
technologies to mitigate problems caused by releases of hazardous substances at hazardous waste
sites. In response to this concern, the 1986 reauthorization of CERCLA, called the Superfund
Amendments and Reauthorization Act of 1986 (SARA), mandates that, to the maximum extent
practicable, U.S. EPA select remedial actions at Superfund sites that create permanent solutions to
effects on human health or the environment. In doing so, U.S. EPA is directed to make use of
innovative, alternative, or resource recovery technologies.
2.1.1
SITE Program
U.S. EPA has established the SITE program to accelerate the development, demonstration,
and use of new or innovative technologies that offer permanent site cleanup. The program is
administered by the Office of Solid Waste and Emergency Response (OSWER) and the Office of
Research and Development (ORD).
Each year U.S. EPA solicits proposals to demonstrate innovative technologies. The most
promising technologies are chosen for participation in the SITE demonstration program. OSWER,
ORD and U.S. EPA regional personnel match these technologies with a list of potentially
appropriate sites.
-------
The demonstration program is designed to develop detailed and reliable performance and
cost data on the innovative alternative technologies, so that potential users have sufficient
information to make sound judgments as to the applicability of the technology to a specific site
and to compare it to other currently available technology alternatives.
The program also identifies the governmental policy and regulatory requirements
applicable to the technology and the hazardous substances being treated or destroyed.
2.1.2
Soliditech Technology
The Soliditech, Inc. solidification/stabilization technology mixes a proprietary reagent,
called Urrichem, with a pozzolanic materials (such as fly ash), or cement, and other proprietary
additives to solidify solids and sludges containing the organic and inorganic chemicals found at
uncontrolled hazardous waste sites (Soliditech, 1987). The Soliditech process claims to chemically
and physically immobilize hazardous constituents in waste material. This immobilization occurs
by one or more of the following processes: encapsulation, adsorption, and incorporation into the
crystalline structure of the solidified material. The final product is claimed to be a monolithic
material with measurable structural strength and significantly reduced leaching potential.
The Soliditech technology was developed in the early 1980s and has been used mainly to
treat industrial sludge. Typical Soliditech projects to date include the bench-scale testing and
treatment of liquid, semi-liquid, and solid waste_.materials.
A more detailed process description is provided in Section 4.
2.1.3
Site Background
The site selected for the Soliditech, Inc., demonstration was the Imperial Oil Company,
Inc./Champion Chemical Company site in Morganville, New Jersey. The location of the site is
shown in Figure 1. This site is on the National Priority List (NPL) of Superfund clean-up sites.
In the past, facilities located on the site processed tomatoes, produced various chemicals, and
recovered waste oil. Present facilities blend and package oils for sale. The site includes a waste
pile containing oil-saturated waste filter cake material, an abandoned storage tank containing oily
-------
FIGURE 1
SITE LOCATION MAP
Source: E. C. Jordan Co., 1987.
10
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sludge, several locations where oily sludge and/or waste filter cake material appear to have either
been deposited or to have migrated, and other areas of surface and subsurface contamination.
The locations of these areas are shown in Figures 2 and 3. (Although Off-Site Areas One and
Two are referred to as "off-site," they are actually within the boundaries of the Superfund-
designated site.)
Based upon past studies, including a treatability and site screening study, chemicals of
concern at this site include petroleum hydrocarbons, other organic chemicals including PCBs, and
metals (E.G. Jordan Co., 1987 and Radian, 1988).
2.2
TECHNOLOGY DEMONSTRATION PROGRAM OBJECTIVES
The SITE program mandate is to seek cost-effective alternatives to the traditional practice
of using land disposal and containment for the remediation of hazardous waste sites. To address
this mandate, the following objectives were developed for the Soliditech SITE demonstration:
Determine the effectiveness of the technology to solidify and stabilize
waste materials found at the site.
Determine whether the solidified material maintains its structural
properties and stabilization effectiveness over a five-year period.
• Determine the volume and mass change of the waste material after
treatment with the pozzolan, reagent, and additive mix.
Develop reliable capital and operating costs for the technology that can be
used in the Superfund decision-making process.
2.3
TECHNOLOGY EVALUATION CRITERIA
A Demonstration Plan was prepared prior to the Soliditech SITE demonstration (PRC,
1988b). This plan contained a Sampling and Analysis Plan designed to address the demonstration
objectives. The Demonstration Plan outlined the following criteria.
A primary criterion for evaluating the effectiveness of the Soliditech process is the
reduction of leachable contaminants, measured by comparing the concentrations of leachable
constituents in the untreated waste materials to those in the treated waste materials. Several
laboratory leaching tests were applied to the analysis of the untreated and treated materials. Each
test attempted to simulate a different set of environmental conditions.
11
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FIGURE 2
IMPERIAL OIL COMPANY/CHAMPION CHEMICALS SITE
WASTE PILE AND ABANDONED STORAGE TANK
/
L_
I /
ABANDONED STORAGE TANK
PRIVATE HOMES
o
Source: Modified from E.G. Jordan, 1987.
12
-------
FIGURE 3
IMPERIAL OIL COMPANY/CHAMPION CHEMICALS SITE
OFF-SITE AREAS
SUSPECTED
WASTE OIL DUMP AREAS
OFF-SITE -
AREA NO. 1
IMPERIAL
OB. COMPANY
Source: Modified from E.G. Jordan, 1987.
13
-------
Another criterion for determining the effectiveness of the Soliditech process is the
physical properties of the solidified material, such as unconfined compressive strength,
permeability, microstructural changes, wet/dry durability, and freeze/thaw durability. These
tests produce information about the long-term potential for water to permeate through a
stabilized waste and about the structural integrity of a stabilized solid. Leaching tests and field
observations of the solidified masses will be made over a five-year period to assess the durability
of the solidified material.
The demonstration generated records of the weight and volume of both raw and treated
waste. This information was used to determine the volume and weight change of the treated
waste.
Costs and the capital expenditures for the Soliditech demonstration were generated and
can be compared to the costs for treatment by other technologies.
A more detailed description of the analytical testing is provided in Section 5.
2.4
DESCRIPTION OF OPERATIONS
Contaminated soil, filter cake, and oily sludge wastes from three areas of the Imperial Oil
Company/Champion Chemical Company site were used for the demonstration test. These wastes
were sampled immediately prior to treatment. The contaminated soil was excavated from an area
approximately 5 feet wide by 8 feet long by 3 feet deep at Off-Site Area One. The waste filter
cake was collected from the open face of the waste pile. The oily sludge was scooped from the
abandoned storage tank with a bucket. The contaminated soil and waste filter cake materials
were both screened to prevent large objects such as rocks, roots, bricks, or other debris from
being incorporated in the process runs. While most large debris would not have affected the
Soliditech process, it could have interfered with the analytical testing and was removed.
The water and Urrichem, were pumped into the mixer and metered to determine their
volume. The other proprietary additives were weighed before they were added to the mixer.
The sludge and contaminated soil were also weighed before they were added to the mixing unit.
The weight of filter cake and cement added to the mixer was estimated from the volume of the
front end loader bucket. The volume of the front end loader bucket was calibrated with weighed
amounts (55-gallon drums) of filter cake and cement. After the components were determined by
Soliditech personnel to be mixed and the treatment was completed, the slurry was discharged
from the mixer into one-cubic-yard plywood forms. Small waxed cardboard and PVC cylindrical
14
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forms were filled from the slurry in the large plywood forms. After curing and transport to the
analytical laboratory, these small forms were removed and the resulting cylindrical samples were
used for analytical testing.
2.5
PROJECT ORGANIZATION
For the SITE program demonstration a cooperative agreement was signed between ILS.
EPA and Soliditech, Inc. Soliditech was responsible for operating its equipment and providing
the chemical additives. U.S. EPA, through its contractor, prepared the Demonstration Plan,
performed the test site preparation, performed the sampling and analyses, evaluated the data, and
prepared the Technology Evaluation Report. The field operations at the Imperial Oil
Company/Champion Chemical Company site were performed by a U.S. EPA contractor.
15
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3.0 CONCLUSIONS
Approximately 350 samples were collected during the Soliditech SITE demonstration. The
data generated from the analyses of these samples as well as cost data were used to evaluate the
Soliditech technology. The evaluation procedures used are standardized analytical methods
prepared by the U.S. Environmental Protection Agency (U.S. EPA), American Society of Testing
and Materials, and American Society of Agronomy. The analytical methods, as prescribed in the
Demonstration Plan (PRC, 1988b), were peer-reviewed and approved by U.S. EPA.
3.1
SUMMARY OF PERFORMANCE DATA
Three waste materials — contaminated soil, filter cake, and a mixture of filter cake and
oily sludge ~ were treated by the Soliditech solidification/stabilization process. These materials
contained metals, volatile and semivolatile organic compounds, and PCBs.
Waste samples were analyzed prior to and after treatment to determine their physical and
chemical characteristics. These data are reported in Sections 7.1 — Physical Tests, and 7.2 —
Chemical Tests. The reagent mix used in the Soliditech process was analyzed to ensure that
contaminants were not added to the wastes. Post-treatment samples were analyzed to determine
the extent of stabilization of the wastes, in terms of physical and chemical characteristics. These
data are reported in Sections 7.3 — Leaching Tests, and 7.4 — Morphological Tests. These
analyses consisted of both total waste analyses and chemical analyses of leachates generated from
both the untreated and treated wastes. Leaching/extraction tests were performed using both
destructive methods (TCLP, EP Toxicity, and BET) and non-destructive methods (ANS 16.1 and
WILT). Destructive methods crush or grind the samples prior to testing destroying the physical
integrity of the solidified waste samples. Non-destructive methods were applied to intact cast
cylinders. In addition, long-term testing is being conducted to evaluate the effectiveness of the
solidification/stabilization technology over a period of five years. This section presents a
summary of the results.
1. For the pretreatment filter cake/oily sludge samples, concentrations of volatile organic
compounds (VOCs) ranged from 1.6 to 32 mg/Kg. For the pretreatment Off-Site Area
One samples, concentrations of VOCs ranged from 2.2 to 8.3 mg/Kg. VOCs were not
detected in the pretreatment filter cake samples or in the post-treatment waste samples.
2. Semivolatile organic compound (SVOC) analyses detected o-cresol in one of three
replicate pretreatment filter cake/oily sludge samples. Post-treatment samples of the
16
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filter cake/oily sludge and filter cake contained phenol (4.8 and 12 mg/Kg), p-cresol (4.4
and 14 mg/Kg), and 2,4-dimethylphenol (3.7 mg/Kg and ND). 2-Methylnaphthalene was
detected in the filter cake/oily sludge and Off-Site Area One samples (4.4 and 3.8
m8/K.g). SVOCs were not detected in the reagent mix samples.
3. Metals were detected in pretreatment, reagent mix, and post-treatment samples. Levels of
metals in the post-treatment waste were generally lower than those detected in the
pretreatment waste.
4. Aroclor 1242 and Aroclor 1260 (PCBs) were detected in both the pretreatment and post-
treatment wastes at levels ranging from 28 to 43 and 15 to 40 mg/Kg, respectively. PCBs
were not detected in the reagent mix samples.
5. The pH of the pretreatment Off-Site Area One waste was 7.9. The filter cake and the
filter cake/oily sludge wastes both had a pH of about 3.5. The post-treatment wastes and
the reagent mix samples had pH values of about 12, which was attributed to the alkalinity
associated with the cement in the solidification/stabilization mix.
6. The Eh (oxidation/reduction potential) of a water extract of the pretreatment wastes
ranged from 100 millivolts (mv) to 370 mv. The Eh of a water extract at the post-
treatment waste arid reagent mix samples ranged from -31 to,-63 mv.
7. The loss on ignition (a measure of water and organic content lost through volatilization)
for the pretreatment waste samples ranged from 36 percent to 70 percent, and from 34
percent to 41 percent for the post-treatment waste samples.
8. The oil and grease content of the pretreatment waste samples ranged from about 2.8
percent to 17 percent. The post-treatment samples ranged from 4.6 percent to 7.7
percent.
9. TCLP Extraction Tests - PCBs were not detected in TCLP extracts of the pretreatment or
post-treatment samples. Oil and grease was detected in both the pre- and post-treatment
samples at concentrations of 1.4 to 12 Mg/L. Lead and arsenic were found at levels as
high as 5.4 mg/L and 0.19 mg/L, respectively, in the pretreatment samples. These metals
were either not detected or were detected at lower levels in the post-treatment samples
(see Tables 3 through 5). Barium, calcium, and sodium levels increased in the post-
treatment samples due to the cement and proprietary additives used during treatment.
17
-------
VOCs were detected at low levels in the reagent mix samples but were not detected in the
post-treatment samples. Toluene (55 and 270 Mg/L) and total xylenes (57 and 26 Mg/L)
were found in the pretreatment filter cake/oily sludge and Off-Site Area One TCLP
leachates. Acetone was detected in all pretreatment wastes, but was also present in
laboratory control blanks. SVOCs were not detected in the reagent mix samples (only
post-treatment samples analyzed) or the filter cake pretreatment samples. In the
pretreatment filter cake/oily sludge and Off-Site Area One samples, SVOCs (o-cresol, p-
cresol, 2,4-dimethylphenol, phenol, and benzyl alcohol) were present at concentrations of
10 to 200 M8/L. The post- treatment samples from all areas contained higher levels of
these compounds, ranging from 1 3 to 630 M8/L. The sources of these compounds are not
known. The pH ranged from 4.6 to 5.1 for the pretreatment samples and from 10.8 to
11.6 for the post- treatment samples. These results indicate that alkalinity added by the
Soliditech process greatly exceeded the acidic capacity of the TCLP. Table 17 in Section
7 present these results.
10. EP Toxicity Tests - PCBs were not detected in EP extracts of the pre- or post- treatment
samples. Oil and grease was not found in the pretreatment samples except for the Off-
Site Area One at 2.6 mg/L. Lead and zinc were detected at levels less than 1 mg/L in the
pretreatment samples. These metals were not detected in the post- treatment samples.
Barium, calcium, and sodium levels increased in the post-treatment samples. The pH
ranged from 3.8 to 4.8 for the pretreatment samples and from 10.9 to 11.8 for the post-
treatment samples. Table 18 in Section 7 present these results.
11. BET Extraction Tests - PCBs were not detected in BET extracts of the pretreatment or
post-treatment samples. The pH for the filter cake and filter cake/oily sludge
pretreatment samples ranged from 3.5 to 4.4; the pH for Off-Site Area One ranged from
8.3 to 9.0. Oil and grease ranged from less than 0.4 mg/L to 16 mg/L for the
pretreatment BET samples. Post-treatment oil and grease levels ranged from less than 0.4
mg/L to 26 mg/L. The concentration of metals detected in the pretreatment and post-
treatment BET samples increased as the solid to liquid ratio of the extract decreased.
Lead and zinc were not detected in any of the post- treatment samples. Tables 19 to 22 in
Section 7 present these results.
12. ANS 16.1 Leaching Tests - This non-destructive leaching test could only be performed on
treated waste samples. PCBs were not detected in the leachates. Oil and grease was not
detected in the filter cake and filter cake/oily sludge samples, but was detected in the
Off-Site Area One sample at 1.1 mg/L to 3.2 mg/L. Lead and zinc were found at the
18
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detection limits in some of the samples, and arsenic was detected at 0.0053 to 0.0080
mg/L in the Off-Site Area One samples. The pH of leachates ranged from 10.7 to 11.7.
Tables 23 through 25 in Section 7 present these results.
13. Morphological features will be determined through radiographic X-ray diffraction and
scanning electron microscope (SEM) analyses. There are no results to report at this time.
14. Physical Tests - The bulk density of the pretreatment wastes ranged from 1.14 to 1.26
g/cm3. The bulk density of the post-treatment wastes ranged from 1.43 to 1.68 g/cm3.
The moisture content in the pretreatment samples ranged from 23.5 to 58.1 percent, and
from 12.6 to 21.0 percent in the post-treatment samples.
The mean particle size for the pretreatment wastes ranged from 0.32 to 0.46 mm. Particle
size on the post-treatment wastes was not determined because the wastes were monolithic
solids.
15.
Permeability of the pretreatment waste was not determined. Permeability of the post-
treatment waste ranged from 8.9 x 10"9 cm/sec to 4.5 x 10"7 cm/sec for the filter
cake/oily sludge and filter cake samples, respectively.
The unconfined compressive strengths ranged from 390 psi for treated filter cake to 860
psi for treated filter cake/oily sludge.
Results of the wet/dry weathering tests for all of the post-treatment wastes indicate no
measurable weight loss from the 12 wet/dry cycles.
No weight loss greater than one percent occurred in the post-treatment cores as a result of
the 12 freeze/thaw cycles.
The acid neutralization capacity of the pretreatment waste was low in all cases. However,
adding the solidifying proprietary additives increased the alkalinity of the treated wastes
to extremely high levels.
Results from the first 16 weeks of leaching by the WILT procedure indicate that
potentially toxic metals and organic compounds released from the solidified wastes were
below levels of concern. Measurable concentrations of major cations and oil and grease
19
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were found in leachates. The pH of leachates ranged from 10.9 to 12.7. These
preliminary data are presented in Appendix G.
Tables 1 and 2 summarize the physical and chemical properties of the untreated and
treated wastes. Tables 3 through 8 summarize the percent changes in TCLP, EP, BET, and ANS
16.1 leachate concentrations due to solidification/stabilization for various analytes of concern.
The percent/reduction (or increase) values have been corrected to account for the dilution of
wastes by adding cement, water, Urrichem, and proprietary additives.
In summary, data from all extraction and leaching tests showed negligible release of
contaminants. Neither PCBs nor volatile organic compounds were detected in the TCLP extracts
of treated wastes. Significantly reduced amounts of metals were detected in the TCLP, EP, BET,
and ANS 16.1 extracts of treated wastes compared to untreated wastes. However, Portland
cement contributed several metals to the treated waste. Low concentrations of phenols and
cresols were detected in post-treatment TCLP extracts. These compounds were possibly formed
during the stabilization reactions. The pH values of the treated wastes were near 12.
Physical stability of the treated wastes was high. Unconfined compressive strength of the
treated waste was significant. Permeability values for the treated waste.s were very low. Weight
loss of the treated wastes after wet/dry and freeze/thaw cycles was negligible.
3.2
SUMMARY OF MAJOR PROBLEMS
No major operational problems were encountered during the Soliditech demonstration.
Various minor problems that did occur are discussed in the appropriate sections of this
Technology Evaluation Report.
3.3
ADVANTAGES AND LIMITATIONS OF THE SOLIDITECH PROCESS
The advantages and limitations of the solidification/stabilization process are summarized
below.
3.3.1
Advantages of the Soliditech Process
The equipment required for the process is relatively simple and easily transported
on two flatbed truck trailers. A dry solids storage hopper and a mixer are the two
major pieces of equipment. The minimal electrical power requirements for
transfer of pozzolans from the hopper to the mixer can be met by a small,
20
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TABLE 3
TCLP AND EP TOXICITY LEACHATE RESULTS FOR FILTER CAKE WASTE
PCBs (/ig/L)
Aroclor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Lead
Metals (ICPES) (mg/L)
Barium
Cadmium
Lead
Nickel
Zinc
Other Chemical Analyses
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
Notes
Untreated
<0.42
<0.84
0.0050
NA
1.4
0.0052
4.3
<0.020
0.28
4,500
1.4
TCLP
Treated
<0.45
<0.90
<0.0020
0.0020
1.3
<0.0050
<0.20
<0.020
<0.020
8,500
4.4
EP Toxicitv
Percent
Reduction
(Increase)""*0
ND
ND
ND
ND
(57)
ND
>92
ND
>88
(220)
(430)
* Percent reduction (increase) was calculated after correcting for dilution due to treatment.
and 41 percent additives by weight.
Equation: Percent Reduction (Increase} = Analvte
Concentration
Untreated
<0.43
<0.86
0.010
0.26
0.21
<0.0050
0.25
<0.020
0.032
90
<0.40
The treated filter
Treated
<0.41
<0.82
0.0023
0.0023
1.4
< 0.0050
<0.050
<0.020
<0.020
9,500
4.0
cake waste was
/ Analvte Concentration Treated V
Untreated - ' Dilution Ratio 1
Percent
Reduction
rincreaseV)(b)
ND
ND
61
99
(1,000)
ND
>66
ND
ND
(18,000)
(> 1,600)
59 percent waste
x 100%
Analyte Concentration Untreated
An increase in metal and TDS concentrations may be due to presence of metals and other inorganics in the reagent mixture.
NA = Not analyzed
ND = Not possible to determine
> = Greater than
< = Less than
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TABLE4
TCLP AND EP TOXICITY LEACHATE RESULTS FOR FILTER CAKE/OILY SLUDGE MIXTURE
EP Toxicilv
PCBs (/ig/L)
Aroclor-1242 '
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Lead
Metals (ICPES) (mg/L)
Barium
Cadmium
Lead
Nickel
Zinc
Other Chemical & Physical Tests
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
Percent reduction (increase) was calculated after correcting for dilution due to treatment. The treated filter cake/oily sludge waste was 40
percent waste and 60 percent additives by weight.
Untreated
<0.43
<0.86
0.014
NA
2.5
0.0093
5.4
0.027
1.3
5,200
1.6
i v^ur
Treated
<0.21
< 0.0020
0.014
5.1
< 0.0050
<0.050
<0.020
<0.020
8,600
2.4
Percent
Reduction
(Increase^1""'
ND
ND
>64
ND
(410)
ND
>98
ND
>96
(310)
(270)
Untreated
<0.43
<0.86
0.011
0.55
1.1
0.0082
0.52
<0.020
0.86
330
<0.40
Treated
<0.42
<0.84
0.0020
0.015
5.7
<0.0050
<0.050
<0.020
<0.020
9,100
3.1
Percent
Reduction
rincreaseV)M
ND
ND
55
93
(1,200)
ND
>76
ND
>94
(6,800)
(> 18,000)
Equation: Percent Reduction (Increase) = Analvte Concentration Untreated -
Analvte Concentration Treated
Dilution Ratio _
x 100%
Analyte Concentration Untreated
" An increase in metal and TDS concentrations may be due to presence of metals and other inorganics in the reagent mixture.
NA = Not analyzed
ND = Not possible to determine
> = Greater than
< = Less than
-------
w
TABLES
TCLP AND EP TOXICITY LEACIIATE RESULTS FOR OFF-SITE AREA ONE WASTE
PCBs (Mg/L)
Aroclor-1242
Arodor-1260
Metals (AA) (mg/L)
Arsenic
Lead
Metals (ICPES) (mg/L)
Barium
Cadmium
Lead
Nickel
Zinc
Other Chemical Analyses
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
Untreated
<0.42
<0.84
0.19
0.55
1.6
< 0.0050
0.46
0.033
0.63
6,300
1.9
Notes
* Percent reduction (increase) was calculated after
waste and 42 percent additives by weight.
TCLP
Treated
<0.44
<0.87
0.017
0.012
2.3
<0.0050
<0.050
<0.020
<0.020
9,000
12
correcting for
EP Toxicitv
Percent
Reduction
(Increase)""")
ND
ND
85
96
(150)
ND
>81
ND
>95
(150)
(990)
Untreated
<0.45
<0.90
0.18
0.12
0.58
0.0052
0.067
<0.020
0.26
790
2.6
dilution due to treatment. The treated Off-Site
/ Analyte
Equation: Percent Reduction (Increase) = Analvte Concentration Untreated - I
Treated
<0.21
<0.42
0.028
0.012
2.4
< 0.0050
<0.050
<0.020
<0.020
9,400
11
Percent
Reduction
nncreaseV"""
ND
ND
73
83
(610)
ND
ND
ND
>86
(2,000)
(630)
Area One waste was 58 percen
Concentration Treated \
Dilution Ratio I
x 100%
Analyte Concentration Untreated
An increase in metal and TDS concentrations may be due to presence of metals and other inorganics in the reagent mixture.
ND = Not possible to determine
> = Greater than
< = Less than
-------
Aroclor-1242
Aroclor-1260
Metals (AA) (mg/l,)
Arsenic
Metals (ICPES) (mg/L)
Barium
Cadmium
Lead
Nickel
Zinc
Other Chemical Analyses
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
Total Organic Carbon
Notes
TABLE 6
BET EXTRACT RESULTS FOR FILTER CAKE WASTE
Untreated
<0.42
<0.84
0.072
0.14
0.0073
0.87
0.063
0.27
440
0.65
91
1:4
Treated
<0.43
<0.86
0.011
6.3
<0.0050
<0.050
< 0.020
<0.020
3,800
6.3
140
Percent
Reduction
(Increase}'8"
ND
ND
74
(7,500)
ND
>90
>46
>87
(1,400)
(1400)
(160)
b) Untreated
<0.41
<0.82
0.014
0.28
<0.0050
0.42
<0.020
0.047
120
053
28
Treated
<0.41
<0.82
0.0037
3.4
<0.0050
<0.050
<0.020
< 0.020
1,700
2.7
43
Percent
Reduclfon(a)(|
ND
ND
55
(2,000)
ND
>80
ND
>28
(2,300)
(770)
(160)
W Untreated
<0.42
<0.84
0.020
0.47
<0.0050
0.18
<0.020
0.020
40
<0.40
11
MOO
Treated
<0.21
<0.42
0.0020
0.92
<0.0050
<0.050
<0.020
<0.020
760
<0.40
14
Percent
Rcduclion
£Increasel(a)
ND
ND
83
(230)
ND
>S3
ND
ND
(3,100)
ND
(120)
8 Percent reduction (increase) was calculated after correcting for dilution due to treatment. The treated filter cake waste was 59 percent waste and 41 percent additives by weight.
r*nnceii|ral'iPn
Equation: Percent Reduction (Increase)
__
Dilution Ratio
.A
x 100%
Analyte Concentration Untreated
b An increase in metal and TDS concentrations may be due to presence of metals and other organics in the reagent mixture.
ND = Not possible to determine
> = Greater than
> = Less than
-------
K>
PCBs(«g/L)
Aroclor-1242
ArocIor-1260
Metals (AA) (mg/L)
Arsenic
Metals (ICPES) (mg/L)
Barium
Cadmium
Lead
Nickel
Zinc
Other Chemical Analyses
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
Total Organic Carbon (mg/L)
Notes
TABLE 7
BET EXTRACT FOR FILTER CAKE/OILY SLUDGE MIXTURE
weight.
Equation: Percent Reduction (Increase)
Solid to Liouid Ratios
Untreated
<1.1
<2^2
0.042
0.83
0.036
1.7
0.049
2.7
1,800
3.2
200
• correcting
1:4
Treated
<0.42
<0.84
0.0080
17
< 0.0050
< 0.050
0.023
<0.020
3,500,
4.9
110
for dilution
Percent
Reduction
1 (lncreasera)(
ND
ND
52
(5,000)
>65
>93
(13)
>98
(390)
(280)
(38)
due to treatment.
b) Untreated
<0.44
<0.88
0.035
0.78
0.0062
0.43
0.028
0.69
470
2.2
60
1:20
Treated
<0.42
<0.84
0.0023
9.6
< 0.0050
< 0.050
<0.020
<0.020
2,300
1.3
32
Percent
Reduction
{Increasel
ND
ND
84
(3,000)
ND
>71
ND
>93
(1,100)
(48)
(33)
The treated filler cake/oily sludge waste
/ Analvtp Pnnrrnlralinn
Analvte Concentration Untreated
- I Dilution Ratio
TrralfA \
}
:a)(b) Untreated
<0.41
<0.82
0.0083
0.48
<0.0050
0.14
0.022
0.16
110
1.3
21
was 40 percent waste
x 100%
1:100
Treated
<0.22
<0.44
0.0030
2.6
<0.0050
< 0.050
<0.020
<0.020
1,200
0.43
8.0
Percent
Reduction
(Increase)*8*"
ND
ND
10
(>1,300)
ND
>11
ND
>69
(2,600)
17
5
and 60 percent additives by
Analyte Concentration Untreated
An increase in metal and TDS concentrations may be due to presence of metals and other organics in the reagent mixture.
ND = Not possible to determine
> = Greater than
> = Less than
-------
TABLE 8
BET EXTRACT FOR OFF-SITE AREA ONE WASTE
PCBs (jig/L)
Aroclor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Metals (ICPES) (mg/L)
Barium
Cadmium
Lead
Nickel
Zinc
Other Chemical & Physical Tests
Filterable Residue (JDS) (mg/L)
Oil & Grease, infrared (mg/L)
Total Organic Carbon (mg/L)
Notes
a
Percent reduction (increase) was calculated
weight.
Equation: Percent Reduction (Increase) =
Untreated
<2.3
0.38
0.11
0.0068
<0.050
< 0.020
<0.020
1,100
16
190
1:4
Treated
<0.43
<0.86
0.067
9.7
< 0.0050
<0.050
<0.033
< 0.020
4,600
26
120
Percent
Reduction .
(Increase)*"*'"
ND
ND
70
(15,000)
ND
ND
ND
ND
(620)
(180)
(9)
Untreated
<2.2
0.29
0.047
0.0055
< 0.050
< 0.020
<0.020
390
12
73
Treated
<0.21
<0.42
0.022
5.5
<0.0050
0.090
< 0.020
<0.020
2,600
15
54
Percent
Reduction,
(lncrease)(a> = Greater than
> = Less than
-------
transportable generator. The mixer is self-powered by a diesel engine. During
the demonstration, the equipment appeared to be problem-free.
The reagent and proprietary additives required for waste treatment are either
readily obtainable, such as cement or pozzoians, and water; or are required in
relatively small amounts that can be readily transported to the treatment location,
such as Urrichem and the other proprietary additives.
The conditions imposed upon Soliditech during the demonstration did not allow
optimum processing of waste, because each test run treated a different type of
waste. Nevertheless, it was apparent that the process was relatively easy to run
and moderately fast. Approximately 5 to10 cubic yards of waste can be treated in
an hour, once the equipment is set up and all reagent, proprietary additives, and
waste materials are ready to be added to the mixer.
The Soliditech process is able to solidify both solid and semi-solid materials. The
oily sludge found at the site was solidified after mixing it with some filter cake
material from the waste pile. Solids such as rocks or other debris up to 4 inches in
diameter can be accommodated by the process. The size of rocks and debris was
limited in this demonstration because of test sample requirements, but techniques
should accommodate any size particles and be limited only by the size of the
equipment used.
3.3.2
Limitations of the Soliditech Process
The process should only be used when the ambient temperature is above freezing
or when the treated material can be maintained at above freezing temperatures
during the first 24 hours after treatment. At lower temperatures the treated
material may not adequately solidify. The temperature during the demonstration
was above 35 degrees F during the day but below freezing at night. As a result,
all analytical samples and one block of solidified material from each test run were
allowed to cure in a heated warehouse at temperatures ranging from 50 to 70
degrees F.
The process is generally limited to treating wastes with a pH of 2 to 12. Waste
material with a neutral pH is ideal for treatment. The pH of the raw waste
material in this case ranged from 3.4 to 7.9.
Accurately determining of the weights of materials added to the mixer was
required for the demonstration but was found to be difficult. If this information
is necessary, more complicated gauges and weight feeders could be added to the
process; however, this would increase the system's complexity.
Since the Soliditech process is a batch process, a number of batches must be run to
treat a large area. During the demonstration, 14 cubic yards of material were
treated in four batches.
The process has certain limits to the amount of water or oil and grease that can be
accommodated without pretreatment of the waste. When large concentrations of
these materials are present, adjustments to the amounts of proprietary additives
must be made. Process limits on water and oil and grease content in the wastes
must be determined on a case by case basis. Waste material treated during the
27
-------
demonstration contained up to 58 percent water, and 17 percent oil and grease and
required no pretreatment.
It is difficult to assess when the treated material is adequately mixed. Some minor
problems were observed during the demonstration. The initial batch of treated
waste material (filter cake/oily sludge) was not totally blended as demonstrated by
unmixed lumps of waste material in the solidified product.
The suitability of the process for treating waste containing volatile organic
compounds is difficult to quantify as these chemicals may be lost during waste
collection and treatment.
The long-term stability of the treated waste material is not known. U.S. EPA will
monitor the solidified wastes for the next five years.
28
-------
4.0 SOLIDITECH PROCESS
4.1
PROCESS DESCRIPTION
The Soliditech, Inc. solidification/stabilization process uses a batch process to treat waste
material. A schematic diagram of this process is shown in Figure 4. The operating capacity of
the process is governed by the size of the mixer, the amount of time required to load and
discharge the mixer, and the amount of mixing time required to achieve homogeneous mixing of
the waste material and the reagent and additives. The two mixers used during the demonstration
had nominal capacities of 2- and 10-cubic yards.
The following materials were added to the Soliditech mixing unit during the
demonstration (Soliditech, I989a), measured either by weight or volume.
Waste Material (contaminated soil and sludge by weight and filter cake by
volume)
• Water (volume)
• Urrichem (volume)
• Proprietary Additives (weight)
• Pozzolanic Material/Cement (volume)
Based on treatability studies of samples of waste material collected at the Imperial Oil site
(PRC, 1988a), Soliditech optimized treatment formulations for each of the waste materials to be
treated. The formulations are presented in Table 9 (Soliditech, 1989a). As this table shows, the
amounts of the reagent, proprietary additives, pozzolanic material, and water were approximately
proportional to the amount of waste treated.
4.2
PROCESS SCHEMATIC
The Soliditech process, as shown in Figure 4, includes the following operations:
• A measured amount of waste material is added to the mixer through the screen
welded to the mixer top. This is accomplished by a front-end loader or drum
grappler.
• Measured amounts of water, reagent, and proprietary additives are added to the
mixer by pump, front-end loader, or drum grappler and thoroughly mixed with
the waste.
29
-------
TABLE 9
SOLIDITECH TREATMENT FORMULATIONS
Estimated Weights
of Materials (lbs.)(a>
Filter Cake/
Reagent Mixture Oily Sludge
Filter Cake Off-Site Area
Waste Material
Type II Cement(c)
Urrichem
Additives
Water
800(b>
442
8.96
16.5
154
3,950
4,970
39.2
140
666
11,200
4,920
111
167
2.687
9,100
4,540
90.7
136
1.830
TOTAL WEIGHT
1,420
9,760
19,100
15,700
Notes:
The weights for cement, filter cake, Urrichem and water were calculated based on
volume.
b Clean sand used rather than waste material for this test run.
c According to Soliditech, fluffing of the cement may cause the cement weight values to be
as much as 5 percent higher than the actual weight, because the weight of cement was
estimated from volume added.
30
-------
FIGURE 4
SOLIDITECH PROCESS SCHEMATIC
Source: Soliditech, 1987.
31
-------
4.3
The cement is then measured and added to the mixer using the front-end loader.
The resulting mixture is mixed for approximately 40 to 60 minutes.
The treated waste mixture is discharged to one-cubic yard forms. Samples to be
used for analyses are collected directly from the cubic-yard forms. All treated
material is allowed to cure for 28 days. At this time, the solidified treated waste
material is removed from the forms and sample containers.
EQUIPMENT SPECIFICATIONS
The equipment used in the Soliditech process can be grouped into four categories,
according to their use:
Equipment for receipt, storage, and handling of incoming raw materials and
hazardous wastes.
• Process equipment for introducing the ingredients into the mixer, blending the
ingredients, and discharging the batches of treated waste.
Containers or mold to hold the batch mixture in a stable configuration while the
mixture reacts and solidifies within the mold.
• Support equipment and facilities such as electrical power and power lines, an
office trailer, a decontamination area, sanitary facilities, decontamination
equipment, maintenance supplies, and tools.
The receipt, storage, and handling equipment for the demonstration consisted of one bulk,
dry solids transfer truck to contain the pozzolanic material or cement; one elevated receiving and
storage bin with dust control filter and blower (requiring a generator or other electrical source
supplying 120 volt, 60 Hz, 30 amp electrical service) to transfer the cement; one portable scale to
pre-weigh raw waste material; an all-terrain forklift to move drums and blocks of raw and
treated materials; and a dump truck to hold the contaminated soil from Off-Site Area One prior
to treatment.
The processing equipment included a 10-cubic-yard mixer with hydraulically actuated
legs, a hydraulic agitator, a screen with 4-inch by 4-inch openings to trap and remove any large
roots, debris, or other material from the waste to be treated, and a small 2-cubic-yard mixer.
The large Soliditech mixer with attached screen is pictured in Figure 5. The small mixer was
brought to the site to demonstrate that small volumes of waste could also be treated by the
Soliditech process. This mixer was used to process sand, Urrichem, cement and proprietary
additives for the reagent mix test run.
32
-------
The molds were reinforced 1-cubic-yard plywood forms. Treated waste material from
the mixing unit was discharged into these forms. An all-terrain forklift was used to move and
store the filled forms.
Equipment was decontaminated with a highr-pressure steam cleaner. Waste water and
solid residual material from decontamination was collected and stored for disposal by New Jersey
Department of Environmental Protection (NJ DEP).
The following specifications describe the equipment in more detail, including capacities,
dimensions, functions, and optional equipment:
• Pozzolanic Material/Cement Bin and Hopper — This upright aluminum hopper
can discharge through a flexible hose. The hopper is 9- by 9- by 16-feet high
and feeds down to an 8-foot-high cone bottom. The hopper is supported on four,
10-foot-legs. During the demonstration the cement was transferred from the
hopper through the hose to the bucket of a front-end loader that transferred the
cement to the mixer. The bucket of the front-end loader was previously
calibrated. Dust emissions during filling and removal were controlled by a
baghouse.
• Bulk Cement Storage Trailer — The bulk transport trailer that delivered the
cement for the demonstration had a hopper adequate to hold 12 tons of cement.
The cement was transferred from the hopper of this trailer to the storage bin and
hopper. Dust emissions during filling and removal were controlled by a baghouse.
• Reagent Storage Tank and Metering System — The reagent storage system
consisted of two 350-gallon steel tanks mounted on the mixer transport trailer, and
a metering pump capable of displacing an accurate volume of liquid. The pump
was used to transfer reagent from the storage tank to the mixing unit.
» Mixing Unit — The large Soliditech mixer is a narrow, low profile, totally
independent and self-contained, 10-cubic-yard unit measuring 20 feet long, 8 feet
wide, and 4 feet high. It is mounted on a low-boy trailer for total mobility. The
mixing unit has a variable speed agitator and specialized lifting mechanism that
allows for total mixing and complete discharge of mixed product. The open top
allows for visual inspection of consistency and volume as well as easy loading from
front-end loaders, and drums. For the demonstration, a screen with 4-inch by 4-
inch openings was welded to the top of the mixer and used for screening waste
material. The mixing unit has an independent four-point body hoist that can raise
the mixing unit to a height of 6 feet, thus allowing the mixing unit to be placed
above drums, plywood forms, or a feed hopper for easy discharge of the treated
waste material with minimal handling and contact.
The mixer blade consists of a full sweep, bi-directional paddle mixer with mixing
speeds between 2 and 16 revolutions per minute. Each paddle sweeps the bottom
of the shell for complete mixing, discharge, and clean-out of the materials, with
no dead areas of mixing. The mixing unit contains an eccentric, weighted,
hydraulic vibrator rated at 2,000 revolutions per minute to aid clean out. All
mixer controls are located at the rear of the mixing unit.
33
-------
The small Soliditech mixer is a self-contained, 2-cubic yard unit measuring 6 feet long, 3
feet wide, and 5 feet high. It is mounted on a trailer. It is operationally similar to the large
Soliditech mixer.
34
-------
5.0 DEMONSTRATION PROCEDURES
This section presents the site description, the waste characteristics, the sampling and
analysis plan, and the QA/QC plan for the Soliditech demonstration.
5.1
SITE DESCRIPTION
The Soliditech technology demonstration was conducted at the Imperial Oil
Company/Champion Chemical Company site in Morganville, Monmouth County, New Jersey.
The site is located on Orchard Place in Morganville, approximately 1/2 mile northwest of the
junction of Rt. 3 and Rt. 79 (Figure 1). The site is situated in a largely rural area with scattered
residential properties along surrounding roads. A commercial shopping center is located 1/2 mile
southeast of the site, and two automobile scrap yards are located just northwest of the site. Lake
Lefferts, a swimming and recreational area, is located approximately 1 mile north of the site.
Lake Lefferts receives surface-water drainage from the watershed that contains the Imperial Oil
site. The average annual temperature (Newark) is approximately 52° F and the monthly average
temperatures range from approximately 32° F in January and February to 76° F in July.
The site is divided into the area presently occupied by the Imperial Oil Company facility
(On-Site Area) and certain immediately surrounding areas (Off-Site Areas One and Two). These
two areas of the Superfund site are shown in Figures 2 and 3. For the purposes of this SITE
demonstration, the NPL definition of the Imperial Oil site will be used. The property occupied
by the Imperial Oil Company, where the demonstration was performed, is enclosed by a security
fence. The surrounding areas, including the areas referred to as Off-Site Area One and Off-Site
Area Two, are not fenced. The off-site areas are undeveloped.
The on-site area immediately adjacent to the waste pile is underlain by 2 to 10 feet of fill
material, consisting of sand, silt, and gravel and containing varying amounts of ash, oil sludge,
waste filter cake, wood fragments, coal, bricks, concrete rubble, vinyl, and fiberglass debris.
This fill material is a result of past activity at the site and is not found in the off-site areas.
Ground-water monitoring has shown considerable contamination of volatile and semivolatile
organic compounds and petroleum hydrocarbons. Surface water in the vicinity of the site has
shown minimal contamination (E.C. Jordan Co., 1987).
Use of the Imperial Oil Co./Champion Chemical Company facility dates back to
approximately 1912, when a factory that produced tomato paste and ketchup was established at
the site. Near the end of World War I the facility was converted to a chemical processing plant,
producing arsenic acid and calcium arsenate as well as artificial flavors and fragrances. In the
35
-------
late 1940s the plant was purchased by Champion Chemical Company and was used as an oil
reclamation facility. Since 1968, Imperial Oil Company has leased the site from Champion
Chemical Company, using the facility for blending and repackaging oils.
No process wastewater is presently generated at the facility. Site precipitation runoff is
reportedly treated by oil-water separators, with the oil being collected for reuse. Waste disposal
practices prior to the 1950s are generally unknown, although it has been reported that an oil-
settling lagoon was once located at the rear (north corner) of the Imperial Oil Company property.
At approximately the same time, large piles of oil-saturated soil or filter cake clay are alleged to
have been stored at the site. Most of this material was subsequently sent off-site for disposal.
The remains of one of these piles is still located along the northwest fence line at the rear of the
property. This is referred to as the waste filter cake pile or waste pile. An old storage tank that
contains an oily sludge of unknown origin is still present at the northern corner of the property.
This is referred to as the abandoned storage tank. In addition to the plant areas, two adjacent but
off-site areas north of the facility were allegedly used as dump sites for waste oil and waste
sludge material.
As a result of past waste handling practices at this facility, surface and subsurface soils
and ground water have been contaminated with organic chemicals, including petroleum
hydrocarbons, metals, and polychlorinated biphenyls (PCBs, also known by their trade name,
Aroclor, which is a mixture of PCB congeners). Potential sources of additional contamination,
such as the waste pile of oil-saturated filter cake clay, still exist on the site.
Previous environmental investigations at the site included the installation of 14 ground-
water monitoring wells and the excavation of six test pits. NJ DEP, with support of the U.S.
EPA, is presently performing a remedial investigation and feasibility study (RI/FS) under the
auspices of the Federal Superfund program to investigate and resolve the environmental
contamination problems associated with the Imperial Oil site. Additional information will be
available when the study is completed.
5.2
WASTE CHARACTERISTICS
Environmental media, such as surface soil, subsurface soil, and ground water, were
sampled and analyzed by E.G. Jordan Company during the Phase 1 sampling as a preliminary
chemical characterization of the Imperial Oil site (E.G. Jordan Co., 1987). Contaminants at the
site included PCBs, metals, and organic chemicals, mainly petroleum hydrocarbons. These
contaminants are thought to be primarily from previous oil recycling operations at the site, but
may also be from other past activities at the facility.
-------
The waste pile contains filter cake material contaminated with waste oil filtrate residues.
The abandoned storage tank contains an oily sludge. Each is expected to contain fairly uniform
contaminant levels. The two other contaminated areas of the site, Off-Site Areas One and Two,
contain soil contaminated with either waste oil or oily filter cake material similar to that in the
waste pile. The two off-site areas contain scattered "hot spots" of contamination that appear to
decrease in intensity with depth. At several locations, these "hot spots" extend to a soil depth of 3
feet or more (PRC, 1988a). As a result of this study, Off-Site Area Two was eliminated from
further study, as it was very similar in chemical composition to Off-Site Area One but less
accessible.
U.S. EPA contractors visited the Imperial Oil Company/Champion Chemical Company
site in May 1988 to survey and sample four possible site locations that were being considered for
treatment during the Soliditech demonstration (PRC, 1988a). The samples were analyzed to
determine contaminant levels at each of the locations, to evaluate their suitability for treatment.
Additional sample material was also provided to allow Soliditech to test its process on actual site
material and formulate appropriate treatment mixtures. In addition, the raw and treated waste
from the site was provided to the analytical laboratory to determine potential analytical problems.
Additional laboratory cleanup procedures were required for all samples due to the high
levels of oil and grease. Diagnosis of this problem saved considerable time when the
demonstration samples were analyzed by the laboratory. (Data from the treatability study are
included as Appendix C.)
The areas of the site selected for the demonstration contain various types and
concentrations of chemical contamination. PCBs of concern in these areas include Aroclors 1242,
1248, and 1,260. Metals found at one or more of these areas include arsenic, beryllium, cadmium,
chromium, copper, lead, mercury, nickel, selenium, thallium, and zinc. High levels of an organic
mixture identified as petroleum hydrocarbons were identified in all areas. Low levels of volatile
organic chemicals (VOCs) have also been detected at the site. VOCs found in samples from these
areas include benzene, ethylbenzene, tetrachloroethene, toluene, trichloroethene, 2-butanone, 2-
hexanone, 4-methyl-2-pentanone, and total xylenes. Semivolatile organic chemicals (SVOCs)
found in samples from these areas include bis(2-ethylhexyl)phthalate, butylbenzylphthatate,
di-n-octylphthalate, 4-bromophenyl phenyl ether, and 2-methylnaphthanene (Radian, 1988 and
Appendix A). This data is presented in Section 7.
37
-------
5.3
DEMONSTRATION PREPARATION
Demonstration preparation included preparing a Demonstration Plan and a Health and
Safety Plan, informing the public of a planned visitor's day, setting up an office trailer with
electrical and phone service, mobilizing earth moving equipment, preparing decontamination
•zones and areas, constructing the large plywood forms to hold the treated waste, setting up
sanitary facilities, making arrangements with the Imperial Oil Company to operate at their
facility, and holding health and safety briefings prior to and during the demonstration.
Established health and safety procedures were followed.
5.4
SAMPLING PROGRAM
The objective of the sampling program was to develop and implement sampling strategies
that produce scientifically valid data useful for evaluating treated waste produced by the
Soliditech process. The sampling protocols were designed to provide statistical comparisons of
the physical and chemical characteristics of the contaminated wastes before and after treatment.
These statistical comparisons provide the basis for determining the success of the Soliditech
process at the Imperial Oil Company/Champion Chemical Company site. This section describes
the waste material collection locations, sampling schedule, sample recovery procedures, and
analytical procedures. Table 10 shows the numbers and sizes of samples collected for testing
during the demonstration.
5.4.1
Waste Material Collection Locations
The waste material collection areas chosen for the demonstration at the Imperial Oil site
are shown in Figures 2 and 3. These locations represent areas contaminated with metals, VOCs,
SVOCs, petroleum hydrocarbons, and PCBs. Preliminary sampling during site screening indicated
that the contaminated soil from Off-Site Area One to be used for treatment could be removed
from a soil depth of up to 30 inches, compatible with the backhoe used to excavate the soil for
treatment. A backhoe was also used to collect waste filter cake from the waste pile. The sludge
from the abandoned storage tank was collected by hand, using a bucket. The sludge was mixed
with waste pile material in the Soliditech mixer before treatment.
5.4.2
Sampling Schedule
A complex array of samples was collected to facilitate an effective evaluation of the
process. Samples of contaminated waste were collected immediately prior to treatment
(pretreatment samples). Process reagent and proprietary additives were used to treat a test run of
38
-------
TABLE 10
SAMPLING REQUIREMENTS
PRETREATMENT WASTE SAMPLES
Number of Samples Collected Containers
Reps Areas Reserve Total per
Parameter (a) (b) Sample
Leaching Tests (d) 3 3 1 12 2
Chemical Tests (e) 3 31 12 1
(g) 3 3 1 12 1
Total
Containers
Used
24
12
12
Containers
Type Size Sampling
(c) Device
Glass 1000 mL Scoop
Glass 1000 mL Scoop
Glass 250 mL Scoop
Preservation
Requirements Holding Time
Cool, 4* C Not specified
Cool, 4J C (0
Cool, 4' C Analyze within 14 days
Engineering/Geotechnical
u, Tens
vo
Notes:
(a)
(b)
(c)
(0)
(e)
(0
(g)
(h)
(0
(h) 3 3 1 12 1
(i) 3 3 1 12 1
Reps = replicates.
Reserve (contingency) samples per area.
All glass jars had teflon-lined closures.
Toxicity Leaching Procedure Test (TC1.P), Batch Extraction Test (BET),
pH, Eh, Loss on Ignition, Acid Neutralization Capacity, Oil and Grease,
Analyze for pH and Eh as soon as possible.
28 days for Mercury, and Oil and Grease.
6 months for all other metals.
Extract for PCBs and SVOCs within 14 days and analyze SVOCs extract
Not specified for Loss on Ignition or Acid Neutralization Capacity.
VOCs.
Panicle size and water content.
Bulk density.
12
12
, and Extraction
Glass 500 ml. Scoop
Shelby 3' x 12' Shelby
lube lube
Procedure Toxicity Test (EP).
Seal Not specified
Seal and Not specified
prevent breaking
Metals, SVOCs, and PCBs.
in 30 days and
PCBs extract in 40 days.
-------
TABLE 10 (Continued)
SAMPLING REQUIREMENTS
REAGENT MIX SAMPLES
Number of Samples Collected
Reps Areas Reserve Total
Parameter (a) (b)
Leaching Tests (c) 3 1 1 4
Chemical Tests (d) 3 1 14
Notes:
(a) Reps = replicates.
(b) Reserve (contingency) samples per area.
(c) TCLP, BET, and EP.
Containers Total
per Containers
Sample Used
.2 8
1 4
•a/-
-------
TABLE 10 (Continued)
SAMPLING REQUIREMENTS
SOLIDIFIED WASTE SAMPLES
Number of Samples Collected
Reps Areas Reserve
Parameter (a) (b)
Leaching Tests (c) 3 3*1
(d) 3 3 2
Chemical Tests (e) 3 3 1
Engineering/Geotechnical
Tests
(g) 3 3 2
(h) 3 3 2
(0331
Notes:
(»)
(b)
(c)
(0)
(e)
(0
(g)
(h)
(i)
Total
12
15
12
15
IS
12
Containers
per
Sample
2
1
1
2
2
1
Reps = replicates.
Reserve (contingency) samples per area.
TCLP, BET, and EP.
American Nuclear Society Test 16.1 (ANS 16.1)
pH, Eh, Loss on Ignition, Acid Neutralization Capacity, Oil and Grease,
Analyze for pH and Eh as soon as possible.
Analyze for volatile organics within 14 days.
28 days for Mercury, and Oil and Grease.
6 months for all other metals.
Extract for PCBs and SVOCs within 14 days and analyze SVOCs extract
Not specified for Loss on Ignition or Acid Neutralization Capacity.
Water content, bulk density, and unconfmed compressive strength.
Wet/dry weathering and freeze/thaw weathering.
Permeability.
Total Containers
Containers Type Size
Used (c)
24 Mold 3"x6"
15 Mold 2.5 cm x
4.8cm
12 Mold 3' x 6"
30 Mold 3" x 6"
30 Mold 4.5 cm x
7.4 cm
12 Mold 3" x 3"
Metals, VOCs, SVOCs, and PCBs.
in 30 days and PCBs extract in 40 days.
Sampling
Device
Dipper
Dipper
Dipper
Dipper
Dipper
Dipper
Preservation
Requirements
Cool, 4* C
Seal and
prevent breaking.
Cool, 4* C
Seal and
prevent breaking
Seal and
prevent breaking
Seal and
prevent breaking
Molding Time
Not specified
Not specified
(0
Not specified
Not specified
Not specified
-------
TABLE 10 (Continued)
SAMPLING REQUIREMENTS
LONG-TERM SOLIDIFIED WASTE SAMPLES
Number of Samples Collected Containers Total Containers ^
Reps Areas Iteserve
Parameter (a) (b) (c)
Leaching Tests (e) 3 3 1
(Q 3 3 1
3 3 1
£ Special Tests (g) 3 3 1
Notes:
Times per Containers lype aizc oampimg
(d) Total Sample Used (c) Device
4 48 1 48 Mold 3" x 6" Dipper
1 12 1 12 Mold 3" x 18" Dipper
1 12 1 12 Mold 6' x 18"
5 60 1 60 Mold 3"x3" Dipper
(b) Long-termPm'cmitoring was performed on the Off-Site Area One soil, the waste filter cake, and the waste filler cake/oily sludge
(c) Reserve (contingency) samples per area. Reserves will not be used for analyses unless original samples are lost or damaged.
(d) Samples for TCLP and EP leaching tests will be taken at 6 months, 12 months, 24 months, and 60 months.
(e) TCLP and EP. .
(0 Waste Interface Leaching Test (WILT). Leachates will be collected from each of 18 molded core samples at two-week intervals
(g) Petrographic examination and air-void content.
; Preservation
Requirements
Cool, 4* C
Seal and
prevent breaking
Seal and
prevent breaking
Holding Time
Not specified
Not specified
Not specified
mixture.
for 30 weeks after the 28-day cure.
-------
clean sand (reagent mix). Samples of all test runs of treated material were collected after
treatment (post-treatment samples). Sampling requirements were also established for a long-term
monitoring program designed to evaluate chemical and physical stability over a period of 5 years.
The sampling and analysis contractor collected pretreatment samples of the contaminated
Off-Site Area One soil, waste pile material, a mixture of storage tank sludge and waste pile
material, clean sand used for the control test run, and residual material (also referred to as the
predemonstration blank) remaining in the Soliditech mixer from previous work. (The residual
material was cleaned out of the mixer as well as possible before the mixer was used.) They also
collected treated slurry from each of the four treatment test runs.
5.4.2.1
Pretreatment Sampling Methods and Types
Pretreatment samples were required to establish the chemical and physical characteristics
of the waste material and the variability associated with those characteristics. Triplicate samples
of the pretreatment waste material were taken for each analytical parameter at each sampling
area. An additional sample of each pretreatment material for each test was collected and held in
reserve.
Undisturbed bulk density samples from Off-Site Area One and the waste pile were
collected with Shelby Tubes prior to the excavation of material for the demonstration. Samples
for bulk density determinations of the oily sludge and waste pile mixture were collected in glass
jars after these materials were mixed in the mixing unit. Two sets of triplicate samples were
collected for the physical tests — one set for particle size and water content and the other set for
bulk density.
Immediately prior to waste material collection, pretreatment samples were collected for
chemical analyses, leaching tests, and chemical analyses of the leachate. The contaminated
material for these samples was collected either from the excavation site (waste pile) or from the
Soliditech mixer, after being thoroughly mixed but prior to adding any reagent or proprietary
additives. Individual grab samples were taken from different parts of the waste pile or from the
mixed raw material in the Soliditech mixer. These samples were transferred to individually
labeled sample jars for shipment to the laboratory. One set of triplicate samples was collected for
the TCLP, BET, and EP leaching tests. Two sets of triplicate samples were collected for chemical
tests and analyzed for the following: pH, Eh, loss on ignition, acid neutralization capacity, oil and
grease, metals, PCBs, VOCs, and SVOCs. The analytical procedures performed on each
pretreatment waste material are shown in Table 11.
43
-------
TABLE II
STANDARD METHODS AND PROCEDURES OF SAMPLE ANALYSIS
Reference
Parameter Samr-le Tvne Mnhnd Number Tille Meinoo lvpc_. """"'.V"
ON-SITE TESTS
Molds for Forming
Concrete
Making and Curing Concrete
Slump of Portland Cement
Concrete
Sampling Freshly Mixed
Concrete
Homogeneity of Mixing
HNGINEERING/GEOTECHNICAI
Particle size
Water Content
Bulk Density
S ASTM C470
S ASTM C31
S ASTM C143
S ASTM C172
S ASTM C136/CI42
-TESTS
U ASTM D-422
U Modified AS™
D-2216
T TMSWC^
U ASA-13-2
T TMSWC-2
Molds for Forming Concrete
Test Cylinders Vertically
Making and Curing Concrete
Test Specimens in the Field
Slump of Portland Cement
Concrete
Sampling of Freshly Mixed
Concrete
Sieve Analysis of Fine and
Coarse Aggregates/Clay Lumps
and Friable Particles in
Aggregates
Particle Size Analysis
Determination of Water Content
of Soil, Rock, and Soil
Aggregate Mixture
Water Content
Bulk Density-Excavation Method
Bulk Density Volumetric
Visual/Gravimetric ASTM (ASTM, 1987)
Specification ASTM
Vertical Distance ASTM
Specification ASTM
Sieve/Gravimetric ASTM
Sieve/hydrometer ASTM
Gravimetric ASTM
.
Gravimetric TMSWC
Gravimetric/ ASA (I'agc, 1982)
Volumetric
Gravimetric TMSWC
Notes:
S = Treated waste, while still a slurry.
U = Untreated waste.
RM = Reagent mix.
T = Treated waste.
LT = Treated waste, long-term
L = Leachate.
monitoring.
LTI, = Ixachate, long-term monitoring.
-------
TABLE 11 (Continued)
STANDARD METHODS AND PROCEDURES OF SAMPLE ANALYSIS
in
Parameter
Sample Type
Method Number
'Pile
ENOINRRRING/GEOTECHNICAI. TESTS (Cont'd)
Permeability T
Unconfined Compressive T
Strength
Wet/Dry Weathering Test T
Freeze/Thaw Weathering Test T
SPECIAL TESTS
TMSWC- 13 Falling-Head Permeability Test Volumetric
Using a Triaxial Cell
ASTM D-1633 Compressive Strength of Molded Stress Resistance
Soil-Cement Cylinders
TMSWC-12 Wet/Dry Weathering Test Gravimetric
TMSWC-11 Freeze/Thaw Weathering Test Gravimetric
TMSWC
ASTM
TMSWC
TMSWC
Petrographic Examination
T/LT
ASTM C856 Petrographic Examination of Visual/Optical
Hardened Concrete
ASTM
Air Void Content
Notes:
S = Treated waste, while still a slurry.
U = Untreated waste.
RM = Reagent mix.
T = Treated waste.
IT = Treated waste, long-term monitoring.
L = Leachate.
LTL = Leachate, long-term monitoring.
ASTM C457 Microscopic Determination of Microscopic
Air-Void and Parameters of the
Air-Void System of Hardened
Concrete
ASTM
-------
o\
TABLE 11 (Continued)
STANDARD METHODS AND PROCEDURES OF SAMPLE ANALYSIS
Method Tvne
Reference
Parameter SamolcTvpc Method Numoer «»!£ r-T — tn-
LEACHING TESTS
TCLP
ANS 16.1
BET
EP
WILT
U/RM/T/LT
T
U/RM/T
U/RM/T/LT
LT
TCLP Toxicity Characteristic
Leaching Procedure
ANS 16.1 American Nuclear Society 16.1
Test
Batch Extraction Test
EPA Method ' Extraction Procedure Toxicily
1310 Test
Waste Interface Leaching Test
TCLP (Federal Register, 1986)
American Nuclear Society (ANS,
1986)
(Cote, 1988)
SW 846 (U:S. EPA, 1986)
Comparison of Laboratory Batch
Methods ind Large Columns for
Evaluating Leachate from Solid
Waste, 1988. (Jackson, 1988)
CHEMICAL TESTS
pH
Eh
Notes:
S =
U =
RM =
T =
LT =
L =
LTL =
U/RM/T
L/LTL
U/T
L/LTL
Treated waste, while still a slurry.
Untreated waste.
Reagent mix.
Treated waste.
Treated waste, long-term monitoring.
Leachate.
Leachate, long-term monitoring.
EPA Method Soil pH Electromelric
9045
EPA Method pH Elcclromctric Measurement lileclromelric
9040
Modified EPA Electromelric
Method 9045
ASTM D-1498 Standard Practice for Oxidation- Electromelric
Reduction Potential of Water
SW846
SW846
SW846
ASTM
-------
TABLE 11 (Continued)
STANDARD METHODS AND PROCEDURES OF SAMPLE ANALYSIS
Parameter
Sample Type Method Number
Title
CHEMICAL TESTS fConfd)
TDS
Acid Neutralization Capacity
TOC
Loss on Ignition
Oil and Grease
Metals
Sb, As, Ba, Be, Cd, Cr, Cu, Ni,
Ag, Tl, Zn, Ca, Al, Pb,
Ni
Sb, Ba, Be, Cd, Cr, Cu, Ni, Ag,
Zn, Ca, Al, Na
Sb, Ba, Be, Cd, Cr, Cu, Ni, Ag,
Zn, Pb, Na
Notes:
L
U/RM/T
L
U/T
U/T
L/3550
Extract
U/RM/T
L/LTL
3050/3010
Digestates
EPA Method
160.1
TMSWC-7
EPA Method
415.1
ASTM C114
Modified EPA
Method 3550
EPA 413.2
EPA Method 3050
EPA Method 3010
EPA Method 6010
Residue, Filterable
Acid Neutralization Capacity
Organic Carbon, Total
Loss on Ignition
Sonication Extraction
Oil & Grease, Total
Recoverable
Acid Digestion of Sediments,
Sludges and Soils
Acid Digestion of Aqueous
Samples and Extracts for Total
Metals Analyses by FAA or ICT
Speclroscopy
Inductively Coupled Plasma
Atomic Emission Spectroscopy
Gravimetric
Elect romclric
Combustion
Gravimetric
IR
ICT Analysis
S = Treated waste, while still a slurry.
U = Untreated waste.
RM = Reagent mix.
T = Treated waste.
LT = Treated waste, long-term
L = Leachate.
LTL = Leachate, long-term moni
monitoring.
itoring.
Reference
EPA 600 (U.S. EPA, 1979)
TMSWC (Environment
Canada/U.S. EPA, no dale)
EPA 600
ASTM
SW846
EPA 600
SW846
SW846
SW846
-------
Parameter
CHEMICAL TESTS (Conl'd)
Pb.Ti
Pb
11
As
Se
Hg
»g
Volatile Organic
Analysis
TABLE 11 (Continued)
STANDARD METHODS AND PROCEDURES OF SAMPLE ANALYSIS
Sample Type Method Numlier
L/LTL EPA Method 3020
3020/3050 EPA Method 7421
Digestates
3020/3050 EPA Method 7841
Digestates
L/LTL/3050 EPA Method 7060
Digestates
L/I.TL/3050 EPA Method 7740
Digestates
U/RM/T EPA Method 7471
L/LTL EPA Method 7470
U/T EPA Method 8240
Notes:
S = Treated waste, while still a slurry.
U = Untreated waste.
RM = Reagent mix.
T » Treated waste.
LT = Treated waste, long-term monitoring.
L = Lcachate.
LTL = Leachate, long-term monitoring.
Title
Acid Digestion of Aqueous
Samples and Extracts for Total
Metal Analysis by GFAA
Spectroscopy
(Atomic Absorption,
Furnace Techniques)
Thallium (Atomic Absorption,
Furnace Technique)
Arsenic (Atomic Absorption,
Furnace Technique)
Selenium (Atomic Absorption,
Furnace Technique)
Mercury in Solid or Semisolid
waste (Manual Cold-Vapor
Technique)
Mercury in Liquid Waste
(Manual Cold-Vapor Technique)
Gas Chromatography Mass
Spectrometry for Volatile
Organics
Method Type
Reference
SW846
AAS-GF
AAS-GF
AAS-GF
AAS-GF
AAS-CV
AAS-CV
GS-MS
SW846
SW846
SW846
SW846
SW846
SW846
SW846
-------
Parameter
CHEMICAL TESTS (Cont'd)
Semivolalile Compounds
Polychlorinaled Biphenyls
STANDARD
Sample Type Method Numlicr
L/LTL EPA Method 3520
EPA Method
3540/3611
TABLE 11 (Continued)
METHODS AND PROCEDURES OF SAMPLE ANALYSIS
Title Mel lux] Type
Continuous Liquid-Liquid
Extraction
Soxhlet Extraction/ Alumina
Column Cleanup and Separation
of Petroleum Waste
3540/3620 EPA Method 8270
Extracts
L/LTL
EPA Method 3520
U/RM/T EPA Methods
3540/3620/3630
3520/3540 EPA Method
Extracts 8080
3520/3540 EPA Method
Extractt680 (Backup)
RM/T
EPA Method
3550/3611
Notes:
S = Treated waste, while still a slurry.
U = Untreated waste.
RM = Reagent mix.
T = Treated waste.
LT = Treated waste, long-term monitoring.
L = Leachate.
LTL = Leachate, long-term monitoring.
GC/MS for Semivolalile GC/MS
Organics: Capillary Column
Technique
Continuous Liquid-Liquid
Extraction
Soxhlet Extraclion/Florisil
Column Cleanup/ Silica Gel
Cleanup
Organochlorine Pesticides and GC/ECD
PCBs
Determination of pesticide PCBs GC/MS
in Water and Soil/Sediment by
GC/MS
Sonicalion Extraction/ Alumina
Column Cleanup and Separation
of Petroleum Waste
Reference
SW846
SW846
SWW6
SW846
SW846
SWS46
EPA Method 680, 1985
SW846
-------
The clean sand used for the reagent mix/control test run and the residual material found
in the Soliditech mixer upon its arrival at the site were also sampled and analyzed for chemical
constituents.
5.4.2.2
Reagent Mix Sampling Methods and Types
Before treating any waste material, Soliditech performed a test run on clean sand using
Urrichem and the same proprietary additives, cement, and water to be used for the waste
treatment runs. Triplicate samples of this treated sand slurry were collected and used as control
samples for chemical and leaching tests. A fourth sample was collected for each sample set and
held in reserve. This treated reagent mix was sampled to establish which additional chemicals
were added to the contaminated wastes and to establish baseline characteristics for various
physical tests. Chemical tests included analyses of pH, acid neutralization capacity, metals, PCBs,
and SVOCs. The leaching tests consisted of the following: TCLP, BET, and EP Toxicity test.
The analytical procedures performed on the control samples are shown in Table 11.
5.4.2.3
Post-Treatment Sampling Methods and Types
Post-treatment solidified samples were required to determine the extent to which
contaminated wastes had stabilized, in terms of physical, chemical, and leaching characteristics.
Post-treatment samples were collected in triplicate as a slurry and allowed to cure for a minimum
of 28 days prior to analyses. An additional sample from each treatment run was collected and
held in reserve. Less significant changes in the chemical and physical nature of the treated
material were anticipated past the 28-day curing period.
Samples to be used for the long-term evaluation of the solidified soil were scooped out of
the large plywood forms, placed in labeled sample molds, and allowed to cure on-site. The size
of the solidified soil sample molds depended upon the volume needed for the chemical analysis or
the sample size specified for physical testing. Both immediate and long-term sample analyses
were run using the solidified slurry samples collected from the cubic-yard forms and placed into
smaller molds at the time of the demonstration. The treated wastes in the cubic-yard forms were
allowed to cure for 28 days before they were uncrated and prepared for long-term storage. This
treated waste will remain on-site for long-term monitoring. They were placed in a closely
formed stack that was wrapped in 40-mil thick high-density polyethylene (HDPE) film for
protection. Periodically, the solidified waste blocks will be unwrapped and examined as part of
the long-term monitoring.
50
-------
5.5
PHYSICAL TESTS
A number of physical tests were performed on the samples collected during the Soliditech
SITE demonstration. Table 11 lists these tests, which are described in this section.
5.5.1
Oil-Site Tests
The treated waste slurry was subjected to the following on-site tests:
ASTM C143: Slump of Portland Cement Concrete — A representative sample of solidified waste
was placed in a dampened slump-test mold on a flat, moist, non-absorbent surface. The mold
was filled in three equal-volume layers. Then, each layer was rodded with 25 strokes of the
tamping rod. After the top layer was rodded, excess concrete was struck off. The mold was
immediately removed from the concrete by raising it vertically. The slump was measured by
determining the vertical difference between the top of the mold and the original center of the top
surface of the specimen. Each test was completed in 2.5 minutes.
ASTM C136 and C142: Homogeneity of Mixing — The homogeneity of mixing of a test run of
treated waste was determined using adaptations of ASTM Methods C136 and C142. ASTM C136
is the Standard Method for Sieve Analysis of Fine and Coarse Aggregates. ASTM C142 is the
Standard Test Method for Clay Lumps and Friable Particles in Aggregates. For this test a sample
of the treated waste slurry was collected immediately after treatment and sieved through three
different-sized sieves. The material remaining on each of the sieves was weighed. All particles
that could be broken with the fingers into fines were removed by wet sieving. The three sieves
were weighed again. The weight differences were due to the fractions initially retained on each
sieve that passed through the sieve after breaking with the fingers. This weight of material was
designated as clay lumps or friable particles. The percentage of material retained on each sieve
was also calculated to determine the particle size distribution of the aggregates. The percent of
clay lumps and friable particles was then calculated.
5.5.2
Laboratory Tests
The raw and treated wastes were received by the analytical laboratory and tested for a
variety of physical parameters. These test methods are described below.
ASTM D422-63: Particle Size Analysis -- The particle-size distribution of the untreated waste
was determined by combined sieve and hydrometer analysis. A sieve analysis was performed on
that fraction of each sample larger than 0.074 mm (retained on the No. 200 sieve). The sieve
51
-------
analysis consisted of passing a sample through a set of sieves and weighing the portion of material
retained on each sieve. Hydrometer analysis was performed on the finer fraction (less than 0.074
mm). The hydrometer analysis is based on Stoke's Law and involves preparing a dilute
suspension of fine particles in water, measuring the specific gravity of the suspension at specified
time intervals, and correlating settling velocity, particle diameter, and time to determine
particle-size distribution.
ASTM D2216-80: Water Content, Untreated Waste ~ Water content is defined as the ratio of
the weight of water retained by a solid to the weight of solids, expressed as percent. ASTM
Method D2216-80 was used to determine the water content of untreated waste. Moisture was
determined on a dry-weight basis by measuring the mass of water removed by drying the sample
to a constant mass at 110° ± 5°C.
TMSWC-4: Water Content, Treated Waste — TMSWC-4 was used to determine the water
content of treated waste. The sample was ground to pass through an ASTM No. 10 sieve. The
sample mass was measured before and after it was dried in an oven maintained at 60° ± 3°C. The
dry weight must be a constant weight (mass change of less than 0.03 grams in 4 hours).
ASA-13-2: Bulk Density, Untreated Waste — The bulk density of untreated waste was
determined using the ASA-13-2 Core Method (American Society of Agronomy). A cylindrical
metal sampler was pressed or driven into the soil to the desired depth and removed to preserve a
known volume of sample as it existed in-situ. Bulk density was calculated based on a soil sample
of known volume and its mass.
TMSWC-2: Bulk Density, Treated Waste — The bulk density of a treated waste was determined
using TMSWC-2. This test was performed after the sample cured. The bulk density was
determined by weighing a cylinder of the treated waste, measuring the dimensions of the cube or
cylinder, and dividing the volume into the mass.
TMSWC-13: Permeability (Falling Head) ~ The permeability test for solidified waste requires a
sample 7.62 centimeters (3 inches) in diameter and 7.62 centimeters high. Permeability was
determined using a triaxial cell and measuring changes of water volume over time under
controlled temperature and pressure. A permeability coefficient was calculated based on the
linear rate of flow of a fluid through a material under a hydraulic gradient of unity.
ASTM D1633: Unconfined Compressive Strength (UCS) — The UCS characteristics of molded
treated waste cylinders were determined using strain-controlled application of an axial load. UCS
52
-------
is defined as the load per unit area, expressed as pounds per square inch (psi), at which an
unconfined cylindrical sample of solids will fail a compression test.
TMSWC-12: Wet/Dry Weathering Test — This test was performed using two 4.5 centimeter
(cm) diameter x 7.4 cm high specimens of solidified waste. One of the specimens was the test
sample, the other was the control. Each sample was removed from its mold, placed in a tared
beaker, and weighed. The control was placed in a humidity chamber maintained at 22 ± 3°C,
while the test specimen was dried in a vacuum oven at 60 ± 3°C for 24 hours. The dried
specimen was cooled to room temperature in a desiccator. Then 230 mL of water was added to
each of the sample beakers. Both samples are placed in the humidity chamber for 24 hours. The
samples were then sprayed with distilled water to remove loosely attached particles from the
specimens. The specimens were transferred to two, new tared beakers. The original beakers
were placed in the oven to evaporate the water and dry them to a constant weight. This was
repeated 11 times, or until the specimen lost its physical integrity, with the weight loss being
recorded each time. The corrected relative weight loss of the test specimen was obtained by
subtracting the relative weight loss of the control from the relative weight loss of the sample.
TMSWC-I1: Freeze/Thaw Weathering Test — This test was performed on two 4.5 cm diameter
x 7.4 cm high specimens of solidified waste. One of these specimens was used as a control. Each
sample was removed from its mold, placed in a tared beaker, and weighed. The control was
placed in a humidity chamber maintained at 22 + 3°C, while the test specimen was placed in a
freezer at -20 ± 3°C for 24 hours. The specimens were removed from the freezer and moisture
chamber and 230 mL of distilled water was added to each beaker. Both beakers were placed in
the moisture chamber for 24 hours. The samples were then sprayed with distilled water to
remove loosely attached particles from the specimens. The specimens were transferred to two,
new tared beakers. The original beakers were placed in an oven to evaporate the water and dry
them to a constant weight. This procedure was repeated 11 times, or until the sample lost its
physical integrity, with the weight loss being recorded each time. The corrected relative weight
loss of the test specimen was obtained by subtracting the relative weight loss of the control from
the relative weight loss of the sample.
5.6
CHEMICAL TESTS
Chemical tests, including actual chemical analyses, and tests for chemical properties were
performed on the untreated and treated waste samples collected during the Soliditech
demonstration. The untreated wastes, reagent mix/control, treated wastes, and resultant leachates
were analyzed for organic and inorganic constituents. The sample preparation and analytical
procedures are summarized below.
53
-------
SW-846 Method 9045: pH-Soil/Solid — Equal weights of the solid and laboratory pure water
were mixed to form a slurry and allowed to settle for 1 hour. The pH of the supernatant was
measured electrometrically using a combination pH electrode. For calcareous waste, the
laboratory pure water was replaced by a calcium chloride solution (0.01 M).
SW-846 Method 9040: pH-Aqueous —• The pH of aqueous samples or leachates was measured
electrometrically using a combination pH electrode.
SW-846 Modified Method 9045: Oxidation-Reduction Potential (Eh), Soil/Solid —
A solid/water slurry was prepared as in Method 9045. The redox potential for the supernatant
was measured electrometrically using a combination oxidation-reduction electrode.
ASTM D1498-76 Oxidation-Reduction Potential (Eh), Aqueous — The oxidation-reduction
potential of an aqueous solution was measured electrometrically using a combination
oxidation-reduction electrode.
U.S. EPA 160.1: Residue, Filterable (Total Dissolved Solids, TDS) — A well-mixed leachate
aliquot was filtered through a standard glass fiber filter. The filtrate was collected in a tared
beaker, evaporated, and dried to a constant weight at 180°C.
TMSWC-7: Acid Neutralization Capacity — A 150-gram sample of the untreated waste, reagent
mix/control, or cured solidified waste was dried to a constant weight at 60 + 3°C. The sample was
then ground to pass an ASTM No. 100 sieve. Ten-gram aliquots of the sample were added to a
series of 10 centrifuge tubes. Distilled water and 2 normal nitric acid were added to each tube in
volumes that resulted in 10 different extraction fluids. The samples were shaken and then placed
on a rotary extractor for 48 hours. The samples were then centrifuged. The pH of each
supernate was measured and recorded. This method did not allow a complete titration of the
post-treatment samples to acidic pH. The neutralization potential (expressed as percent CaCO3)
was determined by titrating a 2.Q gram aliquot of each post-treatment sample with 0.5 N HCI
(U.S. EPA, 1978).
U.S. EPA 600 Method 415.1: Total Organic Carbon (TOC) — An aliquot of the leachate was
acidified with sulfuric acid to a pH of less than 2. An inert gas was bubbled through the sample
to drive off the carbonates. Organic carbon in the sample was then converted to carbon dioxide
by catalytic combustion. The carbon dioxide was measured directly by an infrared detector.
TCLP and EP leachate were not analyzed for TOC. These leachates contain high acetate
concentration that would adversely affect TOC data interpretation.
54
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ASTM C114: Loss on Ignition — The loss on ignition method is a technique for determining the
total moisture and carbon content of a cementitious solid. A sample was ignited at a temperature
of 950°C for 15 minutes. The percent of weight lost was calculated based on the weight of the
original sample. A correction factor was applied when the sample contained a substantial
quantity of sulfide.
U.S. EPA 600 Method 413.2: Oil and Grease — The oil and grease in the untreated and
solidified wastes were extracted by sonication using a modified SW-846 Method 3550. Five
grams of the solid was added to 25 milliliters (mL) of freon and sonicated. The leachates were
acidified with hydrochloric acid to a pH of less than 2 and extracted with multiple aliquots of
freon in a separatory funnel. The extract was then taken up to 100 mL with freon. The oil and
grease in the extracts were then determined by infrared spectroscopy.
SW-846 Method 8240: Volatile Organic Compounds (VOCs) — Method 8240 in SW-846 is a gas
chromatography-mass spectrometry (GC/MS) procedure used to determine the concentration of
VOCs, having a boiling point below 200°C, in solid and liquid samples. Solid samples were
prepared by placing 5 grams of the solid in 10 milliliters of methanol. An inert gas was bubbled
through a solution containing an aliquot of the sample, at ambient temperatures. The VOCs were
transferred from the aqueous phase to the vapor phase. The vapor was swept through a sorbent
column, and the VOCs were absorbed. After purging was completed, the sorbent column was
heated and backflushed with inert gas to desorb the components onto a gas chromatography
column. The VOCs were separated by GC and detected by MS.
SW-846: Semivolatile Organic Compounds (SVOCs) — Several methods were used for SVOC
analyses, based on the form of the waste - soil, sludge, or leachate. The following describes
standard U.S. EPA methods, from SW-846, for extraction and analysis of SVOCs.
1. Method 3520 is a procedure for isolating organic compounds from aqueous
samples. A measured volume of sample was extracted with methylene chloride
using a continuous liquid-liquid extractor. The extract was dried, concentrated,
and, as necessary, exchanged into a solvent compatible with the cleanup or
determinative step to be used.
2. Method 3540 is a procedure for extracting SVOCs from solids such as soils,
sludges, and wastes. The solid sample was mixed with anhydrous sodium sulfate,
placed in an extraction thimble, and extracted using an appropriate solvent in a
Soxhlet extractor. The extract was then dried, concentrated, and, as necessary,
exchanged with a solvent compatible with the cleanup or determinative step being
employed.
3. Method 3611 is a procedure for the cleanup of petroleum wastes from sample
extracts. The cleanup column is packed with alumina, topped with a water
55
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absorbent, and then loaded with the sample. A suitable solvent was used to elute
the analytes while leaving the interfering compounds on the column. The eluent
was then concentrated and submitted for analyses.
4. Method 8270 is a capillary column procedure used to determine the concentration
of SVOCs in sample extracts. Method 8270 was used to quantify most SVOCs that
were soluble in methylene chloride, including polynuclear aromatic hydrocarbons,
chlorinated hydrocarbons and pesticides, phthalate esters, organophosphate esters,
nitrosamine, haloethers, aldehydes, ethers, ketones, anilines, pyridines, quinolines,
aromatic nitro compounds, and phenols.
SW-846: Polychlorinated Biphenyls (PCBs) ~ Several methods were used for PCB analyses,
based on the form of the waste ~ soil, sludge, or leachate. The following describes standard U.S.
EPA methods, from SW-846, for PCB extraction, screening, and analysis.
1. Method 3520 is a procedure for isolating organic compounds from aqueous
samples. A measured volume of sample was extracted with methylene chloride
using a continuous liquid-liquid extractor. The extract was dried, concentrated,
and, as necessary, exchanged into a solvent compatible with the cleanup or
determinative step to be used.
2. Method 3540 is a procedure for extracting SVOCs from solids such as soils,
sludges, and wastes. The solid sample was mixed with anhydrous sodium sulfate,
placed in an extraction thimble, and extracted using an appropriate solvent in a
Soxhlet extractor. The extract was then dried, concentrated, and, as necessary,
exchanged with a solvent compatible with the cleanup or determinative step being
employed.
3. Method 3550 was used to extract SVOCs from the post-treatment waste to allow
easier access to the samples when pH adjusting to retrieve the acid compounds.
The samples were strongly alkaline and required close observation to maintain the
pH required. A 30-gram sample was mixed with anhydrous sodium sulfate. This
mixture was extracted three times using sonication. The extract was separated
from the sample by centrifugation, and then submitted for cleanup. This method
could not be performed on the reagent mix samples because of the excessive
alkalinity of these samples.
4. Method 3620 is a procedure for the cleanup of sample extracts. The cleanup
column was packed with Florisil®, topped with a water absorbent, and then loaded
with the sample. A suitable solvent was used to elute the analytes of interest while
leaving the interfering compounds on the column. The eluent was then
concentrated and submitted for analyses or further cleanup.
5. Method 3630 is another procedure for the cleanup of sample extracts. This
cleanup procedure was applied to the solid sample extracts after they underwent
Florisil* cleanup. This procedure was used to remove pentachlorophenol from the
extracts to be analyzed for PCBs. Pentachlorophenol was found to be present and
to cause interferences in the analysis of PCBs in the preliminary samples. The
cleanup column was packed with silica gel adsorbent, topped with water
absorbent, then loaded with the sample extract. A suitable solvent was used to
elute the analytes of interest while leaving the interfering compounds on the
column. The eluent was then concentrated and submitted for analyses.
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Method 8080 specifies gas chromatographic conditions for detecting PCBs.
Samples were injected jnto the GC column. Compounds in the GC column
effluent were detected by an ECD.
Method 680 covers pesticides and PCBs in waters, soils, and sediments by GC/MS.
It is applicable to samples containing single PCB congeners or to samples
containing complex mixtures, such as Aroclors. PCBs were identified and
measured as isomer groups by levels of chlorination.
Method 680 is designated as a backup for Method 8080 to quantify PCB congeners
in aqueous extracts. Unfortunately, there is no clear protocol for determining
when Method 680 can effectively be used as a backup to Method 8080. The steps
to be followed consist of analyzing an aqueous extract by Method 8080. If no
Aroclor patterns are identified, the chromatogram is visually inspected to
determine the presence of peaks that are suspected of being PCB congeners.
Because the response factor cannot be easily established for peaks by GC analysis,
the best judgment of the analyst is used to determine whether Method 680 should
be employed. It was not necessary to use this method for the Soliditech
demonstration.
SW-846: Metals — Several methods were used for metals analyses, based on the type of metal
and the form of waste — solid, sludge, or leachate. The following describes standard U.S. EPA
methods from SW 846 for digestion and analysis of metals. The appropriate digestion and
analytical procedures for metals are presented in Table 12.
1. Method 3050 is an acid digestion procedure used to prepare sediments, sludges,
and soil samples for analysis by flame or furnace atomic absorption spectroscopy
(AAS) or inductively coupled plasma emission spectroscopy (ICP). A
representative sample was mixed with nitric acid (HNO3) and refluxed. Hydrogen
peroxide (H?O2) was then added to the digestate with gentle heating. If the
sample was being prepared for graphite furnace AAS analyses, then the digestate
was filtered and brought to volume with deionized water. If the sample was being
prepared for ICP analysis, then hydrochloric acid (HC1) was added to the
digestate. After gentle heating, the digestate was filtered and brought up to
volume with deionized water.
2. Method 3010 is a digestion procedure used to prepare aqueous samples for analysis
by flame AAS and ICP. The sample was mixed with HNO, and allowed to reflux
in a covered Griffin beaker, followed by hydrochloric acidto dissolve any
precipitate or residue resulting from evaporation. The sample was then filtered
and brought up to volume using deionized water.
3. Method 3020 is a digestion procedure used to prepare aqueous samples for lead
and thallium analysis by graphite furnace AAS. The sample was mixed with
HNO3 and allowed to reflux in a covered Griffin beaker. A small volume of
deionized water was added with continued warming to dissolve any residue
resulting from evaporation. The digestate was then reconstituted with deionized
water.
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TABLE 12
DIGESTION AND ANALYTICAL TECHNIQUES
FOR ELEMENTAL ANALYSIS
Analvte
Sb, As, Be, Cd, Cr,
Cu, Pb, Ni, Se, Ag, Tl,
Zn, Na
Sb, Be, Cd, Cr, Cu,
Ni, Ag, Zn, Na
Pb, Tl
As, Se
Sb, Be, Cr, Cu, Ni,
Ag, Zn, Pb, Na
As
Pb
Se
Tl
Hg
Hg
Notes:
D = Digestion
A » Analytical
D
D
A
A
A
A
A
D& A
D& A
Technique
D
D
D
D
A
A
A
A
A
D& A
D& A
Matrix Tvoe
Solid
Leachate
Leachate
Leachate
Solid/Leachate 60 10
Solid/Leachate 7060
Leachate
Solid/Leachate 7740
Solid/Leachate 7841
Leachate
Solid
Method Number
3050
3010
3020
7060/7740
7421
7470
7471
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4. Methods 7060 and 7740 describe the digestion procedure used to prepare aqueous
samples for arsenic and selenium analysis by graphite furnace AAS. The sample
was mixed with hydrogen peroxide and nitric acid and allowed to reflux in a
covered Griffin beaker for one hour. The sample was then brought back to
volume using deionized water.
5. Method 6010 describes the simultaneous, or sequential, determination of elements
using ICP. The method measures element-emitted light by optical spectrometry,
Samples are nebulized and the resulting aerosol is transported to the plasma torch.
Element specific atomic-line emission spectra are produced, dispersed by a grating
spectrometer and monitored for intensity by photomultiplier tubes.
6. Methods 7060, 7421, 7740, and 7841 are graphite furnace AAS methods for
determining arsenic, lead, selenium, and thallium, respectively. Following sample
digestion, an aliquot of sample was placed in a graphite tube in the furnace,
evaporated to dryness, charred, and atomized. The materials analyzed were then
placed in the light path of an atomic absorption spectrophotometer.
7. Method 7470 is a cold-vapor atomic absorption (CVAAS) procedure for
determining the concentration of mercury in mobility-procedure extracts. Method
7471 is prescribed for solid and sludge-type wastes. A sample aliquot was
acidified. Potassium permanganate was added to maintain oxidizing conditions.
Potassium persulfate was added, and the sample was heated in a water bath. After
cooling, mercury in the sample was reduced to the elemental state (with the
addition of hydroxylamine hydrochloride and stannous sulfate) and aerated from
solution in a closed system. The mercury vapor passed through a cell positioned in
the light path of an atomic absorption spectrophotometer.
Please note that digestion Methods 3010 and 3050 do not contain antimony (Sb) or silver
(Ag) in their target analyte list. The sample matrices to be analyzed are leachate, soils, and solids
and are not covered by the methods listed for these elements (SW-846 Methods 3005 and 7040).
Radian maintained laboratory control charts that show that the average blank spike recoveries for
Ag and Sb using Methods 3010 and 3050 in their laboratories were within recovery limits. The
median recoveries are 90 percent for both Ag and Sb. Methods 3010 and 3050 were acceptable
and were used to digest leachate, soil and solid samples for Ag and Sb.
5.7
LEACHING TESTS
Leaching/extraction were performed on untreated and treated waste samples collected
during the Soliditech demonstration. These tests were performed using both destructive methods
(TCLP, EP Toxicity, and BET) and non-destructive methods (ANS 16.1 and WILT). Destructive
methods crush or grind the samples prior to testing destroying the physical integrity of the
solidified waste samples. Non-destructive methods were applied to intact cast cylinders. The
procedures are briefly summarized below.
Federal Register. 1986: Toxicity Characteristics Leaching Procedure (TCLP) Test — The TCLP
test was designed to determine the mobility of both organic and inorganic contaminants present
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in liquid, solid, and multiphasic wastes. The sample was prepared by crushing the waste. The
leaching procedure involved a solid-to-liquid ratio of 1:20, maintained at a specified pH that was
agitated in a rotary extractor for 18 + 2 hours, and filtered through a 0.6-mm to 0.8-mm glass
fiber filter. The pH and type of leaching medium used depend on the alkalinity of the solid
phase of the waste. Preparing treated waste samples for the TCLP extraction of VOCs was a
critical concern. A validated laboratory procedure for preparing these samples was not available.
Special care was taken to minimize the chance for VOC releases into the atmosphere. The sample
was placed in the zero headspace extractor (ZHE) immediately after pulverization.
U.S. EPA Method 1310: EP Toxicity Test ~ The extraction procedure (EP) toxicity test is used
to determine whether a waste exhibits the RCRA characteristic of toxicity. This test may also be
used to simulate the leaching' that a waste would undergo in a sanitary landfill. The sample was
prepared by crushing it to pass through a 9.5 mm sieve. A single batch of material was extracted
at a solid-to-liquid ratio of 1:20. The extract was maintained at pH 5.9 + 0.2, using 0.5 normal
acetic acid, and stirred or tumbled for 24 hours. The extract was filtered through a 0.45
membrane filter. The leachate was analyzed for the standard list of EP parameters using
appropriate analytical methods.
C6t6, 1988: Batch Extraction Test (BET) — The BET is a modification of TMSWC-6,
developed by Dr. P. Cote of the Wastewater Technology Center and Alberta Environmental
Center (C6te, 1988). After the 28-day curing period, the treated waste was crushed to pass an
ASTM No. 100 sieve and the water content was determined. Samples of three solid-to-liquid
ratios (1:4, 1:20, and 1:100) were prepared for each treated waste. The samples were extracted on
a rotary extractor for 7 days. The total dissolved solids and the soluble fraction of waste were
determined on the 4:1 liquid-to-solid extract. The pH of each extract was measured, the sample
filtered, and the resulting leachate submitted for chemical analyses.
American Nuclear Society: 16.1 Test (ANS 16.1) — The 28-day modification of ANS 16.1 for
solidified wastes was used to approximate leaching from intact (not crushed) solidified waste by
rapidly flowing ground water. Samples were leached without agitation using demineralized water.
The demineralized water had an electrical conductivity less than 5 /imho/cm at 25°C, and a total
organic carbon concentration of less than 3 milligrams per liter. The samples were totally
submerged in the water for a specified test period, then the leachate was collected and set aside
for analyses. The sample was then re-extracted in another aliquot of demineralized water. This
cycle was repeated until five leachates were obtained for each sample.
Jackson, 1988: Waste Interface Leaching Test (WILT) — The WILT was designed to evaluate
the long-term leaching behavior of intact (not crushed) solidified waste. Two sizes of cores (3-
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inch diameter by 18-inch length, and 6-inch diameter by 18-inch length) of the treated wastes
were prepared in triplicate. Each of these cores was placed into individual leaching columns, and
the annular space between the core and container was filled with acid-washed sand. A 1-inch
layer of acid-washed sand was added to the top of the columns to disperse the leaching fluid
uniformly over the cross-sectional area of the treated waste.
A 0.25-inch diameter tygon tube was connected to the hose-bib at the base of each
column with the opposite end fitted to a three-way stopcock. A second tygon tube was
connected to the stopcock and a fitting on sealed Tedlar* bags. This arrangement allows leachate
from the columns to flow into the Tedlar* bags and facilitates sampling of leachate in the bags
without exposing it to the atmosphere.
Leaching fluid (distilled water) was supplied through the bottom of each column through
tubing connected to a water reservoir. Deionized water was added to fully saturate each column
to the surface level of the sand packing. The columns remained saturated until leachate was
collected at predetermined biweekly or monthly intervals. Biweekly leachate collection and
analysis was performed for a period of 2 months, followed by biweekly leachate collection with
monthly leachate analysis for 4 additional months. After six months, leachates will continue to
be collected biweekly but will be analyzed every other month.
5.8
QUALITY ASSURANCE AND QUALITY CONTROL SUMMARY
The Soliditech Demonstration Plan included a Quality Assurance Project Plan (QAPP) that
detailed quality assurance and quality control (QA/QC) procedures for the demonstration
sampling and analysis activities. These QA/QC procedures included the following:
• QC Check Samples — Standard samples of known analyte concentrations.
• Laboratory Blank Samples ~ The laboratory analyzed calibration or reagent
blanks at the beginning of each analytical run and every 10 samples thereafter.
Calibration blanks consisted of deionized water and were not taken through any
sample preparation steps. Reagent blanks consisted of deionized (or organic-free)
water taken through all sample preparation steps, including adding reagent and
digestion/extraction procedures.
• Calibration Check Compounds — Standards used for ongoing calibration
verification.
• Spiked Samples — A small subset of the samples were spiked with known
concentrations of either reference materials or surrogate standards and taken
through the sample preparation process. Spiked samples allowed the laboratory to
assess the efficiency of extraction processes, the accuracy of the analyses, and
possible matrix effects.
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• Duplicate samples — These samples were analyzed at a 10 percent frequency.
Duplicate sample analyses provided a measure of sample variability.
Replicate samples — Sample extracts, digestates, or leachates were analyzed in
replicate at a 10 percent frequency. Replicate sample analyses provided a measure
of analytical variability.
U.S. EPA performed both a field audit during the demonstration and a laboratory audit to
ensure that all QA/QC procedures were being followed. Both audits found the sampling and
analysis activities satisfactory.
Overall, the quality control results for the Soliditech program were excellent. A few
problems were noted and are listed below:
• Recoveries of matrix spike were outside of the acceptance criteria for selenium
and thallium for both pre- and post-treatment matrices.
• Holding times were exceeded for the extraction of pre-treatment TCLP leachates
analyzed for VOCs by Method 8240.
Poor recoveries were recorded for Method 8270 acid fraction matrix spike and
surrogate compounds for post-treatment samples.
These problems are discussed in detail in Appendix B.
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6.0 FIELD ACTIVITIES
The Soliditech demonstration field activities consisted of the collection of waste materials,
the treatment of the waste materials, and the discharge and sampling of the treated waste.
Section 6.1 discusses collection, Section 6.2 discusses treatment, and Section 6.3 discusses
sampling. The chronology of the major demonstration events is shown in Table 13.
6.1
WASTE MATERIAL COLLECTION
Waste material was collected from three areas of the Imperial Oil Company/Champion
Chemical Company Superfund site. These areas were identified as the abandoned storage tank,
the waste pile, and Off-Site Area One. The locations of these areas are shown in Figures 2 and 3.
6.1.1
Summary of Operations
This section details the waste material collection from each of the three areas previously
chosen for treatment.
Abandoned storage tank. A catch basin was excavated next to the tank manhole and
lined with plastic sheeting to contain any releases of waste. The manhole located in the side of
the tank was then opened, and the oily sludge in the tank was removed by bucket from the tank
and placed in 55-gallon drums. Three full drums of this material were collected, sealed,
weighed, and staged for later treatment. Due to the liquid nature of this waste material,
Soliditech blended the oily waste material from this tank with solid filter cake material from the
waste pile. This blending was performed in the mixer immediately prior to treatment.
Waste Pile. Three 55-gallon drums were filled with filter cake material from the waste
pile, using a backhoe. These drums were weighed to obtain the density of this waste and the
results used to calibrate the bucket of the front-end loader for subsequent transfer of this waste
to the mixer. Once the front-end loader was calibrated, the filter cake material was collected
from the exposed face of the waste pile and directly transferred by the front-end loader into the
Soliditech mixer, through a 4-inch by 4-inch screen welded to the top of the large mixer. Figure
5 shows the 4-inch by 4-inch mesh screen on top of the mixer that was used to remove large
debris from the waste material prior to treatment. No attempts were made to collect this material
from the most contaminated areas of the waste pile.
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TABLE 13
SOLIDITECH DEMONSTRATION CHRONOLOGY
Site Preparation
Obtain sampling and analysis equipment
Establish health and safety zones
Office trailer set-up
Setup decontamination areas
Accommodation of Soliditech equipment
Preparation for visitor's day
Waste collection
Visitor's day
December 1 and 2, 1988
December 2, 1988
December 2 and 5, 1988
December 5 and 6, 1988
December 5 and 6, 1988
December 6, 1988
December 6 and 7, 1988
December 7, 1988
Operations
Arrival of Soliditech equipment
Set-up of the Soliditech equipment
Waste material collection
Off-Site Area One
Filter cake/oily'sludge
Filter cake
Pretreatment sample collection
Off-Site Area One
Filter cake/oily sludge
Filter cake
Waste treatment and post-treatment sampling
Reagent mix/control run
Filter cake/oily sludge
Filter cake
Off-Site Area One
Clean-up activities
December 3, 1988
December 5 and 6, 1988
December 6, 1988
December 6 and 7, 1988
December 7, 1988
December 5, 1988
December 7, 1988
December 7, 1988
December 6, 1988
December 7, 1988
December 7, 1988
December 8, 1988
December 8 through 14, 1988
Sample Collection and Preparation of Long-Term Monitoring Area
Collection of treated waste samples January 9, 1989
Removal of forms from treated
waste monoliths January 9, 1989
Placement of monoliths in long-term
monitoring location January 10, 1989
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FIGURE 5
WASTE CONTAINED IN 10-CUBIC-YARD SOLIDITECH MIXER
-------
Off-Site Area One. Contaminated soil from Off-Site Area One was collected by means
of a backhoe. During collection large pieces of earth and roots were removed. The soil was
placed in the bucket of a tracked front-end loader and transported to a nearby dump truck. The
dump truck gate was sealed with caulking and its bed was lined with two layers of 8-mil
polyethylene. The truck was equipped with a bed cover. When the contaminated soil was
transferred to the dump truck, the soil in the truck bed was covered with the two sheets of
polyethylene, the bed of the truck was covered, and the truck was driven to a scale where it was
weighed. The truck was then driven to the treatment area where it remained overnight. Prior to
treatment, the contaminated soil, still wrapped in polyethylene, was deposited next to the
Soliditech mixer. Prior to treatment this soil was transferred to the mixer via a front-end loader,
and passed through the 4-inch by 4-inch screen welded to the top of the mixer to remove any
large pieces of debris.
6.1.2
Deviations from the Demonstration Plan
The amount of Off-Site Area One soil collected was approximately 57 percent of the
amount planned, because the equipment operator overestimated the amount of contaminated soil
that he collected. The discrepancy was not discovered until the contaminated soil was weighed
and found to be three- to four-cubic-yards less than planned. Soliditech adjusted its treatment
formulation based upon the weight of waste that was loaded in the mixer.
6.2
WASTE TREATMENT
Both mixers were scraped and steam-cleaned prior to use. During each test run, the
contaminated waste material (or clean sand for the control run) was first placed in the Soliditech
mixer. As mentioned in Section 6.1.1, the waste pile material and Off-Site Area One soil were
first screened through a 4-inch by 4-inch screen to remove any rocks, roots, or other large
debris. The oily sludge and the sand for the control run did not require screening. Next,
predetermined amounts of Urrichem reagent, water, and proprietary additives were blended with
the contaminated waste. Finally, a predetermined amount of Type II Portland cement was added,
using the front-end loader with a calibrated bucket, and treatment commenced. Figure 5 shows
the addition of cement to the large Soliditech mixer. During the treatment process, mixing was
continually evaluated by Soliditech personnel.
After approximately 40 to 60 minutes, when Soliditech personnel determined that each
batch was adequately mixed, the slurry was discharged from the mixer into the reinforced one-
cubic yard plywood forms. When one form was filled, it was removed by a forklift and another
66
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empty form moved into place and filled. This process continued until the mixer was emptied.
Figure 6 shows the demonstration in progress, with the large Soliditech mixer discharging into a
plywood form. (The small Soliditech mixer can be seen on to the right of the photograph on the
truck bed, the Soliditech cement storage hopper can be seen to the left of the photograph, and the
waste pile can be seen in the center of the photograph behind the large Soliditech mixer.)
The treated waste in one form from each of the four test runs was allowed to cure indoors
at a temperature of approximately 50 to 70°F for 24 hours (see Section 6.3.2). All other treated
waste cured outdoors at ambient temperatures (25 to 40°F). All treated waste in the plywood
forms completed the prescribed 28-day cure in an unheated warehouse. Although 11 of the
blocks of treated waste were allowed to cure outdoors, at times when temperatures were below
freezing, the treated waste had already hardened prior to being subjected to sub-freezing
temperatures.
After completion of the curing time, the treated waste was removed from the warehouse,
the plywood sides of the forms were removed, the treated waste was organized into a stack and
the stack was wrapped in 40 mil high-density polyethylene (HDPE) film. The stack will remain
on site for long-term study and observation.
6.2.1
Summary of Test Runs
The first test run was performed on a batch of clean sand rather than contaminated waste
material. This test run was used as a control run and is referred to as the reagent mix or control
test run. Due to the small amount (800 pounds) of sand being solidified during this run, the
smaller of the two Soliditech mixers was used. The sand was dumped directly into the Soliditech
mixer from the sand bags. As detailed above, water, reagent, proprietary additives, and cement
were added and thoroughly mixed with the sand. The mixture was blended for approximately 40
minutes.
The second test run was performed on the mixture of oily sludge and filter cake material,
blended at one part oily sludge to two parts waste filter cake material. Approximately 2 cubic-
yards of this waste were treated. Once the two wastes were thoroughly mixed in the large
Soliditech mixer, water, reagent, proprietary additives, and cement were added and thoroughly
mixed with the waste. This mixture was blended for approximately 45 minutes.
The third test run was performed on the same filter cake material but without the
addition of oily sludge. Approximately 5 cubic-yards of this waste were treated. Once the waste
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FIGURE 6
DISCHARGING OF TREATED WASTE INTO PLYWOOD FORMS
-------
was added to the large Soliditech mixer,-water, reagent/proprietary additives, and cement were
added and thoroughly mixed with the waste. This mixture was blended for approximately 45
minutes.
The fourth test run was performed on the Off-Site Area One soil. Approximately 4
cubic-yards of this waste were treated. Once the waste was added to the large Soliditech mixer,
water, reagent, proprietary additives, and cement were added and thoroughly mixed with the
waste. This mixture was blended for approximately one hour.
6.2.2
Deviations from the Demonstration Plan
Overall, the waste treatment phase of the demonstration was considered to be a success.
There were several deviations from the Demonstration Plan. These deviations are discussed
below.
In the first test run of waste material (filter cake/oily sludge mixture), material was
trapped at one end of the mixer and not completely blended. This was discovered as the treated
waste was discharged from the mixer. This was probably due to lack of operator experience with
the mixer and with this waste type. It could have been remedied by more vigorous end-to-end
agitation of the mixer. Since the trapped material was present in the solidified matrix, it will be
evaluated with the samples from this run.
The waste treatment test runs were performed in a different order than originally
planned. The reagent mix (clean sand and all Soliditech's reagent and proprietary additives) was
treated first, as planned. Due to the late arrival of the front-end loader required to collect the
Off-Site Area One soil, the mixture of oily sludge and filter cake material was treated second,
rather than last. The filter cake material was treated third, as planned, and the Off-Site Area
One soil was treated last. This change was inconsequential and did not affect other operating
plans.
The large Soliditech mixer, although cleaned prior to the SITE demonstration, contained
some residual material. Soliditech personnel scraped as much of this material out of the mixer as
possible and then steam cleaned the mixer prior to its use for the demonstration. A sample of the
material scraped from the mixer was collected and chemically analyzed to determine whether it
could contaminate the demonstration samples. From these results it was determined that any
residual material could not have contributed to the contamination found in the treated waste.
These analytical results are presented in Appendix A.
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After treatment of the filter cake/oily sludge mixture, the large Soliditech mixer was
scraped and steam-cleaned, as specified in the Demonstration Plan. After treatment of the filter
cake material alone, however, it was determined that it was not necessary to thoroughly clean the
mixer, since the contaminated Off-Site Area One soil that was to be treated next would be
sampled directly from the mixer. Any residual material from the previous batch would be thus
mixed with the soil, sampled, and treated as part of the contaminated soil. This procedure was
more representative of actual conditions, when, to save operating time, the mixer would not be
cleaned between each batch.
6.3
SAMPLING FOR PROCESS EVALUATION
To evaluate the Soliditech process, samples of waste material were collected before and
after treatment. These samples were analyzed by chemical and physical tests and were exposed to
various extraction liquids in five separate leaching tests. The liquid extracts from these leaching
tests were chemically analyzed. A reagent mix or control test run was also performed, using
clean sand in place of the waste material.
6.3.1
Pretreatment Sampling Procedures
Prior to each test run, samples of each waste material were collected, in triplicate, in glass
jars or Shelby tubes. Shelby tube samples for bulk density determinations on the solid waste
materials were collected from the actual location of the waste material prior to waste collection.
All pretreatment samples from filter cake/oily sludge mixture, including the bulk density
samples, were collected in glass jars directly from the mixer after blending but prior to treatment.
All pretreatment samples from the waste pile were collected from several locations in the waste
pile, which was considered to be uniform in composition. With the exception of the bulk density
samples, all pretreatment samples of the Off-Site Area One soil were collected from the mixer
after blending. This was considered important due to the non-homogeneous nature of this soil.
6.3.2
Post-Treatment Sampling Procedures
Samples of treated waste to be used for testing and analysis were taken from each of the
first, second, and third cubic-yard forms immediately after they were filled with the treated
waste slurry. These samples were collected by a long-handled scoop and transferred to
cylindrical waxed cardboard molds, PVC molds, or other previously designated sample containers.
The molds were individually labeled, placed in open storage containers, covered with plastic
sheeting, and allowed to cure for 28 days in a heated building (approximately 50 to 70 °F) at the
70
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site. Figure 7 shows the samples of treated waste material in the cylindrical molds immediately
after collection,
Some of the treated waste slurry was also used for field testing. The results of these tests
are reported in Appendix D.
A single one-cubic-yard mold from each of the four batches (reagent mix with sand and
three batches of solidified waste) was allowed to cure for the first 24 hours after mixing in a
heated (approximately 50 to 70 °F) building. The remaining molds cured at ambient outdoor
temperatures (approximately 25 to 40 °F). After one to three days outdoors, all cubic-yard molds
were transferred to a non-heated warehouse for the remainder of the curing period.
After the curing period the samples to be used for testing and analyses were removed
from the heated building at the site and transported to the analytical laboratory for analyses.
The field demonstration of the Soliditech SITE technology produced 14 large monoliths,
initially contained within one-cubic-yard plywood molds. A permanent brass marker, with the
block number stamped on it, was imbedded in the top corner of each block before the material
had completely hardened. For purposes of describing specific features of each block, this marker
is defined as resting on the Northwest corner. The wastes contained within each square mold
were:
No. 1
No. 2,3,4
No. 5,6,7,8,9,10
No. 11,12,13,14
Clean sand plus Soliditech reagent and proprietary additives
Mixture of waste pile filter cake and oily sludge
Waste pile filter cake material
Off-Site Area One contaminated soil
The material in Mold Nos. 1, 3, 7, 12 were placed inside a heated warehouse at 50 to 70
°F to cure overnight, since the temperature was slightly below freezing at night during the week
of the field demonstration.
After 28 days, the sides of the plywood mold forms were removed from each monolith.
Loose fragments were chipped off the edges of each cubical block. The treated waste monolith
blocks were then placed in a compact stack for long-term monitoring. Figures 8 and 9 depict the
placement of the blocks.
71
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FIGURE 7
SAMPLES OF TREATED WASTE IN CYLINDRICAL MOLDS
-------
FIGURE 8
LARGE MONOLITHS OF TREATED WASTE BEING PREPARED FOR LONG-TERM STUDY
-------
FIGURE 9
STACKING DIAGRAM OF THE
TREATED WASTE MONOLITHS
9
11
12
3
Bottom Tier
(Plan View)
74
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The stack was placed on a double-thickness of 40-mil HOPE, wrapped up the sides of the
stack to contain any liquid that might seep from the blocks. The stack was covered with a sheet
of 40-mil HOPE to divert precipitation from the blocks. The stack cover was not made airtight;
therefore, temperature and humidity influence on the solidified waste material may have some
long-term effect.
As the plywood side forms of the treated waste monoliths were removed and the blocks
were placed on the stack, initial observations were recorded. Long-term evaluation of the treated
waste monoliths will examine:
• Surface spalling
Grain exfoliation
• Crack and fissure development
Oxidative discoloration
• Salt efflorescence
Pore characterization
6.3.3
Sampling Deviations
Pretreatment samples of the filter cake and the Off-Site Area One waste material were,
according to the Demonstration Plan, to be taken directly from their native areas. The oily
sludge/filter cake material was to be mixed first in the Soliditech mixer and then sampled. These
protocols were followed for the filter cake material and the filter cake/oily sludge wastes.
However, due to perceived non-homogeneity in the Off-Site Area One soil, this waste was first
thoroughly mixed in the Soliditech mixer before it was sampled for chemical analyses, leaching
tests, moisture content, and particle size. The samples to determine bulk density were collected
from the native area using Shelby tubes, as specified in the Demonstration Plan.
75
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7.0 PERFORMANCE DATA AND EVALUATION
The Soliditech SITE technology evaluation was based on laboratory test results on samples
of waste materials collected before and after treatment. Physical tests included bulk density of
treated waste, water content, particle size analysis, permeability of the treated waste, unconfined
compressive strength, and wet/dry and freeze/thaw tests on treated waste. Chemical tests were
applied for pH, Eh, metals, polychlorinated biphenyls, volatile organic compounds, semivolatile
organic compounds, loss on ignition, oil and grease, and acid neutralization
capacity/neutralization potential. Extraction tests included TCLP extraction, EP toxicity, BET,
ANS 16.1, and WILT.
7.1
PHYSICAL TESTS
Physical tests performed on the pretreatment and post-treatment wastes included bulk
density, water content, loss on ignition, particle size analysis, permeability, unconfined
compressive strength, wet/dry weathering, freeze/thaw weathering, and acid neutralization
capacity. These waste characteristics are summarized in Table 14 and are discussed in the
following sections. The detailed data are presented in Appendix A, Tables A.I through A.7 and
Figures A.I through A.3.
7.1.1
Bulk Density
Bulk density of the pretreatment wastes ranged from 1.14 to 1.26 g/cm3. Waste material
from Off-Site Area One was greatest in bulk density because of the high content of indigenous
soil. The filter cake waste was lowest in bulk density because this waste contained a high
proportion of diatomaceous earth. Bulk densities of the post-treatment wastes were significantly
greater than the pretreatment wastes owing to the addition of cement. Bulk densities for the
post-treatment samples ranged from 1.43 to 1.68 g/cm .
7.1.2
Water Content
Water content of the pretreatment Off-Site Area One and filter cake wastes were 23.5 and
28.7 percent, respectively. After the solidification/stabilization treatment, these wastes contained
12.6 and 21.0 percent water, respectively. The difference in water content after
solidification/stabilization was apparently related to the amount of water and cement added in the
solidification/stabilization process. The filter cake/oily sludge waste contained 58.1 percent
water prior to treatment and 14.7 percent in the post-treatment samples.
76
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TABLE 14
CHEMICAL AND PHYSICAL ANALYSES OF UNTREATED AND TREATED WASTE
Filler Cake/Oily
Sludge Manure
Untreated
VoUlile Organic Compoundi (mg/Kj)
Ethyl Benzene
Telnchloroethene
Toluene
Trichloroelbene
Xyleoei
Semtvolatlle Organic Compoundi (mj/Kj)
Butyl benzyl phlhahue
o-Creaol
p-Cretol
2,4-Dimethylphenol
Bu(2-ElhyU>e»yl)phlhalale
2-Melhylniphlhilcne
NiphllukDe
Phenol
PCB. (tag/Kg)
Aroclor-1242
Arodor-1260
Metili (AA) (ln|/Kg)
Aneaic
Mercury
Selenium
Thallium
MetaU (ICPES) (rag/Kg)
Aluminum .
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical A Phyiical Te«li
Bulk Detully (|/cm3)
Eh(mv)
LOB on Ignition il 55O°C (tng/Kg)
Oil and Greaae. inhaled (mg/K«)
Permeability (cm/iec)
Uncbnfined CompretJtvc Strength latil
Particle Size
Water Content (%)
pll (pH until)
Wet/Dry Wealherini (% wt. Ion)
Freeie/Thaw Wealherini (% w. Ion)
NA: Not Analyzed
9J
19
26
< 0.040
10'7
390
NA
21.0
11.8
4J
1.6
8.4
33
32
16
27
14
< 0.040
0.052
1,600
0.13
1.0
1,200
5,7
34
2^00
3.0
950
150
1.19
220
700,000
130,000
NA
NA
0.46
58.1
3.6
NA
NA
Treated
<2.2
<4.9
<2.2
<33
<33
4.4
3.7
<:33
4.4
<33
4.8
6.2
8.4
. 40.
<0.040
0.12
18,000
1,000
023
1.0
190,000
28
43
850
16
1,800
54
1.68
•45
340.000
W.OOO
8.93 i 10's
860
NA
1417
12.0
Off-Sue Area One
Untreated Treated
13
2.2
•ID
<5.0
<50
<5.0
24
6J
<50
<5.0
29
14
94
0.16
0-23
< 0.050
4.000
700
073
13
4.600
11
33
650
2,7
93
120
1 26
100
300.000
28.000
NA
NA
0.42
235
19
NA
NA
<7.9
«U
43
<33
<33
<33
8-2
3.J
<33
<33
33
7J
92
0.17
<0-20
<0.10
11,000
580
<0.10
0.70
150,000
29
43
480
13
480
95
1.59
•S3
340,000
46,000
3.41 I IO"8
680
NA
12.6
110
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7.1.3
Particle Size Distribution
The mean particle size for the pretreatment wastes ranged from 0.32 to 0.46 mm. This
particle size range is representative of a fine textured material, which could be found at many
hazardous waste sites. Particle size was not determined on the post-treatment wastes because the
treated wastes were monolithic solids.
7.1.4
Permeability
Permeability of the untreated wastes was not determined. Permeabilities of the treated
wastes ranged from 8.9 x 10'9 cm/sec for the filter cake/oily sludge to 4.5 x 10'7 cm/sec for the
filter cake.
7.1.5
Unconfined Compressive Strength (UCS)
UCS determinations were performed on molded samples of solidified waste according to
ASTM D1633. UCS values ranged from 390 psi for the filter cake waste to 860 psi for the filter
cake/oily sludge. The USC values were inversely proportional to the permeability of the treated
waste and directly proportional to the weight fraction of cement mixed with the wastes. The
ratio of water and cement to waste varied for each treatment run due to the nature of the
untreated waste materials.
7.1.6
Wet/Dry Weathering Test
Wet/dry weathering tests were performed on molded samples of the post-treatment wastes
according to method TMSWC-12. Results are expressed as the cumulative weight loss incurred
through 12 wet/dry cycles normalized to a control that is not subjected to the wet/dry cycles.
Results for all wastes indicate that less than one percent of the cast cylinder weights were lost
over the 12 wet/dry cycles. UCS determinations were performed on the cast cylinders after
completion of the wet/dry weathering tests. UCS values ranged from 120 psi for the filter cake
waste to 220 psi for the filter cake/oily sludge waste.
7.1.7
Freeze/Thaw Weathering Test
Freeze/thaw weathering tests were performed on molded samples of the post-treatment
wastes according to method TMSWC-11. Results were reported in the same manner as the
wet/dry weathering tests. Results for all wastes indicate that 1 percent or less of the cast cylinder
78
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weights were lost over the 12 freeze/thaw cycles. UCS determinations were performed on cast
cylinders after completion of the freeze/thaw weathering test. UCS values ranged from 130 psi
for the filter cake waste to 290 for the filter cake/oily sludge waste.
7.1.8
Loss on Ignition
The loss on ignition of the pretreatment and post-treatment wastes were determined by
ASTM Cl 14. The loss on ignition for the filter cake samples was 54 percent (by weight) for the
pretreatment waste and 41 percent for the post-treatment waste. The filter cake/oily sludge had
a loss on ignition of 70 percent in the pretreatment waste (due to the high water content of this
waste mixture) and 34 percent in the post-treatment waste. The Off-Site Area One samples had
a loss on ignition of 36 percent in the pretreatment waste and 34 percent in the post-treatment
waste.
7.1.9
On-Site Tests
Field tests performed during the Soliditech demonstration included the Slump of Portland
Cement (ASTM C143) and the Homogeneity of Mixing (a modification of ASTM C136 and C142)
tests. The slump results were 4.1 inches for the filter cake/oily sludge mixture, 5.8 inches for the
filter cake waste, and 5.4 inches for Off-Site Area One. The slump measurement is the vertical
difference between the top of the mold and the top of the slumped waste material. The results
are proportional to the amount of cement in each of the treated waste mixtures.
The results of the Homogeneity of Mixing test indicate that the treated waste materials in
the treated waste slurries were finely divided. The filter cake/oily sludge mixture had the
highest percentage of solids retained on the 0.25 to 0.75 inch sieves, 4.3 percent by weight, while
the values for the filter cake waste and Off-Site Area One waste were 2.3 and 1.9 percent by
weight, respectively. The results of this test appear to correlate with visual observations of
unmixed material in the filter cake oily sludge test run.
The results of these field tests may not be adequate to determine the homogeneity of
mixing of treated waste material. The development of quantitative field tests would be desirable.
7.2
CHEMICAL TESTS
Results of the chemical tests performed on the pre-and post-treatment waste samples, as
well as the reagent mix, are summarized in Table-HrThese tests analyzed the pre- and post-
79
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treatment wastes to determine the changes in chemical composition after treatment. Chemical
composition is not necessarily an indicator of contaminant mobility. Section 7.3 presents the
results of leaching tests. The leaching tests may indicate contaminant mobility. Tables 15 and 16
summarize the results of the chemical tests performed on the sand used for the reagent mix and
the residual material cleaned from the mixer prior to its use. The detailed chemical data are
presented in Appendix A, Tables A.I through A.9. Chemical characteristics analyzed include pH,
Eh, metals, PCBs, VOCs, SVOCs, loss on ignition, and oil and grease.
7.2.1
The pH of the pre- and post-treatment wastes and the reagent mix samples was
determined by U.S. EPA Method 9045. The pH of the pretreatment Off-Site Area One waste
was 7.9. The filter cake and filter cake/oily sludge wastes had a pH values of 3.4 and 3.6. The
post-treatment wastes and the reagent mix had pH values of 11.8 and 12.1. This extremely high
pH reflected the alkalinity associated with the cement in the solidification/ stabilization process.
7.2.2
Eh
The Eh of the pretreatment and post-treatment wastes and the reagent mix samples was
determined with an Eh electrode on waste/water slurries prepared for the determination of pH by
U.S. EPA Method 9045. The Eh of the pretreatment wastes ranged from 100 millivolts (mv) for
Off-Site Area One to 370 mv for the filter cake. The post-treatment wastes and the reagent mix
had Eh values ranging from -31 to -63 mv.
7.2.3
Metals
Several U.S. EPA methods were employed to determine the concentration of metals in the
predemonstration blank, pretreatment and post-treatment wastes, and the reagent mix. These
digestion and analytical methods were discussed in Section 5.6.2.
The pretreatment wastes from the filter cake contained 2,200 mg/Kg lead, 1,900 mg/Kg
barium, 26 mg/Kg arsenic, 21 mg/Kg copper, and 26 mg/Kg zinc. Lead and barium
concentrations in the post-treatment filter cake waste contained higher concentrations of
chromium (20 mg/Kg) and nickel (11 mg/Kg) than the pre-treatment waste (4.7 and 2.7 mg/Kg,
respectively). The post-treatment wastes from the filter cake also contained elevated levels of
calcium, aluminum, and sodium due to the addition of cement to the wastes. All other metal
concentrations were approximately the same in the pre- and post-treatment filter cake wastes.
80
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TABLE 15
CHEMICAL ANALYSIS OF SAND
Metals (AA) (mg/Kg)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/Kg)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
0.11
<0.050
<0.20
<0.20
110
<1.0
<0.20
<0.50
<100
<3.0
<2.0
<5.0
<2.0
<100
<2.0
Note: The sand was used as a waste surrogate in the reagent mix test run.
81
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TABLE 16
CHEMICAL ANALYSIS OF PREDEMONSTRATION BLANK
Volatile Organic Compounds (mg/Kg)
Ethyl benzene
Tetrachloroethene
Toluene
Trichloroethene
Xylenes
Semivolatile Organic Compounds (mg/Kg)
Butyl benzyl phthalate
o-Cresol
p-Cresol
2,4-Dimethylphenol
Bis(2-ethylhexyl)phthalate
2-Methylnaphthalene
Naphthalene
Phenol
PCBs (mg/Kg)
Arcoclor-1242
Arcoclor-1260
Metals (AA) (mg/Kg)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/Kg)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
9.4
17
7.1
2.2
51
<5.0
<5.0
<5.0
<5.0
14
150
55
50
<0.99
<2.0
95
1.0
<0.20
0.10
43,000
2,500
2.2
7.1
130,000
780
380
160
75
5,400
840
Note: The predemonstration blank consisted of residual material removed from the large
Soliditech mixer prior to treatment of waste.
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The pretreatment filter cake/oily sludge waste mixture contained 2,500 mg/Kg lead, 1 ,600
mg/Kg barium, 150 mg/Kg zinc, 14 mg/Kg arsenic, and 34 mg/Kg copper. Lead, barium, and
zinc concentrations in the post- treatment filter cake/oily sludge wastes decreased to 850 mg/Kg,
1 ,000 mg/Kg, and 54 mg/Kg, respectively. The post-treatment filter cake/oily sludge wastes also
contained higher concentrations of chromium (28 mg/Kg) and nickel (16 mg/Kg) than in the
pretreatment wastes (5.7 mg/Kg and 3.0 mg/Kg, respectively). The post- treatment wastes from
the filter cake/oily sludge contained elevated levels of calcium, aluminum, and sodium due to the
cement added to the wastes. All other metal concentrations were approximately the same in the
pre- and post- treatment wastes.
The pretreatment Off-Site Area One waste contained 650 mg/Kg lead, 700 mg/Kg
barium, 120 mg/Kg zinc, 94 mg/Kg arsenic, and 33 mg/Kg copper. Mercury (0.16 mg/Kg) was
also found in the Off-Site Area One pretreatment waste. Lead (480 mg/Kg), barium (580
mg/Kg), and zinc (95 mg/Kg) in the Off-Site Area One post-treatment waste also decreased in
concentration compared to the pretreatment waste. The post-treatment Off-Site Area One waste
also contained higher concentrations of chromium (29 mg/Kg) and nickel (13 mg/Kg) than the
pretreatment wastes (1 1 mg/Kg and 2.7 mg/Kg, respectively). The post^ treatment Off-Site Area
One wastes also contained elevated levels of calcium, aluminum, and sodium due to the cement
added to the wastes. All other metal concentrations were approximately the same in the pre- and
post-treatment wastes.
The reagent mix contained large concentrations of calcium (18 percent by weight),
aluminum (2.2 percent), and sodium (0.25 percent) as expected. The reagent mix also contained
appreciable amounts of the following metals; arsenic (59 mg/Kg), barium (1,700 mg/Kg),
chromium (38 mg/Kg), copper 60 mg/Kg), nickel (21 mg/Kg), and zinc (39 mg/Kg). The
decreasing trends in metal concentrations in the post- treatment versus pretreatment wastes can be
attributed to dilution by the reagent mix when the reagent mix contained a lower concentration
of an element than the pretreatment waste (as in the case of lead, barium, and zinc). Where the
reagent mix contained a higher concentration of a metal than the pretreatment waste, the
concentration of that metal in the post- treatment waste was increased (as with chromium, nickel,
aluminum, calcium, and sodium). The concentration of a metal remained relatively constant if
the pretreatment waste and the reagent mix contained similar concentrations.
The predemonstration blank (scrapings of the residue from the inside of the Soliditech
mixing unit before this demonstration) contained high levels of the elements listed in Table 16.
The impact of the predemonstration solids was considered negligible after dilution with
contaminated soils and reagent.
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A comparative analysis of the pretreatment and "post-treatment wastes showed decreasing
trends in metal concentrations. Where the reagent mix contained a higher concentration of a
metal, the concentration of that metal in the post-treatment waste was increased. The
concentration of a metal remained relatively constant if the pretreatment waste and the reagent
mix contained similar concentrations.
7.2.4
Polychlorinated Biphenyls (PCBs)
The pretreatment and post-treatment wastes, reagent mix, and predemonstration blank
were analyzed for PCBs by U.S. EPA Method 8080. PCBs were not detected in the
predemonstration blank or the reagent mix samples.
Aroclor 1242 and Aroclor 1260 (PCBs) were found in the pretreatment and post-treatment
wastes. The pretreatment filter cake samples contained 9.0 mg/Kg Aroclor 1242 and 19 mg/Kg
Aroclor 1260. The post-treatment filter cake samples contained slightly lower concentrations of
these Aroclors (6.3 and 10 mg/Kg, respectively).
The pretreatment filter cake/oily sludge samples contained 16 mg/Kg Aroclor 1242 and
27 mg/Kg Aroclor 1260. The post-treatment filter cake/oily sludge samples contained 6.2 to 8.4
mg/Kg of each of these Aroclors, respectively.
The pretreatment Off-Site Area One samples contained 29 mg/Kg Aroclor 1242 and 14
mg/Kg Aroclor 1260. Post-treatment samples from Off-Site Area One contained 33 mg/Kg of
Aroclor 1242 and 7.5 mg/Kg Aroclor 1260.
7.2.5
Volatile Organic Compounds (VOCs)
The pretreatment and post-treatment wastes were analyzed for VOCs by U.S. EPA
Method 8240. VOCs were not detected in the pretreatment filter cake samples. The pretreatment
filter cake/oily sludge samples contained 32 mg/Kg total xylenes, 4.3 mg/Kg ethyl benzene, 8.4
mg/Kg toluene, and 3.3 mg/Kg trichloroethene. Tetrachloroethylene was detected in one of the
pretreatment filter cake/oily sludge samples. Off-Site Area One pretreatment wastes contained
8.3 mg/Kg toluene and 2.2 mg/Kg total xylenes. 1,2-Dichloroethane was detected in one of the
pretreatment Off-Site Area One samples. VOCs were not detected in any of the post-treatment
waste samples.
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The predemonstration blank, which consisted of'serapings of residue from the inside of
the Soliditech mixing unit before this demonstration was initiated, was found to contain a number
of VOCs. Due to the absence of VOCs in the post-treatment samples, these scrapings were not
considered to be a source of VOC contamination in this demonstration.
Organic emissions were monitored during waste collection and treatment with no positive
results. It is possible that organics were lost during these operations.
7.2.6
Semivolatile Organic Compounds (SVOCs)
The pretreatment and post-treatment wastes, reagent mix, and predemonstration blank
were analyzed for SVOCs by U.S. EPA Method 8270.
SVOCs were not detected in the pretreatment filter cake samples. Phenol (12 mg/Kg) and
p-cresol (14 mg/Kg) were found at concentrations near the detection limit in the post-treatment
filter cake samples.
The pretreatment filter cake/oily sludge contained 49 mg/Kg of butyl benzyl phthalate
and 14 mg/Kg of 2-methylnaphthalene. Naphthalene (9.4 mg/Kg) and o-cresol (5.0 mg/Kg)
were detected in one of three pretreatment filter cake/oily sludge samples. The post-treatment
filter cake/oily sludge samples contained 2,4-dimethylphenol, 2-methylnaphthalene, phenol,
bis(2-ethylhexyl)phthalate, and p-cresol at concentrations less than 5 mg/Kg each.
Off-Site Area One pretreatment wastes contained 6.2 mg/Kg of 2-methylnaphthalene, 40
mg/Kg of butyl benzyl phthalate, and 24 mg/Kg of bis(2-ethylhexyl)phthalate. Di-n-
butylphthalate was detected in one of the pretreatment Off-Site Area One samples. The post-
treatment Off-Site Area One samples contained detectable quantities of 2-methylnaphthalene,
butyl benzyl phthalate, and bis(2-ethylhexyl)phthalate.
SVOCs were not detected in the reagent mix samples.
The predemonstration blank contained a number of SVOCs. These included: 2-
methylnaphthalene (150 mg/Kg), anthracene (30 mg/Kg), hexachlorobenzene (370 mg/Kg),
naphthalene (55 mg/Kg), pentachlorobenzene (26 mg/Kg), phenanthrene (45 mg/Kg), and phenol
(50 mg/Kg). These scrapings were not considered a source of SVOC contamination in this
demonstration because concentrations of SVOCs were low and the amount of residue was
extremely small compared to the amount of waste being treated.
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7.2.7
Oil and Grease
The oil and grease content of the pretreatment and post-treatment wastes was determined
by a sonication extraction of the soil (modified U.S. EPA Method 3550) followed by U.S. EPA
Method 413.2. The oil and grease content of the filter cake samples was 17 percent (by weight)
in the pretreatment waste and 7.7 percent in the post-treatment waste. The filter cake/oily
sludge samples contained 13 percent oil and grease in the pretreatment waste and 6.0 percent in
the post-treatment waste. Off-Site Area One results indicated that the oil and grease
concentrations increased from 2.8 percent in the pretreatment waste to 4.6 percent in the post-
treatment waste. The reason for this increase is not clear, but may be related dispersion of the oil
and grease by treatment or to the increased pH of the treated waste.
7.2.8
Acid Neutralization Capacity/Neutralization Potential
The acid neutralization capacity results for the pretreatment wastes are presented in Table
A.6 in Appendix A. These data indicate that the pretreatment wastes have very low acid
neutralization capacity. The pH of Off-Site Area One was reduced from 8.7 to 4.4 with the
addition of the first aliquot of acid. The filter cake and filter cake/oily sludge wastes had initial
pH values of 3.4 and 3.6 prior to any acid addition.
Acid neutralization results for the post-treatment wastes could not be determined by this
method. The pH levels of the post-treatment wastes were all greater than 11.8 and the addition
of acid did not appreciably change this pH. The neutralization capacity of the post-treatment
soils was determined by "Field and Laboratory Methods Applicable to Overburdens and
Minesoils" (U.S. EPA, 1978). The neutralization potential, expressed as percent CaCO3, was 43.3
percent for the reagent mix, 31.3 percent for the filter cake, 43.1 percent for the filter cake/oily
sludge, and 39.9 percent for Off-Site Area One.
7.3
LEACHING TESTS
The results of the leaching tests are summarized in Tables 17 through 25. The detailed
chemical data is presented in Appendix A, Tables A. 10 through A.44, which are attached to this
report. A discussion of these results is given below.
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7.3.1
TCLP
The Toxicity Characteristic Leaching Procedure (TCLP) was performed on the
pretreatment and post-treatment wastes and the reagent mix. This procedure, described in the
Federal Register, 1986 (40 CFR, Part 268), is used to determine the extractability of organic and
inorganic constituents using an acidic extraction solution to simulate municipal solid waste
codisposal. The TCLP leachate data are summarized in Table 17. The detailed data are provided
in Appendix A, Tables A.10 through A.13.
7.3.1.1
Reagent Mix
The TCLP leachates produced from the reagent mix samples had pH of 11.4, and Eh of -
23 mv. The leachates contained 8,600 mg/L total dissolved solids (TDS). PCBs and oil and
grease were not detected in any of the reagent mix TCLP leachates. Barium, calcium, and
sodium were found at concentrations of 4.0, 1,900, and 34 mg/L, respectively. Aluminum and
chromium were present at detection limit concentrations. Small concentrations (<0.07 Mg/L) of
six VOCs (acetone, 2-butanone, 4-methyl-2-pentanone, ethyl benzene, toluene, and total xylenes)
were present in the TCLP leachates of the reagent mix. SVOCs were not detected in the reagent
mix leachates. The strong alkalinity of these samples made it difficult to maintain the proper pH
when extracting the acid compounds. Thus, surrogate recoveries and matrix spikes indicate that
the acid compound results are biased 50 to 100 percent low.
7.3.1.2
Filter Cake
The pretreatment TCLP leachate samples from the filter cake had a pH of 4.6 and an Eh
of 270 mv. The post-treatment leachates had a pH of 10.8 and an Eh of -28 mv. The
pretreatment leachates contained 4,500 mg/L TDS while the post-treatment leachates had 8,500
mg/L TDS. Oil and grease was found at 1.4 mg/L in the pretreatment leachate and 4.4 mg/L in
the post-treatment leachate. PCBs were not detected in any of the pretreatment or post-
treatment TCLP leachates.
The pretreatment leachates contained detectable quantities of arsenic (0.0050 mg/L), lead
(4.3 mg/L), zinc (0.28 mg/L), and copper (0.040 mg/L). Arsenic, lead and zinc were not
detected, and copper was found at 0.023 mg/L in the post-treatment samples. Chromium was
present in low concentrations (0.063 mg/L) in the post-treatment leachates. Calcium
concentrations in the post-treatment leachates were greater than in the pretreatment leachates, 9.0
versus 1800 mg/L. Sodium decreased from 1,100 mg/L in the pretreatment leachates to about 13
87
-------
TABIJB 17
CHEMICAL ANALYSES OF TCU» EXTRACT FROM UNTREATED AND TREATED WASTE MATERIALS
oo
00
Filler Cake/Oily
Volatile Organic Compounds (pg/L)
Acetone
Benzene
2-Dulanone
Ethyl benzene
4-Methyl-2-pentanonc
Melhytene chloride
Telnchloroelhene
Toluene
1,1,1-Trichloroelhane
Trichtoroelhene
Xylenes
Semivolalile Organic Compounds (fig/L)
Benzyl alcohol
Butyl benzyl phthalalc
o-Cresol
p-Cresol
2,4-Dimclhylphcnol
Phenol
PCBs (ug/L)
Arcoclor-1242
Arcoclor-1260
MctaU (AA) (mg/L)
Arsenic
Lead
Metals (1CPES) (mg/L)
Aluminum
Barium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh (mv)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
NA: Not Analyzed
Tiller
Untreated
250
<2.0
<2.0
4.3
13
<2.0
<2.0
4.0
<2.0
<2.0
< 10
< 10
<]0
<10
<0.42
<0.84
0.0050
NA
0.50
1.4
0.0052
9.0
<0.030
0.040
4.3
< 0.020
1,100
0.28
270
4400
1.4
4.6
Cake
Treated
<210
<2.0
<2.0
<2.0
<2.0
<2.0
<2.0
<2.0
<2.0
<10
62
440
20
630
<0.45
<0.90
< 0.0020
0.0020
<0.20
1.3
< 0.0050
1,800
0.063
0.023
<0.20
<0.020
13
<0.020
-28
8,500
4.4
10.8
Sludge Mitlure
Untreated
1000
8.2
8.9
60
21
2.9
55
<2.0
27
57
<10
44
47
93
200
<0.43
<0.86
0.014
NA
0.28
2.5
0.0093
21
< 0.030
0.023
5.4
0.027
1,200
1.3
210
5,200
1.6
4.8
Treated
<820
<4.6
<3.7
<55
<2.0
<24
<2.0
""in
88
340
130
340
<0.2\
< 0.0020
0.014
0.47
5.1
< 0.0050
1,900
< 0.030
<0.020
<0.050
<0.020
43
< 0.020
-35
8,600
2.4
11.6
Off-Site Area One
Untreated
200
-------
mg/L in the post-treatment leachates. The different sodium levels are a result of the different
extraction fluids recommended by the TCLP procedure for solids with different pHs. The
extraction fluid for the pretreatment leachates contained sodium hydroxide, while the extraction
fluid used for the post-treatment leachates did not.
Three VOCs — acetone, 4-methyl-2-pentanone, and methylene chloride — were found in
the zero head-space TCLP leachates of the filter cake. These compounds were found at similar
levels in the laboratory blank and are therefore considered to be laboratory contaminants. VOCs
were not detected in the post-treatment leachates.
SVOCs were not detected in the pretreatment TCLP leachates of the filter cake area.
Post-treatment leachates contained phenol (630 Mg/L), p-cresol (440 Mg/L), o-cresol (62
and 2,4-dimethylphenol (20
7.3.1.3
Filter Cake/Oily Sludge
The pretreatment TCLP leachate samples from the filter cake/oily sludge had a pH of 4.8
and an Eh of 210 mv. The post-treatment leachates had a pH of 11.6 and an Eh of -35 mv. The
pretreatment leachates contained 5,200 mg/L TDS; the post-treatment leachates 8,600 mg/L TDS.
Oil and grease was found at 1.6 mg/L in the pretreatment leachate and 2.4 mg/L in the post-
treatment leachate. PCBs were not detected in any of the pretreatment or post-treatment TCLP
leachates.
The pretreatment leachates contained low concentrations of arsenic (0.014 mg/L), lead
(5.4 mg/L), and zinc (1.3 mg/L). Arsenic, lead and zinc were not detected in the post-treatment
leachates. Barium and calcium concentrations were lower in the pretreatment leachates than in
the post-treatment leachates, 2.50 versus 5.1 mg/L and 21 versus 1,900 mg/L, respectively.
Sodium decreased from 1,200 mg/L in the pretreatment leachates to 43 mg/L in the post-
treatment leachates. The different sodium levels are a result of the different extraction fluids
recommended by the TCLP procedure for solids with different pHs. The extraction fluid for the
pretreatment leachates contained sodium hydroxide, while the extraction fluid used for the post-
treatment leachates did not.
Acetone (1,000 Mg/L), 4-methyl-2-pentanone (60 Mg/L), methylene chloride (21 Mg/L),
total xylenes (57 Mg/L), trichloroethene (27 Mg/L), and toluene (55 Mg/L) were found in the
pretreatment zero head-space TCLP leachates of the filter cake/oily sludge for VOCs.
89
-------
Tetrachloroethylene, ethyl benzene, benzene, and 2-butanone were also present at detection limit
levels in the pretreatment leachates. The acetone, 4-methyl-2-pentanone, and methylene chloride
were found at similar levels in the laboratory blank and are therefore considered to be laboratory
contaminants for the pretreatment leachates. VOCs were not detected in the post-treatment
leachates.
Four SVOCs were found in the pretreatment TCLP leachates of the filter cake/oily sludge
area. These were 2,4-dimethylphenol (93 Mg/L), phenol (200 Mg/L), p-cresol (47 Mg/L), and o-
cresol (44 /Lig/L). Post-treatment leachates contained larger concentrations of these compounds:
2,4-dimethylphenol (130 Mg/L), phenol (340 Mg/L), p-cresol (340 Mg/L), and o-cresol (88 Mg/L).
7.3.1.4
Off-Site Area One
The pretreatment TCLP leachate samples from the Off-Site Area One had a pH of 5.1 and
an Eh of 190 mv. The post- treatment leachates had a pH of 1 1.5 and an Eh of -57 mv. The
pretreatment leachates contained 6,300 mg/L TDS; the post- treatment leachates 9,000 mg/L TDS.
Oil and grease was found at 1.9 mg/L in the pretreatment leachate and 12 mg/L in the post-
treatment leachate. PCBs were not detected in any of the pretreatment or post- treatment TCLP
leachates.
The pretreatment leachates contained low concentrations of arsenic (0.19 mg/L), lead
(0.46 mg/L), and zinc (0.63 mg/L). The lead and zinc were not detected in the post- treatment
leachates. The arsenic concentration was 0.017 mg/L in the post-treatment leachates. Barium
and calcium concentrations were lower in the pretreatment leachates than in the post- treatment
leachates, 1.6 versus 2.3 mg/L and 190 versus 1,900 mg/L, respectively. Sodium decreased from
1200 mg/L in the pretreatment leachates to about 16 mg/L in the post-treatment leachates. The
different sodium levels are a result of the different extraction fluids recommended by the TCLP
procedure for solids with different pHs. The extraction fluid for the pretreatment leachates
contained sodium acetate, while the extraction fluid used for the post-treatment leachates
contained acetic acid.
Acetone (200 Mg/L), 4-methyl-2-pentanone (370 Mg/L), total xylenes (26 Mg/L), and
toluene (270 Mg/L) were found in the pretreatment zero head-space TCLP leachates for VOCs.
Ethyl benzene was also present at detection limit levels in the pretreatment leachates. The
acetone and 4-methyl-2-pentanone were found at similar levels in the laboratory blank and are
therefore considered to be laboratory contaminants for the pretreatment leachates. VOCs were
not detected in the post-treatment leachates.
90
-------
Four SVOCs were found in the pretreatment TCLP leachates of the Off-Site Area One
area. These were 2,4-dimethylphenol(10 /ig/L), benzyl alcohol (57 /Ltg/L), butyl benzyl
phthalate (36 M8/L), and o-cresol (18 Mg/L). Post-treatment leachates contained increased
concentrations of 2,4-dimethylphenol (26 Mg/L), benzyl alcohol (72 Mg/L), phenol (100 Mg/L),
and p-cresol( 110 Mg/L).
7.3.2
EP Toxicity
The Extraction Procedure Toxicity Test (EP) is described in U.S. EPA Method 1310. The
leaching test was performed on the pretreatment and post-treatment wastes and the reagent mix.
This procedure is also used to determine extractability of organic and inorganic constituents using
an acidic extraction solution to simulate municipal solid waste codisposal. The EP is currently
used for land disposal restriction regulations. The EP leachate data are summarized in Table 18.
The detailed data are presented in Appendix A, Tables A.14 through A.17.
7.3.2.1
Reagent Mix
The EP leachates produced from the reagent mix samples had a pH of 11.3, and Eh of 9.0
mv. The leachates contained 8,700 mg/L total dissolved solids. PCBs and oil and grease were not
detected in any of the reagent mix EP leachates. Barium, calcium, and sodium were found at
concentrations of 4.3 mg/L, 1,900 mg/L, and 35 mg/L , respectively. Arsenic, selenium,
aluminum, and chromium were detected in at least one of the leachates at detection limit
concentrations.
7.3.2.2
Filter Cake
The pretreatment EP leachate samples from the filter cake had a pH of 3.8 and an Eh of
320 mv. The post-treatment leachates had a pH of 10.9 and an Eh of -2.0 mv. The pretreatment
leachates contained 90 mg/L TDS, and the post-treatment leachates contained 9,500 mg/L TDS.
Oil and grease was not detected in the pretreatment leachates. The post-treatment EP leachates
contained 4.0 mg/L oil and grease. PCBs were not detected in any of the pretreatment or post-
treatment EP leachates.
The pretreatment leachates contained detectable quantities of arsenic (0.010 mg/L), lead
(0.25 mg/L), and zinc (0.032 mg/L). The lead and zinc were not detected, and arsenic was found
at 0.0023 mg/L in the post-treatment samples. Barium, calcium, and sodium concentrations in
the post-treatment leachates were greater than in the pretreatment leachates. Barium increased
from 0.21 to 1.4 mg/L, calcium from 4.8 to 2,000 mg/L, and sodium from 1.4 to 15 mg/L. These
91
-------
TABLE 18
CHEMICAL ANALYSES OF EP EXTRACT FROM UNTREATED AND TREATED WASTE
Filter Cake
Unlrealed Treated
K>
PCBs 0»g/L)
ArocIor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Lead
Mercury
Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barjum
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh(mV)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
<043
<0.86
0.010
0.26
<0.00020
<0.0040
< 0.0010
<0.20
0.21
<0.0020
< 0.0050
4.8
< 0.030
< 0.020
0.25
< 0.020
1.4
0.032
320
90
<0.40
3.8
<0.41
<0.82
0.0023
0.0023
< 0.00020
<0.0040
<0.0010
<0.20
1.4
<0.0020
< 0.0050
2,000
0.083
0.037
<0.050
<0.020
15
<0.020
-2.0
9,500
4.0
10.9
Filler Cake/Oily
Sludee Mixture
Untreated
<0.43
<0.86
0.011
OSS
<0.00020
<0.0040
0.0013
<0.20
1.1
<0.0020
0.0082
11
< 0.030
< 0.020
0.52
<0.020
58
0.86
220
330
<0.40
4.8
Treated
<0.42
<0.84
0.0020
0.015
< 0.00020
< 0.0050
< 0.0010
<0.20
5.7
< 0.0020
<0.0050
2,100
0.037
< 0.020
< 0.050
< 0.020
45
< 0.020
-30
9,100
3.1
11.8
Off-Site
Unlrealed
<0.45
<0.90
0.18
0.12
< 0.00020
<0.0040
<0.0010
0.40
0.58
< 0.0020
0.0052
140
<0.030
< 0.020
0.067
<0.020
2.1
0.26
130
790
2.6
4.8
Area One
Treated
<0.21
<0.42
0.028
0.012
< 0.00030
<0.0050
<0.0010
0.20
2.4
<0.0020
<0.0050
2,100
<0.030
0.060
<0.050
<0.020
16
< 0.020
-10
9,400
11
11.7
Reagent Mix
<0.020
<0.040
<0.0020
< 0.0020
<0.00020
0.017
-------
increases can be attributed to Portland cement and other proprietary additives used during
treatment.
7.3.2.3
Filter Cake/Oily Sludge
The pretreatment EP leachate samples from the filter cake/oily sludge had a pH of 4.8
and an Eh of 220 mv. The post-treatment leachates had a pH of 11.8 and an Eh of -30 mv. The
pretreatment leachates contained 330 mg/L of TDS while the post-treatment leachates contained
9,100 mg/L of TDS. Oil and grease was not detected in the pretreatment leachates. The post-
treatment EP leachates contained 3.1 mg/L of oil and grease. PCBs were not detected in any of
the pretreatment or post-treatment EP leachates.
The pretreatment leachates contained detectable quantities of arsenic (0.011 mg/L), lead
(0.52 mg/L), and zinc (0.86 mg/L). Lead and zinc were not detected and arsenic was found at
0.0020 mg/L in the post-treatment samples. Barium and calcium concentrations in the post-
treatment leachates were greater than in the pretreatment leachates. Barium increased from 1.1 to
5.7 mg/L and calcium from 11 to 2,100 mg/L. These increases can be attributed to the Portland
cement and proprietary additives used during treatment.
7.3.2.4
Off-Site Area One
The pretreatment EP leachate samples from the Off-Site Area One had a pH of 4.8 and an
Eh of 130 mv. The post-treatment leachates had a pH of 11.7 and an Eh of -10.0 mv. The
pretreatment leachates contained 790 mg/L of TDS and the post-treatment leachates contained
9,400 mg/L of TDS. The pretreatment leachates contained 2.6 mg/L of oil and grease. The oil
and grease increased to 11 mg/L in the post-treatment EP leachates. PCBs were not detected in
any of the pretreatment or post-treatment EP leachates.
The pretreatment leachates contained arsenic (0.18 mg/L), lead (0.067 mg/L), and zinc
(0.26 mg/L). Lead and zinc were not detected and arsenic was found at 0.028 mg/L in the post-
treatment samples. Barium, calcium, and sodium concentrations in the post-treatment leachates
were greater than in the pretreatment leachates. Barium increased from 0.58 to 2.4 mg/L,
calcium from 140 to 2,100 mg/L, and sodium from 2.1 to 16 mg/L. These increases can be
attributed to Portland cement and other proprietary additives used during treatment.
93
-------
7.3.3
BET
The BET was performed on the pretreatment and post-treatment wastes and on the
reagent mix samples. The procedure is described in the modification to the Equilibrium
Leaching in the Test Methods for Solidified Waste Characterization - Method 6 (Environment
Canada/U.S. EPA, no date). The leach test assesses the teachability of constituents from the
waste in deionized water with varying solid-to-liquid ratios. Three solid-to-liquid (S/L) ratios
were used for this test: 1:4, 1:20, and 1:100. Leachability of pollutant solutes at all S/L ratios was
considered to be insignificant. Leachability data for aluminum, barium, calcium, and sodium at
various S/L ratios are being evaluated in parallel with data rom other extraction and leaching
tests in order to verify the applicability of the BET to these types of sample materials. Due to
the large number of nondetected values in the data, no interpretation of the effects of these
solid-to-liquid ratios on chemical teachability were made. The BET leachate data are
summarized in Tables 19 through 22. The detailed data are presented given in Appendix A,
Tables A. 18 through A.29.
7.3.3.1
Reagent Mix
The pH of the three BET leachates ranged from 11.8 for the 1:100 S/L leachate to 12.0
for the 1:20 and 1:4 S/L leachates. The Eh of the leachates ranged from -69 to -80 mv. The
TDS and total organic carbon (TOC) concentrations increased from 620 mg/L TDS and 3.0 mg/L
TOC in the 1:100 S/L leachate to 2,900 mg/L TDS and 36 mg/L TOC in the 1:4 S/L leachate.
PCBs and oil and grease were not detected in any of the reagent mix BET leachates.
Arsenic was found at concentrations of 0.0030, 0.0037, and 0.0073 mg/L in the 1:4, 1:20,
and 1:100 S/L leachates. Lead and zinc were not detected in any of the reagent mix leachates.
The concentration of barium and sodium increased as the S/L ratio decreased. Barium
concentrations increased from 1.6 mg/L in the 1:100 S/L leachates to 27 mg/L in the 1:4
leachates. Sodium concentrations increased from 9.0 mg/L in the 1:100 S/L leachates to 160
mg/L in the 1:4 S/L leachates. Conversely, the S/L concentration of aluminum decreased from
4.8 mg/L in the 1:100 S/L leachate to 0.37 mg/L in the 1:4 S/L leachate. Calcium concentrations
were equal, at 540 and 560 mg/L, in the 1:4 and 1:20 S/L leachates, and 210 mg/L in the 1:100
S/L leachate.
94
-------
TABLE 19
CHEMICAL ANALYSIS OF BET EXTRACT FROM
UNTREATED AND TREATED HLTER CAKE WASTE
Ul
PCBs
Aroclor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh (mV)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
Total Organic Carbon (mg/L)
Untreated
<0.42
<0.84
0.072
< 0.00020
<0.0050
<0.0020
270
440
0.65
3.7
91
Treated
<0.43
<0.86
0.011
<0.00020
<0.0040
<0.0010
1.9
0.14
<0.0020
0.0073
30
<0.030
0.050
0.87
0.063
2.3
0.27
0.20
6.3
<0.0020
<0.0050
850
0.046
0.063
< 0.050
<0.020
84
<0.020
-82
3,800
6.3
11.7
140
Solid-to-Liauid Ratio
Unlrealed
<0.41
<0.82
0.014
<0.00020
<0.0050
<0.0020
0.23
0.28
< 0.0020
<0.0050
7.3
<0.030
<0.020
0.42
< 0.020
<1.0
0.047
290
120
0.53
3.5
28
1:20
Treated
<0.41
<0.82
0.0037
<0.00030
<0.0040
< 0.0010
0.47
3.4
<0.0020
<0.0050
480
0.037
0.027
<0.050
<0.020
19
<0.020
-92
1,700
2.7
11.7
43
1:100
Untreated Treated
<0.42
<0.84
0.020
<0.00020
<0.0050
<0.0020
270
40
<0.40
3.9
11
<0.21
<0.42
0.0020
<0.00020
<0.0040
<0.0010
0.37
0.47
< 0.0020
<0.0050
1.2
<0.030
<0.020
0.18
<0.020
<1.0
0.020
1.1
0.92
<0.0020
<0.0050
230
<0.030
<0.020
<0.050
<0.020
4.3
<0.020
-82
760
<0.40
11.5
14
-------
TABLE 20
CHEMICAL ANALYSIS OF BET EXTRACT FROM
UNTREATED AND TREATED FILTER CAKE/OILY SLUDGE MIXTURE
Solid-lo-Liauid RalJQ
1:20
1:100
Untreated Treated
PCBs (Mg/L)
Aroclor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh(mV)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
Total Organic Carbon (mg/L)
umrciucu
<1.1
<2.2
0.042
< 0.00020
<0.0050
<0.0020
0.36
0.83
< 0.0020
0.036
44
< 0.030
<0.020
1.7
0.049
230
2.7
240
1,800
3.2
3.7
200
HQtU&U
<0.42
<0.84
0.0080
< 0.00020
<0.0040
<0.0020
0.23
17
<0.0020
<0.0050
730
< 0.030
0.030
<0.050
0.023
250
<0.020
,101
3,500
4.9
12.0
110
<0.44
<0.88
0.035
< 0.00020
<0.0050
< 0.0020
<0.20
0.78
<0.0020
0.0062
9.1
<0.030
<0.020
0.43
0.028
80
0.69
220
470
2.2
4.2
60
<0.42
<0.84
0.0023
< 0.00030
<0.0040
< 0.0020
0.43
9.6
<0.0020
<0.0050
750
< 0.030
0.023
<0.050
<0.020
58
<0.020
-99
2,300
1.3
11.9
32
<0.41
<0.82
0.0083
<0.00020
<0.0050
<0.0020
<0.20
0.48
<0.0020
<0.0050
2.1
<0.030
<0.020
0.14
0.022
17
0.16
220
110
1.3
4.4
21
<0.22
<0.44
0.0030
<0.00020
<0.0040
<0.0020
1.3
2.6
<0.0020
<0.0050
440
<0.030
<0.020
<0.050
<0.020
13
<0.020
-93
1,200
0.43
11.8
8.0
-------
TABLE 21
CHEMICAL ANALYSIS OF BET EXTRACT FROM
UNTREATED AND TREATED OFF-SITE AREA ONE WASTE
PCBs (/ig/L)
Aroclor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh(mV)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
Total Organic Carbon (mg/L)
1:4
Untreated Treated*
<2.3
0.38
<0.00020
<0.0040
< 0.0010
110
1,100
16
8.3
190
<0.43
<0.86
0.067
<0.00020
0.0070
< 0.0020
<0.20
0.11
<0.0020
0.0068
150
< 0.030
<0.020
<0.050
< 0.020
5.0
<0.020
<0.20
9.7
<0.0020
<0.0050
1,000
< 0.030
0.17
< 0.050
0.033
80
<0.020
-77
4,600
26
12.1
120
Solid-to-Liquid Ratio
1:20
Untreated Treated
<2.2
0.29
<0.00020
<0.0040
<0.0010
150
390
12
8.6
73
<0.21
<0.42
0.022
< 0.00030
0.0060
< 0.0020
<0.20
0.047
<0.0020
0.0055
58
<0.030
< 0.020
<0.050
<0.020
2.2
< 0.020
<0.20
5.5
< 0.0020
< 0.0050
860
< 0.030
0.057
0.090
< 0.020
19
< 0.020
-78
2,600
15
12.1
54
1:100
Untreated Treated
<0.43
<0.86
0.19
<0.00020
<0.0040
<0.0010
0.69
0.023
<0.0020
<0.0050
19
< 0.030
<0.020
< 0.050
<0.020
1.1
< 0.020
100
330
4.4
9.0
30
<0.10
<0.20
0.0097
<0.00020
<0.0040
<0.0020
0.83
1.4
< 0.0020
<0.0050
410
<0.030
0.020
<0.050
<0.020
4.0
<0.020
-50
980
3.7
11.8
14
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TABLE 22
CHEMICAL ANALYSES OF BET EXTRACT FROM REAGENT MIX
PCBs
Aroclor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh (mV)
Filterable Residue (TDS)(mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
Total Organic Carbon (mg/L)
<0.22
0.0030
<0.00020
<0.0020
<0.0020
0.37
27
<0.0020
<0.0050
540
<0.030
<0.020
<0.050
<0.020
160
<0.020
-69
2,900
<0.50
12.0
36
Solid-to-Liauid Ratio
1:20 1:100
-------
7.3.3.2
Filter Cake
The pH of the pretreatment BET leachates ranged from 3.5 to 3.9. The Eh of the
pretreatment leachates were about 270 to 290 mv for the leachates of all three S/L ratios. The
TDS in the pretreatment leachates increased from 40 mg/L in the 1:100 S/L leachates to 440
mg/L in the 1:4 S/L leachates. The TOC concentrations in the pretreatment leachates also
increased, from 11 to 91 mg/L, as the S/L ratio increased. Oil and grease was detected at 0.53 to
0.65 mg/L in the 1:20 and 1:4 S/L leachates, respectively. No oil and grease was detected in the
1:100 S/L leachate. PCBs were not detected in any of the pretreatment leachates.
i
Ten metals were observed in the pretreatment leachates. Most of these increased in
concentration as the S/L ratios increased from 1:100 to 1:4. Metals exhibiting this trend were
arsenic (0.020 to 0.072 mg/L), lead (0.18 to 0.87 mg.L), zinc (0.020 to 0.27 mg/L), aluminum
(0.37 to 1.9 mg/L), calcium (1.2 to 30 mg/L), and nickel (<0.020 to 0.063 mg/L). Cadmium,
copper, nickel, and sodium were also detected in the 1:4 S/L leachate. Barium decreased from
0.47 mg/L in the 1:100 leachate to 0.14 mg/L in the 1:4 leachate.
All of the leachates from the post-treatment filter cake wastes had pH levels between 11.5
and 11.7 and Eh levels of -82 to -92 mv. The TDS in the post-treatment leachates increased
from 760 mg/L in the 1:100 S/L leachates to 3830 mg/L in the 1:4 S/L leachates. The TOC
concentrations in the post-treatment leachates also increased, from 14 to 140 mg/L, as the solid-
to-liquid ratio increased. Oil and grease was detected at 2.7 to 6.3 mg/L in the 1:20 and 1:4 S/L
leachates. PCBs were not detected in any of the post-treatment leachates.
Seven metals were observed in the post-treatment leachates. Most of these increased in
concentration as the solid-to-liquid ratios increased from 1:100 to 1:4. Metals exhibiting this
trend were arsenic (0.0020 to 0.011 mg/L), barium (0.92 to 6.3 mg/L), chromium (<0.030 to 0.046
mg/L), copper (<0.020 to 0.063 mg/L), calcium (230 to 850 mg/L), and sodium (4.3 to 84 mg/L).
Aluminum decreased from 1.1 mg/L in the 1:100 S/L leachate to 0.20 mg/L in the 1:4 S/L
leachate. Lead, cadmium, nickel, and zinc were not detected in the post-treatment leachates.
7.3.3.3
Filter Cake/Oily Sludge
The pH of the pretreatment BET leachates ranged from 3.7 to 4.4. The Eh of the
pretreatment leachates ranged from 220 to 240 mv for the leachates of all three solid-to-liquid
ratios. The TDS in the pretreatment leachates increased from 110 mg/L in the 1:100 S/L
leachates to 1,800 mg/L in the 1:4 S/L leachates. The TOC concentrations in the pretreatment
99
-------
leachates also increased, from 21 to 200 mg/L, as the solid-to-liquid ratio increased. Oil and
grease increased from 1.3 mg/L in the 1:100 leachates to 3.2 mg/L in the 1:4 S/L leachates. PCBs
were not detected in any of the pretreatment leachates.
Nine metals were observed in the pretreatment leachates. Most of these increased in
concentration as the solid-to-liquid ratios increased from 1:100 to 1:4. Metals exhibiting this
trend were arsenic (0.0083 to 0.042 mg/L), barium (0.48 to 0.83 mg/L), lead (0.14 to 1.7 mg/L),
zinc (0.16 to 2.7 mg/L), calcium (2.1 to 44 mg/L), and cadmium (<0.0050 to 0.036 mg/L).
Aluminum, nickel and copper were also detected in the leachates.
The leachates from the post-treatment filter cake/oily sludge wastes had pH values
ranging from 11.9 to 12.0 and Ens of -93 to -101 mv. The TDS in the post-treatment leachates
increased from 1200 mg/L in the 1:100 S/L leachates to 3,500 mg/L in the 1:4 S/L leachates. The
TOC concentrations in the post-treatment leachates also increased, from 8.0 to 110 mg/L, as the
solid-to-liquid ratio increased. Oil and grease concentrations increased from 0.43 mg/L in the
1:100 leachates to 4.9 mg/L in the 1:4 leachates. PCBs were not detected in any of the post-
treatment leachates.
Seven metals were observed in the post-treatment leachates. Most of these increased in
concentration as the solid-to-liquid ratios increased from 1:100 to 1:4. Metals exhibiting this
trend were arsenic (0.0030 to 0.0080 mg/L), barium (2.6 to 17 mg/L), calcium (440 to 730 mg/L),
and sodium (13 to 250 mg/L). Aluminum decreased from 1.3 mg/L in the 1:100 leachates to 0.23
mg/L in the 1:4 leachate. Copper, which was not detected in the pretreatment samples, and
nickel were detected in the 1:4 leachates. Cadmium, lead, and zinc were not detected in the post-
treatment leachates.
7.3.3.4
Off-Site Area One
The pH of the pretreatment BET leachates ranged from 8.3 to 9.0. The Eh of the
pretreatment leachates ranged from 100 to ,150 mv. The TDS in the pretreatment leachates
increased from 330 mg/L in the 1:100 S/L leachates to 1,100 mg/L in the 1:4 S/L leachates. The
TOC concentrations in the pretreatment leachates also increased, from 30 to 190 mg/L, as the
solid-to-liquid ratio increased. Oil and grease increased from 4.4 mg/L in the 1:100 S/L
leachates to 16 mg/L in the 1:4 S/L leachates. PCBs were not detected in any of the pretreatment
leachates.
100
-------
Six metals were observed in the pretreatment BET leachates. Most of these increased in
concentration as the solid-to-liquid ratios increased from 1:100 to 1:4. Metals exhibiting this
trend were arsenic (0.19 to 0.38 mg/L), calcium (19 to 150 mg/L), and barium (0.023 to 0.11
mg/L). Aluminum, cadmium, and sodium were present at detection limit concentrations in one
or more of the leachates. Lead was not detected in the pretreatment BET leachates.
BET leachates from the post-treatment Off-Site Area One wastes had pH values ranging
from 11.8 to 12.1. The Ehs ranged from -77 mv in the 1:4 S/L leachates to -50 in the 1:100 S/L
leachates. The TDS in the post-treatment leachates increased from 980 mg/L in the 1:100 S/L
leachates to 4600 mg/L in the 1:4 S/L leachates. The TOC concentrations in the post-treatment
leachates also increased, from 14 to 120 mg/L, as the solid-to-liquid ratio increased. Oil and
grease concentrations increased from 3.7 mg/L in the 1:100 S/L leachates to 26 mg/L in the 1:4
S/L leachates. PCBs were not detected in any of the post-treatment leachates.
Nine metals were observed in the post-treatment BET leachates. Most of these increased
in concentration as the solid-to-liquid ratios increased from 1:100 to 1:4. Metals exhibiting this
trend were arsenic (0.0097 to 0.067 mg/L), copper (0.020 to 0.17 mg/L), barium (1.4 to 9.7
mg/L), calcium (410 to 1,000 mg/L), and sodium (4.0 to 80 mg/L). Aluminum decreased from
0.83 mg/L in the 1:100 S/L leachate to <0.20 mg/L in the 1:4 S/L leachate. Selenium, lead, and
nickel were present at detection limit concentrations in one or more of the post-treatment BET
leachates. Zinc was not detected in the post-treatment leachates.
7.3.4
ANS 16.1
The modified American Nuclear Society 16.1 (ANS 16.1) leaching test was performed on
three replicate waste samples of the three treated wastes. This test simulates leaching from the
intact (not crushed) treated waste in contact with rapidly flowing ground water by using a static
sequential leaching method. Leachates were collected at 1, 3, 7, 14, and 28 days during the
leaching test. All of the post-treatment samples maintained their structural integrity throughout
the test period. No contaminants of concern were found in the ANS 16.1 leachates in
concentrations sufficient to allow calculation of a leachability index, as described in the ANS 16.1
procedure. The ANS 16.1 leachate data are summarized in Tables 23 through 25. The detailed
data are presented given in Appendix A, Tables A.30 through A.43.
101
-------
TABLE 23
CHEMICAL ANALYSES OF ANS 16.1 LEACHATE FROM TREATED FILTER CAKE WASTE
PCBs
Aroclor-1242
ArocIor-1260
o
K»
Metals (AA) (mg/L)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh (mV)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
Total Organic Carbon (mg/L)
<0.21
<0.0020
<0.00030
<0.0040
<0.0020
<0.20
0.17
<0.0020
<0.0050
63
<0.030
<0.020
<0.050
<0.020
7.3
<0.020
-20
310
<0.40
10.7
6.6
DAY 3
<0.10
<0.21
<0.0020
<0.00020
<0.0040
<0.0020
0.27
0.19
<0.0020
<0.0050
63
<0.030
<0.020
<0.050
<0.020
5.2
<0.020
-15
270
<0.40
10.9
5.2
<0.22
< 0.0020
<0.00030
<0.0050
<0.0020
0.30
0.22
<0.0020
<0.0050
72
<0.030
<0.020
<0.050
<0.020
4.4
<0.020
-36
310
<0.50
11.0
53
<0.020
<0.040
<0.0020
<0.00020
<0.0040
<0.0010
<0.20
0.25
<0.0020
<0.0050
81
<0.030
<0.020
<0.050
<0.020
5.3
<0.020
-41
340
<0.40
10.7
6.3
DAY 28
<0.22
<0.0020
<0.00020
<0.0040
<0.0020
0.37
0.28
<0.0020
<0.0050
100
<0.030
<0.020
<0.050
<0.020
5.0
<0.020
-57
490
<0.40
113
7.0
-------
TABLE 24
CHEMICAL ANALYSES OF ANS 16.1 LEACHATE FROM TREATED FILTER CAKE/OILY SLUDGE MIXTURE
PCBs
ArocIor-1242
Aroclor-1260
Metals (AA) (mg/L)
Arsenic
Mercury
-Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
Copper
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh (mV)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
Total Organic Carbon (mg/L)
<0.21
<0.0020
<0.00020
<0.0040
<0.0020
0.57
0.32
<0.0020
<0.0050
93
<0.030
<0.020
<0.050
<0.020
17
<0.020
-24
380
<0.40
11.1
6.3
DAY 3
<0.10
<0.20
< 0.0020
<0.00020
<0.0040
<0.0020
0.57
0.35
<0.0020
<0.0050
95
<0.030
<0.020
<0.050
<0.020
11
<0.020
-22
310
<0.40
11.1
5.3
DAY 7
<0.22
<0.0020
<0.00020
<0.0050
<0.0020
0.53
0.37
<0.0020
<0.0050
98
<0.030
<0.020
<0.050
<0.020
9.8
0.037
-33
340
<0.40
11.2
5.3
DAY 14
<0.020
< 0.040
<0.0020
< 0.00020
<0.0040
<0.0010
0.50
0.39
<0.0020
<0.0050
93
<0.030
<0.020
<0.050
<0.020
12
<0.020
-52
350
<0.50
10.9
5.3
DAY 28
<0.10
<0.20
-------
TABLE 25
CHEMICAL ANALYSES OF ANS 16.1 LEACHATE FROM TREATED OFF-SITE AREA ONE WASTE
DAY1
DAY 3
DAY 7
DAY 14
DAY 28
i Vxuo ^g/ is)
Aroclor-1242
Aroclor-1260
Metals (AA) (rag/L)
Arsenic
Mercury
Selenium
Thallium
Metals (ICPES) (mg/L)
Aluminum
Barium
Beryllium
Cadmium
Calcium
Chromium
CoDoer
r r
Lead
Nickel
Sodium
Zinc
Other Chemical Tests
Eh (mV)
Filterable Residue (TDS) (mg/L)
Oil & Grease, infrared (mg/L)
pH (pH units)
Total Organic Carbon (mg/L)
<0.21
<0.42
0.0070
< 0.00020
<0.0040
<0.0020
<0.20
0.33
<0.0020
<0.0050
110
<0.030
<0.020
<0.050
< 0.020
17
< 0.020
-32
610
1.9
11.1
13
<0.21
<0.42
0.0053
<0.00020
<0.0040
<0.0020
0.30
0.42
<0.0020
<0.0050
130
<0.030
<0.020
<0.050
<0.020
11
<0.020
-28
570
1.7
11.4
11
<0.11
<0.22
0.0063
<0.00020
<0.0050
<0.0020
0.37
0.54
< 0.0020
<0.0050
150
<0.030
<0.020
<0.050
<0.020
9.9
<0.020
-48
620
1.9
11.4
13
<0.020
<0.040
0.0063
<0.00030
<0.0040
<0.0010
0.43
0.67
<0.0020
<0.0050
170
<0.030
<0.020
<0.050
<0.020
11
<0.020
-67
740
1.1
11.1
11
<0.11
<0.22
0.0080
<0.00020
<0.0040
<0.0020
0.73
0.90
<0.0020
<0.0050
220
<0.030
<0.020
<0.050
<0.020
13
<0.020
-78
870
3.2
11.7
20
-------
7.3.4.1
Filter Cake
The pH remained essentially constant throughout the leach test, ranging from 10.7 to 11.3
pH units. The Eh also exhibited little change over the test period, increasing from about -15 to -
57 mv. Oil and grease was not found in any of the ANS 16.1 leachates generated from the post-
treatment filter cake wastes. The total organic carbon remained essentially constant (5.2 to 7.0
mg/L) over the test period. The total dissolved solids of the post-treatment leachates ranged
from 270 to 490 mg/L.
PCBs were not detected in the leachates. The only metals detected in the leachates were
aluminum (<0.20 to 0.37 mg/L), barium (0.17 to 0.28 mg/L), calcium (63 to 100 mg/L), and
sodium (4.4 to 7.3 mg/L). Silver and lead were each found at detection limit concentrations in
only one of the fifteen ANS 16.1 leachates analyzed.
7.3.4.2
Filter Cake/Oily Sludge
The pH of the filter cake/oily sludge ANS 16.1 leachates ranged from 10.9 to 11.3. The
Eh ranged from -24 mv in the day 1 leachates to -62 mv in the day 28 leachates. Oil and grease
was not detected in any of the ANS 16.1 leachates. The total organic carbon and the total
dissolved solid remained essentially constant over the test period, ranging from 5.3 mg/L to 6.3
mg/L and 310 mg/L to 380 mg/L, respectively.
PCBs were not detected in the filter cake/oily sludge ANS 16.1 leachates. Aluminum
(0.50 to 0.70 mg/L), barium (0.32 to 0.40 mg/L), calcium (88 to 98 mg/L), and sodium (9.8 to 17
mg/L) were found in the ANS 16.1 leachates. Silver, thallium and zinc were found at detection
limit concentrations in one of more of the leachates.
7.3.4.3
Off-Site Area One
The pH of the Off-Site Area One ANS 16.1 leachates ranged from 11.1 to 11.7. The Eh
values ranged from -28 mv to -78 mv. The oil and grease content of the leachate ranged from
1.1 mg/L to 3.2 mg/L. The TOC varied from 11 mg/L to 20 mg/L. Total dissolved solids
increased from 570 mg/L to 870 mg/L.
PCBs were not detected in the Off-Site Area One ANS 16.1 leachates. Barium (0.30 to
0.90 mg/L) and calcium (110 to 220 mg/L), increased slightly throughout the leach test. Sodium
105
-------
(9.9 to 17 mg/L) and arsenic (0.0053 to 0.0080 mg/L) remained relatively constant in all 15
leachates.
7.4
MORPHOLOGICAL TESTS
The Demonstration Plan provides for periodic petrographic examination of cement-
solidified waste samples over the next several years. Data from these analyses will determine the
extent to which several routine characteristics of structural concrete are present or change:
• Adequacy of curing
• Degree of carbonation
• Degree of hydration and nature of hydration products
• Weather effects on the integrity of the cemented mass
• Degree of mixing of waste with cementitious materials
At the field demonstration, cast cylinder molds of each of the three wastes treated, plus
molds of the sand reagent blank, were prepared. The absence of reliable published methods for
petrographic examination and sample preparation of cement-solidified oily waste required in-
depth consultation with experts in this field. As a result, an array of laboratory tests was
devised, to be conducted by both U.S. EPA contractor laboratories and the U.S. Army Corps of
Engineers Waterways Experiment Station (WES). These tests include:
• X-ray radiography of cast cylinders (of cement-solidified waste)
• Sonic pulse analysis of cast cylinders
• Void characterization on polished surface of cast cylinders
• Preparation and examination of thin-sections of cast cylinders
• X-ray diffraction analysis of minerals in cast cylinders
• Electron microscope examination
Three cylinders of each of the post-treatment filter cake, filter cake/oily sludge, Off-Site
Area One, and the reagent mix/control samples were initially submitted for X-ray radiographic
analyses. At the time of preparation of this report, only preliminary X-ray radiographs of these
samples had been completed. These clearly showed numerous small round spots throughout the
three cylinders photographed in preliminary work. Since the photographs were at scale, it could
106
-------
be seen that the observed spots corresponded, both in approximate size and distribution, to the
dark oily spots observed in the treated waste monoliths (see Section 7.5). These early observations
lend credibility to the representativeness of cast cylinders to the larger treated waste monoliths.
Each of the twelve cylinders mentioned above will also be subjected to sonic pulse
analysis. This test will be used to assess the long-term stability of the cylinders. Four of these
cylinders, one from each area plus a reagent mix, will be retained for periodic long-term analysis.
Longitudinal slabs approximately 75 x 150 mm in size and 20 mm in thickness will be cut
from the above cylinders. One slab will be prepared from the reagent mix. One slab will be
prepared from each of the two cylinders for each treatment area. Slab preparation will entail
cutting and then polishing one surface of each slab.
The polished slabs will be analyzed to determine the distribution of air and waste-filled
voids in the surface of the slabs. These slabs will then be analyzed to assess incorporation of oily
material by a technique that measures ultraviolet reflectance on the polished surface. X-ray
radiographic analysis will also be performed on the slabs. Point counts of voids will be
performed using a stereoscopic microscope and computerized image analysis techniques. The
prepared slabs will also be photographed.
Scanning electron microscope (SEM) analysis will be conducted to determine
morphological features of the solidified matrix under moderately high magnification (lOOx-
lOOOx). This analysis will include visual interpretation of the slab surface as well as a
determination of the distribution of diatomaceous earth in cylinders containing the filter cake
waste.
X-ray diffraction (XRD) analysis will be conducted to determine the presence of
crystalline material in the solid waste matrix. The XRD analysis will also be used to help
identify the types of cementitious hydration products in the solidified materials.
Methods for preparing thin sections of the solidified wastes will be investigated. This
task is complicated by the presence of oil in the solidified waste, as cutting the thin sections is
expected to disturb the oil. After the sections have been prepared, they will be analyzed and
photographed using a petrographic microscope with transmitted light.
107
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7.5
LONG-TERM TESTS
This section discusses the planned long-term tests on the treated waste materials from the
Soliditech demonstration. These include the Waste Interface Leaching Test (WILT), TCLP and
EP extraction tests, and physical stability testing of the treated waste material.
7.5.1
Waste Interface Leaching Test
The purpose of the WILT is to determine if the Soliditech process will reduce the long-
term teachability of the waste to safe levels. The WILT consists of two sizes of solidified
cylinders (3"d x 18"h and 6"d x 18"h) from each of three solidified wastes (Off-Site Area One,
filter cake, and filter cake/oily sludge). Leachate will be collected and analyzed from the WILT
on a biweekly basis for a period of one year. The first 16 weeks of WILT results are contained as
preliminary data in Appendix G of this report. Each of three replicate cores of each type of
waste was placed in an individual HDPE tank and the annular space between the core and the
container was filled with acid-washed sand. A 1-inch layer of sand was added to the top of the
column to disperse the leaching fluid (distilled water) uniformly over the cross-sectional area of
the waste core. Leachate from each column was collected in a Tedlar* bag fitted to the base of
the tank. Distilled water was added to saturate each column to the surface level of each column.
Each column remained saturated over the two-week interval prior to sampling. The leachates
were analyzed for pH, Eh, metals, and PCBs.
PCBs, lead, and zinc were not detected in the WILT leachates from the solidified wastes.
The cumulative amounts (mass/cm2) of aluminum, barium, calcium, TOC, and TDS leached from
the solidified wastes over a 16 week period are shown in Table 26. TSD concentrations leached
from the solidified wastes, which are indicative of the porosity of the solidified wastes, were
lowest from the filter cake/oily sludge mixture. These results are supported by the physical test
data which indicate that the filter cake/oily sludge mixture is the least permeable of the solidified
wastes (Table 14). Concentrations of metals and organics in leachate from the WILT are reported
in Appendix G. All elemental and organic concentrations were below levels of concern for
protection of groundwater quality.
7.5.2
TCLP and EP Extracts of Solidified Waste
TCLP and EP tests will be performed on molded waste samples from three types of waste
(Off-Site Area One soil, filter cake, and filter cake/oily sludge mixture). Aging periods for the
molded waste samples will consist of 28 days, 6 months, and 1, 2, and 5 years. Three replicate
108
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TABLE 26
WILT TEST RESULTS THROUGH WEEK 16
Parameter
PH
PCBs8 (Mg/cm2)
Metals8 (Mg/cm2)
Aluminum
Barium
Calcium
Lead
TQCa (Mg/cm2)
TDS" (mg/cm2)
Off-Site
Area One
Column
Small Large
12.1 11.5
NDb ND
Filter Cake
Column
Small Large
11.4 11.3
ND ND
Filter Cake/
Oily Sludge
Column
Small Large
11.6 11.4
ND ND
15
20
3400
ND
NCC
NC
29
3.9
1100
ND
520
13.5
17
9.4
2680
ND
ND
NC
IS
7.6
2640
ND
446
15.5
25
8.0
- 1380
ND
NC
NC
33
4.1
930
ND
147
6.3
Notes:
Cumulative amount leached from cylinders over 16 weeks is expressed as mass per cm of
cylinder surface area. The small cylinders are 3 inches in diameter and 18 inches in height.
The large cylinders are 6 inches in diameter and 18 inches in height.
Not detected.
Not calculable.
109
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samples of each waste type will be extracted at each time period. For each of these cases, a
single core will be used for TCLP and EP extractions, resulting in a total of 60 cores over the
entire test period.
Results from the TCLP and EP tests will provide data on the relative concentration of
contaminants in extracts over a period of five years. These results will indicate any changes in
extract toxicity that may be attributed to aging or weathering of the solidified waste.
7.5.3
Physical Stability of Treated Waste Monoliths
Initial observations indicate that, of the following characteristics, some will be easier to
assess than others. Some features may be disregarded or others added at future observation
points.
7.5.3.1
Surface Spalling
Upon removal of the plywood sides of the molds, a thin, dusty patina was present on the
surface of the treated waste monoliths. An imprint of the texture of the plywood surface was
obvious in this patina. This feature appeared to be a few millimeters in thickness and was easily
removed with an armstrong wire brush. The presence of this material at the interface with the
plywood container emphasizes the need to be cautious in describing monolith properties without
first being sure that the container or other accessory to this demonstration does not contribute
artifacts.
Block 1, containing the reagent mix or control sample, appeared to be similar to a
competent commercial concrete, with no particularly notable features. All the blocks with waste
in the composition had a thin veneer that appeared to form from splashing onto the inside of the
plywood form when the fluid mix was discharged into each form. This material was easily
chipped off with light hammer blows after the plywood forms were removed. Easily removed
thin layers of solidified waste were hand-chipped off the top edges of all blocks prior to stacking
for long-term evaluation.
Blocks 2, 3, and 4 contained black masses, several centimeters in dimension, over areas of
tens of centimeters, on most faces of these blocks. These masses appeared to consist of relatively
unmixed waste material. This was the first waste batch mixed, and thorough mixing may not
have been achieved in this batch. Observations at the next time interval should include note of
these masses.
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Blocks 5-10 contained no particular or notable features. The solidified waste appeared
uniform as a blocky mass.
Blocks 11-14 also contained no particular or notable features.
7.5.3.2
Grain Exfoliation
No initially notable grain looseness was noted on any of the blocks except for the dusty
surface adjacent to the plywood form sides. As noted previously, this was easily removed with a
hand-operated wire brush, into a light dusty form. Other than occasional brushing on a few
blocks, no attempt was made to remove this surface material.
7.5.3.3
Crack and Fissure Development
Except for Block 1, nearly all blocks containing waste exhibited circular cracks near the
corners of the top surface. These are believed to be normal stress-relief cracks resulting from the
use of square box forms. These weaknesses suggest that round forms be used in any subsequent
construction of treated waste monoliths. Blocks 3, 5, and 11 exhibited these corner cracks one
day after pouring the fluid waste, with Block 3 being most pronounced.
The northeast corner of Block 5 exhibited a severe crack with separation of a triangular
corner volume approximately 6" in dimension and at least 12" length after Block 10 was placed
upon it in the long-term stack.
No remarkable cracks or fissures were seen on any of the faces of the blocks after
removing the plywood forms.
7.5.3.4
Oxidative Discoloration
No clear indications of oxidative processes were noted either after initial setting of the
cement-solidified waste or after the 28-day curing period. A lightening of color of the blocks
was noted within fractions of an hour after the plywood forms were removed. This was
attributed to air-drying of the block surfaces.
Blocks 5 through 10, comprised of the solidified filter-cake waste pile material, were the
darkest in overall color. Blocks 2 through 4 contained large black masses visible on all faces; as
indicated earlier, these appeared to be unmixed masses of oily material.
Ill
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On many of the blocks, where the plywood-surface-influenced finish of block faces or
corners were chipped away, numerous rounded black spots were obvious. These appeared to be
oil- or grease-filled voids; or alternatively, small volumes of oily waste surrounded by the
cementitious matrix. The spots varied in size up to several millimeters. Some spots were
surrounded by a "halo", indicating that liquid or volatile components of the oily matrix had
migrated radially outward from the original globule. These halos ranged both in clarity and size,
up to a few centimeters in diameter. At the time the blocks were stacked for long-term
evaluation, the texture and composition of the black spots were not probed or assayed in the
field, nor were samples specifically taken for detailed assay. These features will be examined as
part of the long-term monitoring study.
7.5.3.5
Salt Efflorescence
A significant accumulation of white salt was observed on the top surface of Block 8. This
accumulation was present in the concave depressions remnant from the removal of sample
material from the block surface after the fluid mix was discharged from the mixer. Although
other blocks may have contained salt accumulations, none was as concentrated as that of Block 8.
This material was undisturbed and not sampled at the time the blocks were stacked for long-term
evaluation. This material will be examined and sampled during long-term monitoring activities.
7.5.3.6
Pore Characterization
This parameter is vividly illustrated by the presence of the black spots noted previously.
Initial conclusions represent these spots as oil- or grease-filled voids or pores. This must be
verified by laboratory examination of similar features in the cast cylinders taken for laboratory
study. This detailed examination should determine whether the black spots are indeed filled
voids or waste globules surrounded by cementitious matrix. No clearly visible air voids could be
seen in the treated waste monoliths. Planar cracks of various sizes were occasionally visible in
some blocks. The major cracks were described earlier.
7.6
MATERIALS BALANCE
Table 27 presents material balance information for each of the four treatment runs
performed by Soliditech during the demonstration. The data in this table are based upon
information collected during the demonstration by Soliditech (Soliditech, 1989a). Table 28 gives
the observed volumes and weights of the treated waste monoliths.
112
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TABLE 27
MATERIALS BALANCE
Estimated Weights of Materials in Pounds
Filter Cake/
Reagent Mixture Oily Sludge
Filter Cake Off-Site Area
Waste Material
Volume (yd3)
Type II Cementcb>
Urrichem
Additives
Water
TOTAL ESTIMATE WEIGHT
Material in Large Forms
Laboratory Samples
Field Tests
Residual(c>
Screened Material
Weight Differential
Percent Weight Difference(9>
a Clean sand used
800(a)
0.24
442
8.96
16.5
154
1,420
Measured
1,250
31.0
0
50
1,330
0.455
90
6.7
3,950
1.94
4,970
39.2
140
666
9,760
Weights of
8,410
305
144
250
9,110
3.08
650
7.1
rather than waste material
11,200
5.83
4,920
111
167
2.687
19,100
Products in Pounds
15,400
266
188
250
16,100
6.25
3,000
18.6
for this test run.
According to Soliditech, fluffing of the cement may cause the
9,100
4.28
4,540
90.7
136
1.830
15,700
10,900
291
206
300
11,700
4.10
4,000
34.2
cement weight
--, , . .
values to be as much as 5 percent high.
According to Soliditech, the residual in the mixer after treatment might be as
much as 1/10 cubic-yard, or approximately 250 pounds in the large mixer and
approximately 50 pounds in the small mixer. We will assume the maximum
amount for each test run. The mixer was not cleaned prior to treating the Off-Site
Area One waste, so no correction was made to that value.
The residual of the preceding test run was allowed to remain in the mixer and was
treated with this test run. It was assumed that the residual weight was equal for
each of these test runs. Thus, the amount of residual remaining in the mixer after
treatment should equal the amount of residual in the mixer prior to treatment and
no correction was needed.
Approximate amount of material removed by screening according to Soliditech.
The total cubic-yards measured plus volume of treated material collected for
laboratory and field experiments.
Weight Differential divided by Total Measured Weight times 100.
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TABLE 28
OBSERVED VOLUME AND WEIGHT OF TREATED MATERIAL
Plywood Form Number(a)
Reagent Mix/Control
1
Oily Sludge/Filter Cake
2
3
4
Filter cake
5
6
7
8
9
10
lOa
Off-Site Area One Soil
Volume of Material
Before Cure After Cure
1248
3116
3228
2070
2512
2700
2958
2380
2432
2026
342
1258
3080
3186
2062
2484
2668
2934
2354
2406
2004
374
11
12
13
14
0.972
1.08
1.06
0.806
2644
3034
2940
2256
2608
3000
2910
2240
TOTALS
13.3
35,886
35,700
See Section 6.3.2 for a description of the treated waste material contained in each
form.
Volume is expressed in cubic-yards.
Net weight is expressed in pounds. These weights were obtained by weighing the
treated waste monoliths both before and after the 28 day curing period. No
attempt was made to explain the small variations in the two field weights.
114
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The waste content of the treated material ranged from 40 to 59 percent by weight, with
an average of 52 percent. The volume increase of the waste due to treatment ranged from no
increase to 59 percent increase, with an average of 22 percent. The bulk density of the treated
waste increased by 25 to 41 percent, with a 31 percent average.
It should be noted that the weights of the ingredients for each of the four runs were
found to be greater in sum than the weight of the treated material. This can be attributed to
several factors. The amount of waste material treated in each of the waste runs, particularly the
Off-Site Area One soil, was probably overestimated. The actual weight of cement added to each
mixture may also be overestimated by as much as 20 percent. It is unlikely that the weight of the
water, Urrichem, or additives is significantly different than that reported, because these
ingredients were either carefully measured or metered into the mixture.
7.7
CONCLUSIONS
The unconfined compressive strength values, very low permeability, and high resistance
to wet/dry and freeze/thaw deterioration demonstrates a high degree of physical stability of the
three treated wastes. Although the treated waste had a higher bulk density than the raw waste, a
small volume increase accompanied the solidification/stabilization process.
The concentrations of all contaminants found in the EP and TCLP extracts of treated
samples are low. It is significant that lead, as measured by TCLP, EP, ANS 16.1, and WILT
procedures, is barely detectable in extracts of treated wastes. This indicates a high degree of
stability in the solidified/stabilized matrix of treated waste. The BET data confirm the stability
of the treated wastes against leaching loss of lead and arsenic. The low amounts of contaminant
solutes found in the preliminary WILT leachates confirm the parallel findings in the TCLP, EP,
BET, and ANS 16.1 extraction tests.
Measurable amounts of arsenic, barium, chromium, copper, lead, nickel, and zinc
appeared in the treated wastes. The source of these elements is believed to be Portland cement.
Decreases in loss-on-ignition are most likely due to dilution by the added cement.
The absence of any mechanical equipment problems during the demonstration illustrated
the reliability of the Soliditech system. After the equipment operator gained familiarity with
waste materials at this site, the process mixed all components into a homogenous solidified
product.
115
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8.0 COST OF DEMONSTRATION
The cost of demonstrating Soliditech's solidification/stabilization process at the Imperial
Oil site was approximately $958,300. This cost includes site characterization and preparation,
demonstration planning and field work, chemical analyses, and report preparation. The
developer's portion of this cost was $232,600. The balance of $725,700 was allocated to the U.S.
EPA SITE Program.
8.1
U.S. EPA SITE CONTRACTOR COSTS
Technical support to the U.S. EPA SITE program for the evaluation of the Soliditech
technology was provided by a contractor. Each SITE project is divided into two phases —
planning (Phase I) and demonstration (Phase II). Phase I costs are actual costs; Phase II costs
include actual costs plus labor estimates through the completion of report preparation. Specific
activities under each phase and a cost breakdown for each phase are presented below (all costs are
rounded to the nearest $100).
8.1.1 Phase I: Planning Stage
Phase I activities included:
• Solidification/stabilization technology review
• Protocol evaluation
• Site sampling and treatability testing
• Development of the demonstration plan
• Site subcontractor procurement
Costs for Phase I activities are summarized below:
Labor $ 82,200
• Equipment and supplies 9,300
Travel 8,300
• Chemical analyses 29,200
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8.1.2
Phase II: Demonstration Stage
Phase II activities included: . . . •
• Mobilization and site preparation
• Sample collection and field oversight
Sample processing after the 28-day curing period
• Chemical analyses
• Report preparation
Costs for Phase II activities are summarized below:
Labor $244,100
• Equipment and supplies 63,400
Travel/transportation 21,400
• Chemical analyses 261,900
Miscellaneous 5,900
Labor costs include estimates through report preparation. Miscellaneous costs include the
demonstration area security and the decontamination facility. Transportation costs include
equipment mobilization and demobilization.
8.2
DEVELOPER (SOLIDITECH) COSTS
The costs presented in this section were provided by Soliditech (Soliditech, 1989b). These
costs were based upon all expenses incurred by Soliditech in preparing for and conducting the
SITE demonstration.
Labor
Laboratory
Travel
Equipment
Transportation
Raw materials
Miscellaneous
$ 21,600
7,400
10,600
177,000
13,000
1,300
1,700
117
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Equipment and miscellaneous costs include such one-time costs as health and safety
equipment and training. Raw materials costs include pozzolan (portland cement), Urrichem, and
other proprietary additives. Transportation costs include equipment mobilization and
demobilization.
118
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Society, LaGrange Park, Illinois, 1986.
ASTM, 1987. Annual Book of ASTM Standards. American Society of Testing and Materials,
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C6te, 1988. Draft Investigation of Test Methods for Solidified Waste Characterization (TMSWC).
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Burlington, Ontario, 1988.
E.G. Jordan Co., 1987. Draft Phase 1 Sampling Report, Imperial Oil Co., Inc./Champion
Chemicals Site, for New Jersey Department of Environmental Protection, July 1987.
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PRC, 1988a. Memorandum: SITE Trip Report: Preliminary Sampling, Imperial Oil Site, June
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Radian, 1988. SITE Preliminary Sampling Report, Imperial Oil Company, Inc./Champion
Chemicals Site, Prepared by Radian Corp., Austin, Texas, October 1988.
Soliditech, 1987. Proposal for Development of Innovative Technologies for Hazardous Waste Site
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Bruckdorfer of Soliditech Inc., to Ken Partymiller, PRC EMI Soliditech Demonstration
Project Manager, March 21, 1989.
Soliditech, 1989b. Economic Analysis of Soliditech SITE Project. Prepared by Soliditech, Inc.,
March 23, 1989.
U.S. EPA, 1978. Field Laboratory Methods Applicable to Overburdens and Minesoils, U.S. EPA
2-78-054, March 1978.
U.S. EPA, 1979. Methods for the Chemical Analysis of Water and Wastes. U.S. EPA, 4-79-020,
March 1979.
119
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U.S. EPA, 1985. Method 680: Determination of Pesticides and PCBs in Water and Soil/Sediment
by GC/MS, U.S. EPA, November 1985.
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1C, and II, Third Edition, U.S. EPA Document Control Number 955-001-00000-1,
November 1986. t
U.S. EPA, 1988. Draft Protocol for a Solidification and Stabilization Demonstration Plan, Office
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