EPA/540/R-92/QQ2
JUNE 1992
TECHNOLOGY EVALUATION REPORT
THE CARVER-GREENFIELD PROCESS
DEHYDRO-TECH CORPORATION
RISK REDUCTION ENGINEERING LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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Notice
The information in this document has been prepared for the U.S. Environmental Protection
Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program under Contract No. 68-
CO-0047. This document has been subjected to the EPA'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 an endorsement or recommendation of use.
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Foreword
The Superfund Innovative Technology Evaluation (SITE) Program was authorized in the
Superfund Amendments and Reauthorization Act of 1986 (SARA). The SITE Program is
administered by the U.S. Environmental Protection Agency (EPA) Office of Research and
Development (ORD). The purpose of the SITE Program is to accelerate the development and use of
innovative cleanup technologies applicable to Superfund and other hazardous waste sites. This is
accomplished through demonstrations designed to provide performance and cost data on selected
technologies.
A field demonstration was conducted under the SITE Program to evaluate the Dehydro-Tech
Corporation Carver-Greenfield Process*. The technology demonstration took place at EPA's Edison,
New Jersey facility. The demonstration effort was directed to obtain information on the performance
and cost of the technology regarding its utility for treating hazardous wastes. Documentation consists
of two reports: (1) an Applications Analysis Report, which interprets the data and discusses the
potential applicability of the technology, and (2) this Technology Evaluation Report, which describes
the field activities and laboratory results.
A limited number of copies of this report are available at no charge from EPA's Center for
Environmental Research Information, 26 West Martin Luther King Drive, Cincinnati, Ohio, 45268.
Requests should include the EPA document number found on the report's cover. When the limited
supply is exhausted, additional copies can be purchased from the National Technical Information
Service, Ravensworth Building, Springfield, Virginia 22161, 703/487-4600. Reference copies are
available at EPA libraries in the Hazardous Waste Collection. Furthermore, the SITE Clearinghouse
hotline at 800/424-9346 or 202/382-3000 in Washington, D.C., can supply information about the
availability of all SITE reports.
E. Timothy Oppelt, Director
Risk Reduction Engineering Laboratory
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Abstract
This report evaluates the ability of Dehydro-Tech Corporation's (DTC) Carver-Greenfield
Process to separate oil contaminated waste drilling muds to their constituent solids, oil and water
fractions.
The Carver-Greenfield Process (C-G) was developed by DTC in the late 1950's and is
licensed in over 80 plants worldwide. The technology is designed to separate solid-liquid mixtures
into three product streams: a clean, dry solid; a water product substantially free of solids and
organics; and a concentrated mixture of extracted organics (indigenous oil). A mobile pilot plant was
used for the demonstration. Waste material was first slurried with a solvent to fluidize the waste and
extract soluble organic contaminants to the solvent phase. The slurry was then dried in a single stage
evaporator. Separation of the solids from the dried slurry was accomplished by centrifugation. The
resultant cake was reslurried, heated, and centrifuged twice more to simulate a three-stage extraction
process. Cake produced after the third extraction was further desolventized in a high temperature
stripping process to produce a dry solids product. Process condensates were manually separated into
water and solvent phases. Although not part of the demonstration, centrate and extracted indigenous
oils typically undergo fractional distillation to recover the solvent for recycling to the fluidization
operation and to separate the indigenous oils for subsequent disposal.
The C-G Process demonstration was conducted at EPA's Edison, New Jersey facility in
August 1991. Waste drilling muds from the PAB Oil and Chemical Services, Inc. (PAB Oil), site in
Vermilion Parish, Louisiana were processed in a mobile pilot plant. PAB Oil, which ceased
operation in 1983, operated three oil drilling mud separation pits from which the waste material used
in the demonstration was collected.
The demonstration consisted of two test runs. Both test runs produced a dry solids product
similar to bentonite in appearance. Indigenous oil removal was 91.8 percent and 88.3 percent in Test
Runs 1 and 2, respectively. Indigenous total petroleum hydrocarbon and water removal was greater
- than 99.9 percent in both test runs. The dry solids product complied with RCRA Toxicity
Characteristic (TC) limits for metals, volatile organics, and semivolatile organics.
During the demonstration, the C-G Process pilot plant experienced no major operational
problems. The most significant deviation from the intended operation was the desolventizer
temperature. The operating temperature of the desolventizer should be 225 to 350°F, but due to a
malfunction in the desolventizer's thermal oil jacket during shakedown runs, the actual operating
temperature was 185 to 220°F. The lower temperature may have contributed to slightly higher than
predicted solvent concentrations in the final solids product.
EPA has projected treatment costs for the PAB Oil site drilling muds by the C-G Process to
be $523 per wet ton of waste. Of this total, $221 per ton is technology specific and $302 per ton is
site specific. Of the site specific costs, $240 per ton is for incineration of the indigenous oil extracted
from the waste.
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TABLE OF CONTENTS
Section
NOTICE
FOREWORD
ABSTRACT
LIST OF FIGURES
LIST OF TABLES
ACKNOWLEDGEMENTS
LIST OF ACRONYMS AND ABBREVIATIONS
1.0 EXECUTIVE SUMMARY 1
1.1 OVERVIEW OF THE CARVER-GREENFIELD SITE DEMONSTRATION ... 2
1.2 TECHNOLOGY DESCRIPTION 3
1.3 ANALYTICAL RESULTS 5
1.4 QUALITY ASSURANCE PROCEDURES 8
1.5 CONCLUSIONS 9
1.6 COMMENTS 10
2.0 INTRODUCTION 11
2.1 TECHNOLOGY EVALUATION REPORT ORGANIZATION 11
2.2 BACKGROUND 12
2.2.1 SITE Program 12
2.2.2 Demonstration Program Objectives 13
2.2.3 Technology Evaluation Criteria 13
2.2.4 Demonstration Preparation 14
2.2.5 Project Organization and Responsibilities 15
3.0 SITE BACKGROUND 16
3.1 PAB OIL SITE 16
3.1.1 Site History 16
3.1.2 Site Characteristics 17
3.1.3 Site Contamination 19
3.2 DEMONSTRATION FACILITY 20
4.0 CARVER-GREENFIELD PROCESS DESCRIPTION 22
4.1 PROCESS DESCRIPTION 22
4.1.1 Slurrying 23
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iii
viii
ix
xi
xii
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Section
TABLE OF CONTENTS
Page
4.1.2 Evaporation 24
4.1.3 Solids Separation 24
4.1.4 Desolventization 25
4.1.5 Distillation 25
4.1.6 Oil/Water Separator 25
4.1.7 Vent Gases 25
4.2 MOBILE PILOT PLANT 26
4.2.1 Slurrying 26
4.2.2 Evaporation 29
4.2.3 Solids Separation 29
4.2.4 Desolventization 30
4.2.5 Distillation 30
4.2.6 Oil/Water Separation 30
4.2.7 Vent Gases 30
4.3 COMPARISON WITH COMMERCIAL SCALE SYSTEMS 31
5.0 DEMONSTRATION PROCEDURES 33
5.1 DEMONSTRATION PREPARATION 33
5.2 DEMONSTRATION OPERATIONS 33
5.2.1 Waste Handling 35
5.2.2 Operating Plan 36
5.3 SAMPLING PROGRAM 40
5.3.1 Sampling Locations and Parameters 40
5.4 SAMPLE FREQUENCY DESIGN 48
5.5 SAMPLING METHODS 49
5.6 MONITORING POINTS AND OPERATING RANGES 49
6.0 PERFORMANCE DATA AND EVALUATION 56
6.1 TREATABILITY TESTS 56
6.2 DEVIATIONS FROM DEMONSTRATION PLAN 58
6.2.1 Modifications to the Demonstration Plan Content 59
6.2.2 Summary of Pilot Plant Shakedown and Trial Runs 59
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TABLE OF CONTENTS
Section Page
6.2.3 Changes Made to the Pilot Plant Operating and Monitoring Plan 61
6.2.4 Modifications to the Sampling and Analysis Plan 64
6.3 OPERATING CONDITIONS 65
6.4 RESULTS OF BLANK RUN 67
6.5 FEEDSTOCK CHARACTERIZATION 71
6.6 SEPARATION OF SOLIDS, OIL, AND WATER MATRICES BY
THE CARVER-GREENFIELD PROCESS 77
6.7 FATE OF METALS THROUGH THE
CARVER-GREENFIELD PROCESS 79
6.8 FATE OF VOCs AND SVOCs THROUGH THE CARVER-GREENFIELD
PROCESS 80
6.9 TCLP ANALYSIS OF FINAL PRODUCT 82
6.10 SUMMARY OF RESIDUALS CHARACTERISTICS 82
6.11 MATERIAL BALANCES 84
6.11.1 Gross Material Balance 86
6.11.2 Material Balance of Selected Parameters 90
7.0 QUALITY ASSURANCE/QUALITY CONTROL 94
7.1 ANALYTICAL METHODS 94
7.2 SAMPLING HOLDING TIMES 97
7.3 MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERIES 103
7.4 LABORATORY DUPLICATES 103
7.5 REFERENCE STANDARDS 105
7.6 FIELD AND EQUIPMENT BLANKS 105
7.7 METHOD BLANKS 105
7.8 LABORATORY INSTRUMENT CALIBRATION 106
7.9 DETECTION LIMITS 106
7.10 QUALITY ASSURANCE CONCLUSIONS 113
8.0 COST OF DEMONSTRATION 114
8.1 EPA SITE CONTRACTOR COSTS 114
8.1.1 Phase I: Planning 114
8.1.2 Phase II; Demonstration 115
REFERENCES . . 116
APPENDIX A: DEMONSTRATION MONITORING DATA
APPENDIX B: SUMMARY OF ANALYTICAL RESULTS
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ANALYTICAL PROCEDURES FOR SOW AND SOLVENT
QUALITY CONTROL/QUALITY ASSURANCE DATA
EQUIPMENT CALIBRATION DOCUMENTATION
VII
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LIST OF FIGURES
Ejses Ease
1-1 SIMPLIFIED DIAGRAM OF SITE REMEDIATION BY THE CARVER-GREENFIELD
PROCESS AS TESTED IN THE DEMONSTRATION 4
3-1 LAYOUT OF PAB OIL AND CHEMICAL COMPANY SITE 18
4-1 PROCESS FLOWSHEET FOR THE MOBILE PILOT PLANT 27
4-2 GENERAL PROCESS SCHEMATIC FOR COMMERCIAL CARVER-GREENFIELD
SYSTEMS 32
5-1 PLOT PLAN OF CARVER-GREENFIELD SITE DEMONSTRATION AT EDISON,
NEW JERSEY 34
5-2 LABORATORY TRAILER USED FOR THE CARVER-GREENFIELD
DEMONSTRATION , 38
5-3 FLOWSHEET FOR THE MOBILE PILOT PLANT SHOWING SAMPLING
LOCATIONS 41
5-4 FLOWSHEET FOR THE MOBILE PILOT PLANT SHOWING MONITORING
LOCATIONS 51
6-1 COMPONENTS OF MATERIAL BALANCE AROUND THE CARVER-GREENFIELD
PROCESS (BATCH OPERATION) 85
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LIST OF TABLES
Table Page
4-1 MOBILE PILOT PLANT EQUIPMENT LIST 28
5-1 SUMMARY OF SAMPLE COLLECTION AND ANALYSIS . . . . 42
5-2 SUMMARY OF SAMPLING METHODS AND CONTAINER REQUIREMENTS .... 50
5-3 CARVER-GREENFIELD PROCESS MONITORING LOCATIONS 52
6-1 SUMMARY OF CRITICAL OPERATING DATA . . 66
6-2 CARVER-GREENFIELD PROCESS BLANK RUN AVERAGE ANALYSIS DATA ... 69
6-3 COMPOSITION OF WASTE FEEDS 72
6-4 CARVER-GREENFIELD PROCESS AVERAGES FOR TEST RUN 1 73
6-5 CARVER-GREENFIELD PROCESS AVERAGES FOR TEST RUN 2 75
6-6 OIL REMOVAL EFFICIENCY OF EXTRACTIONS 78
6-7 INDIGENOUS OIL AND TPH REMOVALS 79
6-8 SUMMARY OF SIGNIFICANT METALS (DRY WEIGHT BASIS) 80
6-9 SUMMARY OF VOC AND SVOC RESULTS 81
6-10 GROSS MATERIAL BALANCE FOR BLANK RUN 87
6-11 GROSS MATERIAL BALANCE FOR TEST RUN 1 88
6-12 GROSS MATERIAL BALANCE FOR TEST RUN 2 89
6-13 MATERIAL BALANCE ON INDIGENOUS OIL FOR CARVER-GREENFIELD
PROCESS DEMONSTRATION 91
6-14 MASS BALANCE ON METALS FOR TEST RUN 1 92
6-15 MASS BALANCE ON METALS FOR TEST RUN 2 93
7-1 QA OBJECTIVES FOR LIQUID SAMPLE MATRIX 95
7-2 QA OBJECTIVES FOR SOLID AND SLURRY MATRICES 96
7-3 DATES OF SAMPLE COLLECTION, PREPARATION, AND ANALYSIS -
BLANK RUN 98
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LIST OF TABLES (CONTINUED)
Table Page
7-4 DATES OF SAMPLE COLLECTION, PREPARATION, AND ANALYSIS
-TEST RUN! • 99
7-5 DATES OF SAMPLE COLLECTION, PREPARATION, AND ANALYSIS
-TEST RUN 2 101
7-6 SUMMARY OF QA/QC RESULTS FOR MATRIX SPIKE, DUPLICATE
ANALYSIS, AND REFERENCE STANDARDS 104
7-7 RANGE OF DETECTION LIMITS FOR METALS 107
7-8 RANGE OF DETECTION LIMITS FOR VOLATILE ORGANICS 108
7-9 RANGE OF DETECTION LIMITS FOR SEMIVOLATILE ORGANICS - ACID
EXTRACTABLES 109
7-10 RANGE OF DETECTION LIMITS FOR SEMIVOLATILE ORGANICS
- BASE/NEUTRAL EXTRACTABLES 110
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Acknow led gemen ts
This document was prepared under the direction and coordination of Laurel J. Staley, EPA
SITE Technical Project Manager at the Risk Reduction Engineering Laboratory, Cincinnati, Ohio.
Mr. Thomas Raptis was Project Manager for the PRC SITE Project Team. Contributors and
reviewers of this report included Thomas Holcombe and Theodore Trowbridge of Dehydro-Tech
Corporation.
This report was prepared for EPA's SITE Program by 0. Karl Scheible, Gary Grey, and
Ashok Gupta of HydroQual, Inc. (HQI), and Thomas Raptis and Ken Partymiller of PRC
Environmental Management, Inc. (PRC). Robert Laufenberg and David Sexton of HQI, with Mr.
Grey and Mr. Gupta, performed all process sampling and monitoring and conducted all on-site
laboratory analyses. General Testing Corporation provided all off-site analytical support.
The authors would also like to acknowledge the cooperation of EPA Region 2 in providing
facilities for the demonstration and Foster Wheeler for providing support services. The cooperation
and support provided by Dehydro-Tech in planning and preparing the demonstration and in
conducting the demonstration itself are also greatly appreciated.
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LIST OF ACRONYMS AND ABBREVIATIONS
Acid Ext.
Acid extractable
ASTM
American Society for Testing and Materials
ATM
Atmospheres
b/n
Base/neutral extractable
BOD
Biochemical oxygen demand
BOD,
Five-day biochemical oxygen demand
C-G Process
Carver-Greenfield Process
CERCLA
Comprehensive Environmental Response, Compensation and Liability Act of
1980
CFR
Code of Federal Regulations
COD
Chemical oxygen demand
°C
Degrees Centigrade
DTC
Dehydro-Tech Corporation
EPA
U.S. Environmental Protection Agency
Ext.
Extraction
°F
Degrees Fahrenheit
GAC
Granular activated carbon
GC
Gas chromatography
GC/MS
Gas chromatograph/mass spectrophotometer
GTC
General Testing Corporation
g/kg
Grams per kilogram
g/g
Grams per gram
gpm
Gallons per minute
Hazardous I.D.
Hazardous identification
Hg
Mercury
HPLC
High pressure liquid chromatography
HQI
HydroQual, Inc.
HSL
Hazardous Substance List
L
Liters
lbs.
Pounds
lbs/min
Pounds per minute
LCSs
Laboratory control samples
MCAWW
Methods for the Chemical Analysis of Water and Wastes
MDLs
Method detection limits
mg/kg
Milligrams per kilogram
mg/L
Milligrams per liter
xii
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LIST OF ACRONYMS AND ABBREVIATIONS (CONTINUED)
mL Milliliters
mL/min Milliliters per minute
MS Matrix spike
MS/MSD Matrix spike/matrix spike duplicate
M/V Mass and volume
Hg/g Micrograms per gram
tig/kg Micrograms per kilogram
^g/1 Micrograms per liter
Microliter
n No
NA Not analyzed
ND Not detected
NHj-N Ammonia-nitrogen
NPL National Priority List
OCPSF Organic Chemicals, Plastics and Synthetic Fibers
ORD Office of Research and Development
oz. Ounce
PAB Oil PAB Oil and Chemical Services
PAHs Polyaromatic hydrocarbons
POTW Publicly owned treatment works
PRC PRC Environmental Management, Inc.
psi Pounds per square inch
psig Pounds per square inch gage
PQLs Practical quantitation limits
QA Quality assurance
QAPjP Quality Assurance Project Plan
QA/QC Quality assurance and quality control
QC Quality control
RCRA Resource Conservation and Recovery Act
RREL Risk Reduction Engineering Laboratory
SARA Superfund Amendments and Reauthorization Act of 1986
SITE Superfund Innovative Technology Evaluation
SMEWW Standard Methods for Examining Water and Wastewater
S04 Sulfate
SOW Solids/oil/water
S/SD Sample/sample duplicate
SSM Standard soils mixture
SSR Standard Soil Reference
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LIST OF ACRONYMS AND ABBREVIATIONS (CONTINUED)
svoc
Semivolatile organic compound
SW-846
Test Methods for Evaluating Solid Waste, U.S. EPA, 1986
TCLP
Toxicity Characteristic Leaching Procedure
TC Rule
Toxicity Characteristic Rule
TKN
Total Kjeldahl nitrogen
Total P
Total phosphorus
TPHs
Total petroleum hydrocarbons
TSS
Total suspended solids
VOC
Volatile organic compound
wt.
Weight
y Yes
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1.0 EXECUTIVE SUMMARY
In response to the Superfund Amendments and Reauthorization Act of 1986 (SARA), the U.S.
Environmental Protection Agency (EPA) established the Superfund Innovative Technology Evaluation
(SITE) Program to accelerate the development, demonstration and use of new or innovative
technologies that offer permanent, long-term cleanup solutions at Superfund sites. The SITE Program
is administered by the EPA Office of Research and Development (ORD) and has four primary goals:
• Identify and remove obstacles to the development and commercial use of
alternate technologies
• Structure a development program that nurtures emerging technologies
• Demonstrate promising innovative technologies to establish reliable
performance and cost information for site characterization and cleanup
decision-making
• 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
As a part of the SITE Program, EPA solicits proposals from innovative waste treatment
technology developers who have expressed an interest in participating in the SITE Program. Based
on these proposals, EPA selects technologies for inclusion in the demonstration portion of the SITE
Program. One of the selected technologies is the Dehydro-Tech Corporation (DTC) Carver-
Greenfield (C-G) Process.*
The demonstration of the DTC C-G Process occurred at EPA's Edison, New Jersey facility,
using waste oilfield drilling muds from the PAB Oil and Chemical Services, Inc. (PAB Oil),
Superfund site in Vermilion Parish, Louisiana. The technology is designed to separate a solids, oil,
and water mixture to its constituent fractions by evaporation and solvent extraction.
The primary objectives of the C-G Process SITE demonstration were as follows:
• Assess the ability of the process to effectively separate petroleum-based
hydrocarbon contaminated soils into their constituent solids, oil, and water
fractions
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W.lSlii I 1 I l.lllljlllll)
AZfths-. b ^O^CT
Solvent
4
i «.i «i
Bymrtna
Make-Up
S< ilvt.'iil
i I 11 i
Iih.IihIihI ill
Demonstration
I limit/alum ®
lank
Oil/Watei
Separator
isr—*
Sloan i
(kHhitiiibot
MecovHfiHj
I 1.1 si I
Distillation
Solvent
Recovery
(ii ntiau»
I Itiavy (Jib ^ 1 1 lyht Oilt,
i !K
ro ochj
InilMjotioutj Oil
t )lt Sit'.1 Disposal
Treatment
Condensed Water
. Discharge to POTW
or On Site Treatment
Sltiiiy Centntuyation
Cake Solventi/atton
J irut Prodnt t
Hetnm to Silt:
Excavation
* Waste was screened at the PAB Oil site
I lyun? I I I >i«it)i.iiit ol Situ Hi'modioli! >u I>y the
Ciirvur (irocnlield Process as Tested id tlic OcinonslMlion
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1.3
ANALYTICAL RESULTS
The primary objective of the C-G Process demonstration was to evaluate the ability of the
process to separate petroleum based hydrocarbon contaminated soil into its constituent solids,
indigenous oil, and water fractions. Important analyses included solids/oil/water (SOW) content,
TPH, and solvent concentration. The solvent used for the demonstration was Isopar-L, a food grade
iso-paraffin Cn oil. Results of these analyses were interpreted to characterize the efficiency of the
process in meeting this objective.
In Test Run'l-, the feedstock consisted of 52.35 percent solids, 17.48 percent indigenous oil,
and 21.75 percent water. The indigenous TPH for the feedstock was 14.68 percent. Test Run 2
feedstock consisted of 52.44 percent solids, 7.24 percent indigenous oil, and 34.77 percent water,
with an indigenous TPH content of 8.94 percent.
In both runs, effectively all the water was removed in the first evaporationyextraction pass, as
expected. Only trace amounts of water were observed after the subsequent two extraction passes. A
major fraction of the indigenous oil was also removed (to the solvent phase) in the first extraction
pass, with 78.1 and 65.9 percent removals observed in Test Runs 1 and 2, respectively. Further
indigenous oil removal was accomplished with each subsequent extraction.
r
The measured indigenous oil consists of TPHs and other material detected as oil by the special
SOW fractionation procedure used for this study. These other materials may be polar organics or
surfactants which are soluble in toluene (SOW procedure) but are retained on silica gel (TPH
procedure). Since TPH is the more commonly regulated parameter with regard to oil contamination,
oil removals were developed both in terms of oil determined by the SOW procedure and "indigenous"
TPH. Indigenous TPH removal is a calculated value (feed TPH minus final product TPH minus final
product Isopar-L), which represents the estimated quantity of TPH that originates in the waste feed
and remains on the final product. The calculation must be made because Isopar-L is detected in the
TPH procedure.
Indigenous oil removals (as measured by the SOW analysis) were 91.8 and 88.3 percent for
Test Runs 1 and 2, respectively. The measured TPH removals were 94.6 and 92.6 percent for Test
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Runs 1 and 2, respectively. By calculation, indigenous TPH removal was over 99.9 percent for both
test runs.
The C-G Process separates VOCs and SVOCs in the feed, depending on their boiling points.
Compounds with boiling points higher than the solvent are retained in the indigenous oil. Those with
boiling points lower than the solvent are collected in the process condensates or are adsorbed onto
activated carbon in the vent vapor treatment process. Compounds with boiling points near that of the
solvent may be retained in the solvent and actually reduce solvent make-up requirements. During
analysis, the presence of indigenous oil and Isopar-L in the samples (even at residual levels) interfered
with the detection of VOCs and SVOCs, requiring sample dilution and a consequent increase in
detection limits. This precluded any quantitative tracking of specific organics through the process.
The C-G Process is not represented to have any metals fixation capacity. Metals could either
be retained on the solids or dissolve into the aqueous and/or the solvent/oil phases in the slurry.
Several metals were detected in the feedstock, the most significant of which were aluminum, barium,
calcium, iron, magnesium, sodium, potassium, and zinc (all greater than 500 /xg/g wet weight).
Very few metals were detected in the centrate and condensed oil. Those detected were found
at relatively low levels in comparison to the feedstock. Metals in the water condensate were also
found at low levels. The final solids product results indicate that most metals contained in the
feedstock were retained in the final solids product. The process, in removing water and oil,
concentrated the solids by volume reduction, thereby concentrating the metals which preferentially
partitioned to the solids. This resulted in a proportional increase in the metals concentration of the
TCLP extract.
TCLP tests were performed on the final solids product from both test runs. TCLP results
indicate that the final solids product in Test Runs 1 and 2 were not a Resource Conservation and
Recovery Act (RCRA) characteristic waste. The dry solids product did not leach metals, VOCs, or
SVOCs above the RCRA regulatory limits.
When solids fractions increase from 50 percent in the feedstock to 98 percent in the final
product, at least a proportional increase in metals in the final solids should be expected due to volume
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reduction, presuming the metals stay bound to the solids. This may result in a proportional increase
in the metals concentration of the TCLP extract. An increase in TCLP extract metals concentration
was observed in both test runs. This concentration effect could be a consideration in selecting the C-
G Process. Although not observed in this demonstration, the process could produce a hazardous
material, with respect to TCLP metal levels, from a nonhazardous raw waste with significant metals
content. However, in all cases, the C-G process will produce a final solids product that is
significantly smaller in volume than the original waste feed.
Overall, the residuals generated from the C-G Process comprise the final dry solids product,
the separated water and indigenous oil phases, the vapor phase, and spent solvent. The final solids
product was a dry powder similar to bentonite in appearance. Values for all organics (VOCs and
SVOCs) and metals were below the RCRA TC limits for characteristic hazardous wastes. Residual
TPH levels in the final solids product were also at trace levels, indicating that the solids product
would be suitable for land disposal.
The water product produced in Test Runs 1 and 2 was a clear liquid with a strong odor, with
low suspended solids and biochemical oxygen demand (BOD), but high chemical oxygen demand
(COD) levels. TPH results compared well with the COD results in both test runs, indicating that
most of the COD was related to the presence of Isopar-L and lighter organics in the water product.
Acetone and 2-butanone were detected at trace levels. Other than these, no other volatile or
semivolatile organic was detected. Metals analyses also showed trace levels. The waters were also
found to comply with the OCPSF industrial categorical discharge limits with respect to metals and
organics concentrations.
The condensed solvent product was a clear liquid in both the test runs. Metal analyses found
most metals at trace or below detection limits. The condensed solvent was mostly Isopar-L and hence
could be recycled as solvent in the C-G Process. Although most of the vapors produced in the
evaporation step were condensed, some did escape to the vent. These vapors were passed through a
canister filled with activated carbon. Solvent analysis of the activated carbon showed the presence of
approximately 5 to 10 percent Isopar-L on carbon.
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Centrate produced in both test runs was a dark liquid with strong odor. The analyses of the
centrates produced in both runs showed higher indigenous oil and TPH levels in the first extraction
centrate, decreasing sharply in the subsequent extractions. Solvent analysis indicated approximately
87 to 89 percent Isopar-L in the first extraction centrate. The second and third extraction centrates
had Isopar-L levels above 98 percent. Due to lack of time and other problems, the final distillation
step demonstrating the separation of solvent from the indigenous oil was cancelled. As such, the
characteristics of the final indigenous oil product and solvent produced after distillation were not
demonstrated. However, that the centrate should be easily separated by fractional distillation to its
constituent heavy indigenous oil and solvent (Isopar-L) components.
1.4 QUALITY ASSURANCE PROCEDURES
The primary quality assurance (QA) objective of all SITE demonstrations is to produce
well-documented sampling and analytical data of known quality. To accomplish this goal, a detailed
and comprehensive Quality Assurance Project Plan (QAPjP) was developed before the demonstration.
The QAPjP contained specific QA targets for precision, accuracy, representativeness, completeness,
and comparability. It also specified (1) the analytical methods to be used; (2) data for holding times;
(3) number and types of blanks; (4) matrix spikes and matrix spike duplicates; (5) laboratory
duplicates; (6) reference standards; and (7) detection limits.
Two of the principal analyses used to evaluate the C-G Process were the SOW procedure and
a gas chromotography (GC) technique for analyzing solvent. The SOW technique is based on an
American Society for Testing and Materials (ASTM) Dean-Stark distillation procedure, modified by
DTC. The GC solvent procedure is based on a method developed by DTC. Both procedures were
further developed for the demonstration, including evaluation for different sample matrices and
development of quality assurance and quality control (QA/QC) information, which were used to set
QA/QC requirements.
VOC and SVOC organic analyses were included to track the fate of any detected compounds
through the process. Sample matrix interferences were encountered due to the presence of the Isopar-
L. Several sample locations for organics were dropped because of this interference, and samples that
were analyzed had high detection limits due to the necessary sample dilutions. VOC and SVOC mass
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balances were not attempted; rather a qualitative assessment of the fate of these compounds was made
on the basis of limited sample analyses.
During a laboratory QA audit, a concern was raised about the applicability of the metals
digestion method for organometallics. A separate investigation indicated that organometallic standards
were recovered within the required QA/QC limits for the demonstration, demonstrating the suitability
of the digestion procedure.
1.5 CONCLUSIONS
(1) The C-G Process separated a petroleum oil-contaminated waste drilling mud
into its solids, oil, and water phases. The C-G Process removed about 90
percent of the indigenous oil (as measured by the SOW procedure). No
detectable levels of indigenous TPHs were found on the final solids product
from either test run.
(2) The final solids product was a dry powder similar in character to dry
bentonite. Isopar-L solvent, a food grade oil, comprises the bulk of the
residual oil content on the final solids product.
(3) Values for all metals and organics'were well below the"RCRA TCLP limits'
for characteristic hazardous wastes. Additionally, the indigenous TPH
concentrations were reduced to trace levels on the final solids product.
Residues from the C-G Process may still require disposal as hazardous
materials, due to the regulatory constraints governing the disposal of
Superfund wastes.
(4) The C-G Process, as demonstrated on the PAB Oil site wastes, does not
remove metals bound to the solids phase. The process may increase the
apparent metals concentration in the solids fraction by volume reduction.
(5) The resulting water product requires further treatment due to the presence of
light organics and solvent. In some cases, the wastewater may be disposed of
at a local publicly owned treatment works (POTW).
(6) A full-scale C-G Process system can process drilling mud waste from the PAB
Oil site at an estimated cost of $523 per wet ton of feed. Of this total, $221
is C-G Process technology-specific and $302 is site-specific. Of the $302 per
ton site-specific cost, about $240 is for the incineration of indigenous oil
separated from the feed. Treatment costs are highly site-specific, and accurate
cost estimation requires data from a site remedial investigation or waste
profile, as well as specific treatment goals. Variability in the waste
characteristics or pretreatment requirements could significantly affect treatment
costs.
9
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1.6 COMMENTS
Several comments are necessary to put the demonstration results in perspective with respect to
the needs of a full-scale site remediation. Several fundamental differences exist between the batch
operated process used in the demonstration and an actual full-scale process that would be used in a
site remediation.
Bench-scale and possibly pilot-scale treatability studies should be performed with the actual
waste material to aid in solvent selection and to identify operating parameters and extraction
sequence. These studies should simulate continuous or semi-continuous operations. Add-back of an
inert material or start-up with surfactant may be needed; however, the studies should be sufficiently
long to minimize any influence that this material may have on the final products. Ideally, add-back
should be generated from the waste rather than introducing a virgin inert material as was done in the
demonstration.
The efficiency of two critical unit operations was compromised due to the age and condition
of the equipment. The centrifuge used in the demonstration was old and not as efficient as those
currently available. This resulted in a need to double centrifuge the slurry after the last extraction.
The desolventizer malfunctioned prior to the blank run. Although operable during the demonstration,
the operating temperature was lower than projected for the runs. This may have resulted in higher
solvent levels than projected on the final product.
10
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2.0 INTRODUCTION
The purpose of this Technology Evaluation Report (TER) is to provide a comprehensive
description of the C-G Process demonstration and its results. It is intended for engineers and others
evaluating the technology for a specific site and waste. This report can be used to understand the
performance of the technology during the demonstration and the advantages, risks, and costs of the
technology for a specific application. This information can be used to produce conceptual designs in
sufficient detail to make preliminary cost estimates for the demonstrated technology. For a discussion
of advantages, disadvantages, and limitations of the technology, refer to the Applications Analysis
Report (AAR) for the G-G Process (EPA, 1992).
2.1 TECHNOLOGY EVALUATION REPORT ORGANIZATION
This report is organized into eight sections. Section 1.0 is an executive summary. Section
2.0 presents introductory and background information on the SITE Program in general, and
specifically of the C-G Process demonstration. Section 3.0 describes the site from which the wastes
were obtained and the EPA-Edison facility where the SITE demonstration was conducted. Section 4.0
provides a detailed description of the C-G Process. Section 5.0 describes the demonstration
operations, including demonstration test and site preparations and the sampling program, and
summarizes the demonstration runs. Section 6.0 discusses the analytical results and performance data
in relation to the demonstration objectives. Section 7.0 presents the demonstration QA/QC objectives
and results, and Section 8.0 presents the EPA and developer costs for the demonstration. A list of
references is provided at the end of this report.
Five appendices are included. Appendix A summarizes monitoring data from the
demonstration. A compilation of laboratory data is provided in Appendix B, including TCLP results
and TC Rule limits. Appendix C contains a summary of the SOW and solvent analytical procedures
used for the demonstration. Appendix D presents the laboratory QC data, and Appendix E compiles
calibration documentation from the study.
11
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2.2 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 handle emergencies at uncontrolled hazardous waste sites and to clean up the sites; this
fund has become known as Superfund. EPA has investigated hazardous waste sites and established
national priorities for site cleanups. The ultimate objective of these investigations is to develop plans
for permanent site cleanups, although EPA does initiate short-term removal actions when necessary.
The National Priorities List (NPL) is EPA's list of the nation's top-priority hazardous waste sites that
are eligible to receive federal cleanup assistance under the Superfund Program.
Congress recently expressed concern over the use of land-based disposal and containment
technologies to address problems caused by releases of hazardous substances at hazardous waste sites.
Because of this concern, the 1986 reauthorization of CERCLA mandates that EPA select, to the
maximum extent practicable, remedial actions at Superfund sites that create permanent solutions to the
sites' effects on human health or the environment. In doing so, EPA is directed to consider use of
alternative or resource recovery technologies.
2.2.1 SITE Program
EPA 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
ORD.
Each year EPA solicits proposals to demonstrate innovative technologies. The most
promising technologies are chosen for participation in the SITE Demonstration Program. ORD and
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
daita on innovative alternative technologies so that potential users can judge the applicability of the
technology to a specific site and compare it to other available alternatives. The program also
12
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identifies the governmental policy and regulatory requirements applicable to the technology and the
hazardous substances treated or destroyed.
2.2.2 Demonstration Program Objectives
The SITE Program mandate is to seek cost-effective alternatives to land disposal and
containment for the remediation of hazardous waste sites. To address this mandate, the following
general objectives were developed for the SITE Demonstration Program:
• Assess the effectiveness of the process using analytical results
• Identify the potential need for pre- and posttreatment of raw and treated
materials
* • Identify the types of wastes and media to which the process can be applied
• Identify the hazardous substances treated or destroyed by the process
• Identify potential process problems and their possible resolutions
• ^Determine approximate capital, operating, and maintenance costs
• Determine projected long-term operating and maintenance costs
• Identify governmental policy and regulatory requirements applicable to the
process
2.2 J Technology Evaluation Criteria
A Demonstration Plan was prepared for the C-G Process demonstration (PRC, 1991). It
included a sampling and analysis plan that addressed the general demonstration program objectives.
The technical criteria used to evaluate the effectiveness of the C-G Process focused on its ability to
treat petroleum-based hydrocarbon laden soils (that also contain low levels of other "priority"
organics and metals) and to produce final streams (indigenous organics/oils, water, and solids) that
comply with regulatory requirements. The primary objectives of the C-G Process demonstration were
as follows:
13
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(1) Assess the ability of the process to effectively separate petroleum-based hydrocarbon
contaminated soils into their constituent solids, oil, and water fractions. Analysis of
raw wastes and process residues, and mass balances of the major fractions were used
to meet this objective.
(2) Evaluate the system's reliability in treating petroleum-based hydrocarbon contaminated
soils. The degrees of treatment achieved in separate test runs were compared to meet
this objective.
(3) Develop capital and operating costs for the C-G Process that can be readily used in
the Superfund decision-making process. Data collected during the demonstration as
well as the information supplied by the developer from case studies of full-scale
application of the technology were used to estimate these costs.
Secondary objectives of the C-G Process demonstration were also identified:
(1) Characterize the residuals (water, oil, vapor, and solids) relative to applicable
standards for final disposal or further treatment. Primary emphasis was placed on the
clean residual solids, relative to compliance with TPH and TC Rule limits for land
disposal.
(2) Document the important operating conditions of the C-G Process for application to
hazardous wastes sites. Operating data collected during the test runs were used to
assess operating conditions.
3) Assess the fate and movement of VOCs, SVOCs, and metals contained in the waste.
Mass balance evaluations of organic and metals data were used to make this
qualitative assessment.
2.2.4 Demonstration Preparation
The DTC mobile, trailer-mounted pilot plant was newly constructed and first used for the
demonstration at the EPA-Edison facility. The installation of the system and ancillary support
equipment (utilities, boiler, etc.) was completed in July 199 i; an on-site laboratory was also set up to
support the sampling and monitoring effort and some analytical needs. Shakedown of the pilot unit
occurred through July to identify and correct mechanical or other equipment related problems. This
was done by circulating a solvent and silt through each unit operation.
Pretest runs were then conducted in late July 1991 using a solvent and solids mixture with
water added. These runs identified specific problems relating to the free-water content of the mixture
and specific changes to how the feedstock would be fluidized in the solvent.
14
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^ The demonstration occurred from August 4 to 16, 1991, consisting of one blank run and two
test runs. (Originally, three test runs were planned, but Test Run 3 was cancelled due to scheduling
limitations imposed by EPA Region 2.) During the test runs, more than 640 pounds of waste drilling
muds were processed. Each test run consisted of processing the PAB Oil site samples, fluidized at a
solvent-to-solids ratio of 10:1, through three extractions. The first extraction evaporated and
separated the water phase. Final desolventization of the centrifuge cake was accomplished after the
third extraction. The blank run involved passing a clean solids/solventywater mixture through each
unit operation.
2.2.5 Project Organization and Responsibilities
For the demonstration, EPA, DTC, and the PRC SITE team (EPA's contractor) collected data
of known quality to evaluate the performance of the C-G Process. EPA had overall responsibility for
the project: overseeing, reviewing, auditing, and approving technical and QA aspects. DTC was
responsible for providing and operating all of the demonstration equipment. The PRC SITE team
prepared the Demonstration Plan and test site, performed the sampling and analysis, evaluated the
data, and prepared the AAR and this TER.
15
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3.0 SITE BACKGROUND
This section describes the PAB Oil and Chemical Services, Inc. (PAB Oil), site, which was
the source of the demonstration waste, and the EPA-Edison facility, where the demonstration was
performed.
3.1 PAB OIL SITE
3.1.1 Site History
PAB Oil began operations in 1979, disposing of drilling mud wastes and salt water resulting
from the drilling and production operations of oil and gas wells. PAB Oil sold to reclaimers waste oil
skimmed from the drilling mud separation and disposal pits. The site was used for agriculture prior
to the PAB Oil operation.
In 1979, no regulations existed covering the off-site disposal of drilling muds and salt water;
however, regulations became effective in July 1980 (Statewide Order 29-B). PAB Oil was
accordingly notified to obtain a permit from the Office of Environmental Affairs of the Louisiana
Department of Natural Resources (LDNR). EPA became aware of the site in 1980, after acting on a
citizen's complaint of discharge from the site into an off-site drainage ditch. Notices of Violation
(NOV) were issued to PAB Oil in December 1980 by LDNR; in June 1981 by the Department of
Environmental Quality; and in March 1982 by LDNR.
PAB Oil was owned by Alex Abshire until February 1982, when it was sold to a consortium
headed by William H. Lambert and Jack Clothier. PAB Oil reported that it stopped receiving oil
field waste in August 1982 because of its inability to meet the disposal requirements. In November
1982, LDNR revoked PAB Oil's interim authority to operate the disposal site and asked it to proceed
with a closure plan for the site. In January 1983, on-site storage tanks and the gates to the facility
were sealed by LDNR contractors; there was open leakage from the pits, and an unknown party had
placed petroleum waste in a tank at the site. All NOVs were referred to the State Attorney General's
office for prosecution in January 1983.
16
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In 1983, the company reported that it lacked funds for a proper closure and went out of
business. PAB Oil's lease was cancelled in November 1984, and the property was returned to the
landowner, Edmund Mouton.
3,1.2 Site Characteristics
The PAB Oil site is located in Vermilion Parish, a rural flat coastal plain area, approximately
20 miles north of the Gulf of Mexico. The site consists of 16.7 acres adjacent to Highway 167, about
3 miles north of Abbeville, Louisiana. A layout of the PAB Oil site is presented in Figure 3-1. Four
interconnected impoundments occupy approximately 70 percent of the site. The three drilling mud
separation and disposal pits at the site's east side have levees that extend approximately 6 feet above
grade. These pits are connected by a discharge pipe to the larger water impoundment, which is
surrounded by levees 2 to 4 feet high. Three oil reclamation tanks are located between the three
smaller pits and the large water impoundment. Photographs from the 1980 site inspection show that a
fourth tank was present in this area.
Wastes were transported to the disposal site in vacuum trucks and then transferred to the
separation and disposal pits. Drilling muds were pumped into the first disposal pit for gravity
separation of the solids, oil, and water phases. Waste oil floating on the surface of the pits was
skimmed and pumped to the on-site collection tanks until eventually sold to oil reclaimers. The three
interconnected disposal pits (exclusive of the water impoundment lagoon) cover an area of 350 by 300
feet and are approximately 10 feet in depth.
Vermilion Parish has the subtropical humid climate characteristic of areas near the Gulf of
Mexico. Rainfall averages 58 inches per year. Normal daily temperatures average approximately
54°F in January and 83#F in July. There are usually less than 10 days in a year when the temperature
falls below 32°F. The annual mean relative humidity is 75 percent.
17
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M* S
rum**** wo*o
I'll
pab OIL sm
Ol/tfcll n | Mud
Impour J rxntt
Soil *oIb Impoundment
H» I
rm cm.
SIC LA TOUT
PRC OMMNMkm MMIMMI, WC
Figure 3-1 Layout of PAB Oil and Chemical Company Site
-------
The site is located in a gently sloping area of the Gulf Coast. Elevation is approximately 17
feet above mean sea level. The area topsoils (0 to 2 feet) are largely silty loam formed from deposits
of the Quaternary Prairie Formation and are underlain by layers of clay and silty clay. Surface
drainage is mainly from the north to the south, through a system of natural pathways. Drainage from
the site is to the west and northwest to Coulee Kenny, which flows south and eventually joins the
Vermilion River approximately 1 mile south of Abbeville.
The largest topographic features in the immediate vicinity are the dikes and levees along an
abandoned irrigation canal and around the on-site impoundments. The site is situated on Quaternary
deposits consisting of undifferentiated Pleistocene and Recent age sediments, which form the Chicot
Aquifer, the principal source of fresh water in the area.
Recharge to the aquifer is mainly by rainfall in outcrop areas. Additional sources of recharge
include water moving through confining beds and the Vermilion and Atchafalaya Rivers, which incise
the aquifer. Prior to large-scale pumping in the area, the hydraulic gradient was southerly to
discharge areas near the Gulf of Mexico. However, ground-water usage has altered the gradient such
that it is now usually to the west and northwest of the site. The ground-water surface is
approximately 30 feet below ground level. Water from the Chicot Aquifer is generally hard and of
the calcium magnesium to calcium sodium type. Large-scale pumping has caused salt water intrusion
from lower portions of the aquifer in some areas.
Ground-water usage in the immediate vicinity is generally domestic or agricultural. The
Louisiana Department of Health and Human Resources reported that 568 homes with private wells are
located within a 3-mile radius of the site. Three of Abbeville's water supply wells are located
approximately 2.5 miles south of the site.
3.1.3 Site Contamination
Sampling was conducted in 1980 and 1985 by EPA contractors as part of a preliminary site
investigation. Analysis of samples from the separation and disposal pits indicated elevated levels of
barium, chromium, and lead. The soil and liquid samples also exhibited high levels of organics
19
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typical of hydrocarbons. Significant levels of acetone, total xylene, and bis(2-ethylhexyl)phthalate
were also noted in the on-site samples.
A pit sample was taken in May 1990 as part of the selection process for the SITE Program
and analyzed for VOCs, SVOCs, and metals. The solid (soils) content was approximately 27 percent
(by weight), and the sample had the consistency of machinery oil or grease. VOCs detected at
significant levels were toluene (4.47 mg/kg dry weight) and tetrachloroethene (0.94 mg/kg dry
weight). The detection limits for this sample were relatively high, ranging from approximately I to 4
mg/kg dry weight. Methylene chloride was also detected, although this was also found in the
laboratory blank.
Base/neutral and acid extractable SVOCs were not found above the detection limits for this
sample. The detection limits, again, were relatively high, ranging between 300 and 1,200 mg/kg dry
weight. Of the hazardous substance list (HSL) metals, the following were found in the sample:
Aluminum 148 mg/kg dry weight
Barium 349
Calcium 937
Copper 10
Iron 637
Selenium 3.7
Sodium 323
Vanadium 16.7
Zinc 32
Overall, the materials found at the PAB Oil site were petroleum-based, indicative of its use as
a waste drilling mud disposal facility. Other material may have been disposed of at the site, as
suggested by the presence of toluene and tetrachloroethene. These may have originated from cleaning
solvents.
3.2 DEMONSTRATION FACILITY
Originally, the demonstration was to take place at the PAB Oil site in Louisiana. However,
because of the construction delays in the pilot plant assembly at Edison, New Jersey, and severe
weather conditions in Louisiana, the demonstration was moved to New Jersey. The demonstration
/
20
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was conducted at EPA's research facility in Edison, New Jersey over a 2-week period. The trailer
mounted C-G Process pilot unit was located in Bay 2 of Building 245 at the EPA-Edison facility.
The building was equipped with necessary utilities and safety equipment. Safety signs and postings
describing emergency procedures were posted throughout the building.
21
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4.0 CARVER-GREENFIELD PROCESS DESCRIPTION
This section describes the basic unit operations of the C-G Process and the mobile pilot plant
used for the demonstration. The last part of this section discusses important differences between the
pilot scale system used for the demonstration and a commercial scale plant.
4.1 PROCESS DESCRIPTION
The primary purpose of the C-G Process is to separate multi-phase mixtures into their
respective solids, oils, and water fractions. The basis of the process is the suspension of solids,
containing water and oils, in a solvent. The solvent keeps the viscosity of the mixture low, permits
high heat transfer rates, and prevents scaling or fouling of the heat transfer surfaces as the water
content of the mixture is evaporated. The resultant solids are virtually water-free (<5 percent by
weight).
The C-G Process involves slurrying the feed material with a solvent, evaporating water from
the slurry in an evaporator, separating the feed solids from oil phases in a centrifuge, and evaporating
the solvent from the solids in a desolventizer. Multiple extractions may be carried out. The removed
oil phases are distilled to separate the indigenous organics and to recover reusable solvent. Residuals
(products) from the process include the following:
• a concentrated mixture of the extracted indigenous organics
• a water product substantially free of solids and oils
• a clean, dry solid
Several factors affect how effectively the C-G Process treats waste. Important among them
are solids size distribution, oil-soluble organics content, water content, nature of impurities and
solvent selection, and operating parameters:
Solids Size Distribution: Maximum size of the solids fed to the process is restricted to 1/4
inch. Large solids, such as stones and metals, must be excluded. If necessary, soils must be
screened and pretreated using a grinder to achieve a maximum particle size of less than 1/4 inch.
22
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Oil-Soluble Oreanics Content: The term "oil-soluble" refers to organics which are extracted
into and dissolved by a solvent. The C-G Process can treat soils, wastes, and sludges with oil-soluble
contents from parts per million (ppm) levels to levels of 75 percent and higher. Feeds having higher
oil-soluble content may require some pretreatment for efficient operation, such as simple gravity
separation of free oils.
Water Content: Waste streams having up to 99 percent water can be treated with the C-G
Process, although these could be pretreated with some dewatering device if desirable. Two full-scale
C-G Process facilities treating wastes containing 99 percent water were constructed in the early 1970s.
All other full-scale facilities are for treatment of wastes containing up to 98 percent water. Treating
wastes with high water contents will result in higher energy costs relative to feeds with lower water
levels.
Solvent Selection: The choice of solvent is generally governed by the impurities in the
waste. Extraction of indigenous oil/organic materials from solids can be enhanced by specific
solvents which have a high degree of solvency for target organic components, or by use of additives.
For example, an aromatic based oil could be used for extraction of aromatic materials such as
anthracene or naphthalene.
Operating Parameters: Certain operating parameters such as residence times, solvent
recycle ratio, temperature, and number of extractions required for a specific treatment goal will affect
performance of the C-G Process. Operating parameters may require some modifications depending
on the waste characteristics. These parameters are best determined from bench- and/or pilot-scale
treatability evaluations and can be optimized to meet the treatment goals most economically.
The following discussions briefly describe the major unit operations in the C-G Process.
4.1.1 Slurrying
The first step involves slurrying the feedstock with a solvent. The solvent used depends on the
specific application and the final disposal method for the extracted material. Generally, a hydrocarbon
based solvent having a narrow boiling point range around 400°F is used with petroleum oil laden
solids. Five to 10 pounds of solvent per pound of waste solids is typically needed for the slurrying.
23
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The solvent-to-sol ids ratio is generally based on the feed characteristics and the process objective.
Higher ratios promote fluidization for easy transfer of the slurry and increase efficiencies for
extraction of soluble organics into the solvent.
4.1.2 Evaporation
The solvent/feed slurry is circulated through an evaporator to remove the water. The solvent
is thoroughly mixed and agitated with the solids to encourage extraction of the soluble organic
compounds from the solids, including the petroleum based oils. Vaporization of the water, in certain
cases, can enhance extraction efficiency by breaking up emulsions holding the compounds in the
solids. In addition, VOCs in the feed are stripped during the evaporation step and are condensed with
the vaporized water and small quantities of solvent. Any pathogens or microorganisms in the feed are
also destroyed by the heating in the process, yielding a sterile final product.
In other cases, higher organic extraction efficiencies can be accomplished by modifying the
evaporator operations to perform several solvent extractions prior to removing the water. In this case,
the evaporator section heats the slurry, but at temperatures less than required for removal of the
water. The slurry is centrifuged to remove the solvent; the solids are then reslurried with the solvent
and returned to the evaporator section for an additional extraction. The final step is to dry the slurry
of residual water via the evaporation step described above; this means operating the evaporator
section at higher temperatures, under vacuum.
4.1 J Solids Separation
The slurry is sent to a solids separation device, often a centrifuge, to separate most of the oil
phase (mixture of solvent and indigenous oil) from the solids. The solids cake, after centrifuging,
typically contains 50 percent solvent (with extracted organics) and 50 percent solids. The centrifuge
centrate is essentially the mixture of solvent with dissolved indigenous organics and less than 1
percent solids (fines).
24
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4.1.4 Desolventization
After final centrifuging, residual solvent is removed from the solids by desolventization. This
process relies on evaporation and mild gas stripping to separate the solvent from the solids. The
heated stripping gas (such as steam or nitrogen) is scrubbed (of solvent) and recirculated to the
desolventizer. The final dry product typically contains less than 5 percent water. The residual
indigenous organics (petroleum hydrocarbons) levels on the solids generally depend on the extraction
efficiency, the number of extractions, and the initial levels in the feed. The desolventizer does not
evaporate the indigenous oils remaining in the centrifuge cake; these normally remain with the solids
fraction.
4.1.5 Distillation
Fractional distillation is used to separate extracted impurities from the solvent, producing a
recovered solvent substantially free from impurities and a concentrated stream of extracted "light" and
"heavy" organics (relative to the boiling point of the solvent). The recovered solvent can be reused in
the slurrying process. The concentrated stream of extracted "indigenous" organics can either be
incinerated or reclaimed.
4.1.6 Oil/Water Separator
The water removed from the slurry during the evaporation step is collected in a decanter after
condensation. Solvent condensed with the evaporated water is removed, leaving a relatively clean
water, virtually free of solids, with a low residual solvent content. The water product contains
water-soluble compounds extracted from the feed waste and can normally be treated with standard
wastewater treatment technologies, either on site or at an off-site treatment plant. Treatment options
vary depending on the characteristics of the raw material processed.
4.1.7 Vent Gases
All unit operations of the C-G Process are closed; vent gases are collected into a single
stream. The major source of vent gas is the evaporation section, but losses from this are small. The
vents are treated by passing the gas through granular activated carbon canisters.
25
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4.2 MOBILE PILOT PLAINT
A process schematic of the pilot plant is presented in Figure 4-1, This illustrates ail major
components of the pilot plant, which are also summaraized in Table 4-1, All process equipment was
installed on an open 8- by 48-foot trailer. To achieve the desired separations, the plant was operated
in two modes:
Solvent Extraction/Dehydration Mode: This mode included slurrying the waste with solvent,
and heating and centrifuging the slurry. This was done three times; the first time, the heating step
also evaporated the water.
Desolventization Mode: This mode included desolventizing the treated solids discharged from
the centrifuge.
The feedstock was separately screened at the PAB Oil site to remove debris greater than 1/4
inch in diameter and stored in 55-gaJlon drums. The feedstock was then mixed in a cement mixer (to
obtain homogeneous samples) and lifted to the loading point at the top of the fluidizing tank
(TK-102). The feed was manually charged to the fluidizing tank using a large portable funnel
equipped with a 1/4-inch screen.
4.2.1 Slurrying
Fresh solvent was pumped into the fluidizing tank (TK-102) from a 55-gallon drum elevated
with a fork lift. The quantity of solvent used met the prescribed ratio (about 10:1) of solvent to feed
solids. Isopar-L, a food grade oil manufactured by Exxon, was used as the solvent. Isopar-L is a
"pure-cut" hydrocarbon oil composed primarily of C,,-C,3 iso-paraffmic hydrocarbons. The tank was
equipped with an agitator to thoroughly mix the feed and solvent. While charging the feedstock, the
agitator (M-102) was kept on and solvent was recirculated through E-101, E-102, TK-101, and
TK-102.
26
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figure 4-i Process Flowsheet for the I'obile Pilot Plant
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TABLE 4-1
MOBILE PILOT PLANT EQUIPMENT LIST
Equipment Number
Evaporator Praheat Exchanger
E-101
Evaporator Falling Film Exchanger
E-102
Evaporator Condanaer
E-103
Vent Condanaer
E-107
Deaolventizer Circuit Superheater
E-111
Scrubber Cooler
E-112
Deaolventizer Circuit Preheater
E-113
Recovered Solvent Heater'*'
E-114
Recovered Solvent Cooler
E-115
Feed Grinder-
M-101
Fluidizing Tank Agitator (TK-1021
M-102
Product Slurry Tank Agitator (TK-103)
M-103
Centrate Tank Agitator (TK-105)
M-105
Centrifuge
M-106
Evaporator Vacuum Pump
M-107
Desolventizer
M-108
Vent Blower
M-110
Deaolventizer Blower
M-111
Steam Condensate Pot1"
M-11 2
Proceea Condeneete Pot
M-113
Vent Decanter
M-114
Sludge Feed Pump"'
P-101
Fluidizing Tank Pump
P-102
Eveporator Circulation Pump
P-103
Sludge Recirculation Pump"1
P-106
Centrate Pump
P-108
Solvent Pump
P-110
Scrubber Circulation Pump
P-111
Process Condensate Pump
P-112
Product Slurry Pump
P-118
Steam Condanaata Pump1"
P-117
Centrifuge Circulation Pump
P-118
Centrifuge Feed Pump
P-1 20
Vapor Chamber
T-101
Deeoiventizer Scrubber
T-106
Feed Hopper"
TK-101
Weigh Scalew
TK-101W
Fluidizing Tank
TK-102
Product Slurry Tank
TK-103
Centrate Tank
TK-10S
Solvent Holding Tank
TK-106
Proceea Condensate Decanter1"
TK-107
Air Compressor1*1
U-101
'•"These itema were not used for the SITE project.
28
-------
4.2 J2 Evaporation
The feedstock was loaded at room temperature. The heat exchangers were then activated to
bring the slurry temperature to the desired level. Although the evaporator vacuum pump (M-107) was
not in operation during the charging, the system was still under slight vacuum (1 inch water) from the
vent blower (M-110). Recirculation continued for approximately 1 hour. Heating was accomplished
with steam, and the steam condensate was sent to drain. The vapor phase (water and solvent) off the
vapor chamber (T-101) was condensed in E-103 under the desired vacuum by the evaporator vacuum
pump. Evaporation took place only in the first extraction pass. The process condensate was collected
in the process condensate pot (M-l 13). -
The slurry batch, properly fluidized, was continuously recirculated through the evaporation
section of the process by the fluidizing tank pump (P-102). The material was circulated through a
preheater (E-101) and a falling film evaporator (E-102) to a vapor chamber (T-101). The slurry was
then recirculated to the fluidizing tank via the evaporator circulation pump (P-103). The temperature
was raised to 260°F, with high vacuum during the first evaporation/extraction. Subsequent extractions
were run at near atmospheric pressure.
4.2 .3 Solids Separation
Once an extraction pass was completed (with or without drying), the slurry was transferred
(via P-116) to the product slurry tank (TK-103), which was kept mixed (M-103) with recirculation
(P-118). The slurry was fed to the centrifuge (M-106) by the centrifuge feed pump (P-120). The
solids were separated from the solvent/extracted organics phase in the centrifuge. The centrate was
discharged to the centrate tank (TK-105) and then transferred (via P-108) to the solvent collecting
drums (PD-4). The centrate from each extraction was collected separately.
The centrifuge solids were either fed to the desolventizer or returned for reslurrying and
additional extractions. A chute fitted to the desolventizer diverted centrifuge cake to either the
desolventizer, for desolventizing, or to drums for additional extractions. For subsequent extractions
the fluidizing tank was partially charged with fresh solvent. Centrifuged cake was then charged to the
fluidizing tank, the tank mixture was turned on, and additional fresh solvent was added to reconstitute
29
-------
the solids to the prescribed sol vent-to-sol ids ratio (10:1). The centrifuge cake from the third
extraction was recycled through the centrifuge to produce a cake suitable to be processed in the
desolventizer.
4.2.4 Desolventization
The recycled centrifuge sludge cake was transferred to the desolventizer by gravity through a
chute, continuously mixing the material as it was conveyed through the unit. The solvent was
evaporated and stripped using a hot stripping gas. The operating temperature in the desolventizer was
typically 225 to 300°F. The final solids product was drummed. The solvent laden stripping gas was
scrubbed at 200 to 250°F in the scrubbing column (T-106), with scrubber recirculation through pump
P-ill and cooler E-112; this was started with a fresh solvent heel. Nitrogen was used as the stripping
gas.
4.2.5 Distillation
Fractional distillation of the centrates and condensed oils was not demonstrated due to a
compressed demonstration schedule. Demonstration of distillation could not be done efficiently with
the pilot plant and was not considered a primary objective; as such, this element of the Demonstration
Plan was cancelled.
4.2.6 Oil/Water Separation
Separation of the process condensate to its oil and water phases was done manually, rather
than via the pilot plant decanter. Operating in a batch mode made manual separation a simple, more
time-efficient procedure.
4.2.7 Vent Gases
All process vent gases and vapors were first passed through a condenser and then through a
180- pound activated carbon canister. A new canister was used for the blank run and for each test
ran.
30
-------
4 J COMPARISON WITH COMMERCIAL SCALE SYSTEMS
A simplified general process schematic for commercial C-G Process systems is presented in
Figure 4-2. Commercial scale systems are normally operated on a continuous or semi-continuous
basis. The mobile pilot unit used during the demonstration differed in the following aspects from the
commercial system:
• Operations were on a batch basis
• Instead of multi-effect evaporator, a single-effect evaporator step was used for drying
• Preliminary handling equipment (feed hopper, sludge recirculation pump, weigh scale,
sludge feed pump and feed grinder) was not used
• The distillation step for separation and recovery of the solvent and indigenous oil was
not demonstrated
• Solvent was not recycled. Full recovery of the solvent by distillation would have
added significantly to operation requirements and the amount of time on site. Instead,
fresh solvent was used with each slurrying or reslurrying step.
31
-------
PW > PREPARATION MULTI-EFFECT EVAPORATION
SOLDS/OL SEPARATION
VACUUM
FUSQNS to.VENT VM»0« 4 ITZAM
cw
WET
FEED
REED
TAMC
QCSOL
IOW
RECOVERED SOIVEWT
C*.
OL
WATER
Q
wato-c*.-s
-------
5.0 DEMONSTRATION PROCEDURES
This section discusses the demonstration preparation, operations, and sampling program.
5.1 DEMONSTRATION PREPARATION
Prior to the demonstration, a Demonstration Plan for the C-G Process was prepared (PRC,
1991) and approved by EPA's Risk Reduction Engineering Laboratory (RREL). The plan consists of
four sections. The first section provides background information for the SITE Program and the C-G
Process. The second section contains the operating plan for the demonstration. The third section is a
QAPjP that presents testing and QA objectives, a detailed sampling and analysis plan and quality
control (QC) measures. The fourth section contains a Health and Safety Plan. Hie Demonstration
Plan was modified several times prior to the demonstration. These changes were conveyed to RREL
through memoranda and were approved by the RREL Project Manager before the demonstration
began.
5.2 DEMONSTRATION OPERATIONS
The mobile, trailer mounted pilot plant was newly constructed and first used for the
demonstration at the EPA-Edison facility. Figure 5-1 shows a plan view of the pilot plant and
support facilities. The installation of the system and ancillary support equipment (utilities, boiler,
etc.) was completed in July 1991. An on-site laboratory was also set up to support the sampling and
monitoring effort and some of the analytical needs. Shakedown of the pilot unit occurred through
July to identify and correct mechanical or other equipment related problems. This was done by
circulating a solvent and silt through each unit operation.
Pretest runs were then conducted in late July 1991 using a solvent and solids mixture with
water added. These runs identified specific problems relating to free water in the mixture and
specific changes to how the feedstock would be fluidized in the solvent.
33
-------
BAY #2
BAY #1
BUILDING 246
o o
o o
o o
o c
o o
o o
o o
o c
Bermed
Drum
Storage
Door Fan
L_
Ventilation
Hood
1
Waste
_ Mixer
Bermed (Bermed)
Waste
Storage
BAY #2
Bay
Door*
BUILDIN
HnUl
Exploslmeter
Decon'd Sampling
Equipment Storage
Sample Breakdown
Bench •
Sample Storage
Laboratory
Trailer
Boiler
b
Barm
Pilot
Plant
v
Floof Nn
Fane
Bermed Full I sop an—i
Temporary Storage1—1
Berimed Hazardous Waste BAw j.j
Satellite Storage A/«a BAY #1
Q 245
SSM Lab
Mechanical
• Shop
Area
Platform Scale
Bay Doors
00000000
00000000
Bermed 90 Day
Hazardous Waste Storage
n
Bay Doors
Rest Rooms
' Bemried Empty Isopar and Process
Product Temporary Storage
Bay Deer
OTC Trailer
Figure 5-1 Plot Plan of Carver - Greenfield SITE
Demonstration at Edison, New Jersey
34
-------
The demonstration occurred from August 4 to 16, 1991, consisting of one blank run and two
test runs. (Originally, three test runs were planned, but Test Run 3 was cancelled due to scheduling
limitations imposed by EPA Region 2.) During the test runs, more than 640 pounds of waste drilling
muds were processed. Each test run consisted of processing the PAB Oil waste, fluidized at a
solvent-to-solids ratio of 10:1, through three extractions. The first extraction evaporated and
separated the water phase. Final desolventization of the centrifuge cake was accomplished after the
third extraction. A blank run was performed before the test runs. This involved passing a clean
solids/solvent/water mixture through each unit operation.
5.2.1 Waste Handling
The petroleum contaminated wastes from the PAB Oil site were collected in four drums. The
waste was taken from the drilling mud waste pits at various locations with shovels and scoops. Each
55-gailon drum was filled to about 6 inches from the top. An attempt was made to collect the waste
soils with different solids, oil, and water ratios in different drums; this was done to construct a waste
feed with desired ratios of solids, oil, and water. The four drums were shipped to the EPA research
facility in Edison, New Jersey.
The drums were stored within a bermed storage area in Building 245, which was restricted to
authorized personnel. Before each test run, approximately 300 pounds of feedstock was shoveled into
a cement mixer, located in a separate spill containment area. The feedstock was mixed for
approximately 15 minutes to homogenize the waste feed. Homogenization was confirmed by replicate
analysis of the raw waste, using the SOW procedure. After mixing, the required samples were taken,
and the feedstock was discharged to 5-gallon buckets on a wooden skid. The skid and buckets were
then weighed to determine gross weight. A fork lift raised the skid up to the top of the fluidizing
tank where DTC personnel charged the waste feed to the tank. The empty buckets and skid were
then weighed to determine tare weight. The difference was the quantity of waste feed charged to the
process. Bentonite was handled in the same manner for the blank run.
All process residuals, including solids product, condensed oil and water, centrate, and
flushing oil, were drummed and retained in a bermed storage area until the demonstration was
35
-------
complete. After the derrionstration, all waste materials and excess feedstock were removed for off-
site disposal by the Edison facility's disposal contractor.
5.2.2 Operating Plan
The operating plan for the C-G Process demonstration is discussed in this section.
5.2.2.1 Demonstration Venue
The demonstration was conducted in Building 245 at the EPA-Edison facility. Building 245 is
equipped with all the necessary utilities such as electricity, water supply, sanitary facilities, internal
lighting, and telephones. The building has a separate storage area for chemicals and reagents. It also
has a satellite hazardous waste collection area. All hazardous waste generated in the building is
stored in this area for a maximum of 90 days before off-site disposal. Safety signs and postings
advising emergency procedures are posted inside and outside the building. Fire extinguishers are
located at various points inside the building. Safety glasses, hard hats and respirators were supplied
to the workers and visitors as a safety requirement. Normal operations required safety glasses, hard
hats, and safety shoes.
5.2.2.2 Pilot Plant Assembly
The mobile, trailer mounted pilot plant was newly constructed and first used for the
demonstration at the EPA-Edison facility. The pilot plant was located in Bay 2 of Building 245 at the
EPA-Edison facility. The pilot plant required on-site assembly of many unit operations. It was
assembled on a 8- by 48-foot trailer by DTC. During shakedown all unit operations and support
equipment were checked for leaks, and any required repairs or modifications were made. An oil-fired
boiler was installed near the pilot plant to supply steam to the process. The installation of the system
and ancillary support equipment (utilities, boiler, etc.) was completed in July 1991.
36
-------
5.2.2 J Office and Laboratory Trailer
An on-site office trailer was provided to DTC and was equipped with a telephone and other
necessary utilities. A 10- by 35-foot laboratory trailer was installed next to the pilot plant to provide
on-site analytical support, as needed for process control. Sufficient bench space was provided for
conducting all necessary on-site analyses. In addition to an existing ventilated hood, three additional
hoods were installed in the laboratory trailer and necessary modifications were made to the vent
system. Hoods were checked for air velocity and other required parameters by authorized personnel.
A schematic of the laboratory trailer is shown in Figure 5-2.
The laboratory trailer was equipped with necessary safety equipment such as fire
extinguishers, eye wash stations, safety shower, and first-aid kit. Chemicals were properly labeled,
and their material safety data sheets were enclosed in a file for reference. Safety signs and
emergency telephone numbers and instructions were posted inside the trailer. Six distillation
assemblies were installed in a hood for the SOW analysis. One Hewlett-Packard gas chromatograph
and integrator were set up inside the trailer to conduct solvent analysis. Two refrigerators were
located outside the trailer for storage. The on-site laboratory was completed in June 1991.
5.2.2.4 Pilot Plant Shakedown
The pilot plant went through a rigorous shakedown in late July. A slurry of clean silt and
Isopar-L was processed through each major unit operation. Details of various problems encountered
during the shakedown and subsequent modifications made to the procedures are described in Chapter
6 of this report.
5.2.2.5 Pilot Plant Cleaning
Before the blank and test runs, the pilot plant was cleaned by flushing a drum of Isopar-L
through the wet and dry sides of the process at room temperature. To avoid the formation of
"gummy" materials, water was not added during the cleaning procedure.
37
-------
GC hoi Solvent
Analysis
Open Bench Space
EPA/Foster Wheeler
Area
¦i
Cenlriluge and
Lab Waste Storage
(Hooded)
Walkway
s Six Place Distillation
Apparatus (Hooded)
1
( )'. H )! M
i I
Compressed Gas
Storage
Chemical
Storage
(Ventilated)
Vacuum f illralion
(Hooded)
Sink Waste
Collection
V
A
Sample
Refrigeration
I Sink
Vacuum
Oven
(Hooded)
Glove
Box
A
Dessicator
Balance
k
Figure 5-2 Laboratory Trailer Used for the Carver-Greenlield Demonstration
-------
5.2.2.6
Blank Run
One equipment blank run was performed before charging the system with raw waste. The
initial blank run resulted in modifications to the operating procedure. Bentonite was used as the solid
matrix for the blank run. The procedure and the changes made are described in Section 6 of this
report.
5.2.2.7 Test Runs
Two test runs using PAB Oil waste material were-performed during the demonstration.
Initially three test runs were planned; however, the third run was cancelled primarily due to
scheduling constraints. The two runs were identical except for the composition of the feedstock. The
details of the operation, including modifications made to the procedure, are given in Chapter 6 of this
report.
5.2.2.8 Collection of Wastes
Wastes generated during the demonstration included process residuals, laboratory wastes,
wastewaters, residual feedstocks, disposable supplies, and decontamination wastes. The larger
volumes of waste consisted of process residuals generated during the blank and test runs. These
included final solids product, water product, centrate, and other oil phases. Other large volumes of
the waste included laboratory wastes from the on-site laboratory analytical effort.
Laboratory and process wastes produced from the demonstration were drummed and properly
labeled. Active waste'droms were stored in the pilot plant and laboratory containment areas. The
final solids product and recovered water did not require special handling. Product water was
collected in 55-gallon drums. Extracted oils and spent solvent required special handling. These
residuals were collected in 55-gallon drums and were properly labeled as hazardous material. Full
drums were stored in the satellite hazardous waste collection area in Building 245 before disposal at a
RCRA hazardous waste facility.
39
-------
5.2.2.9 Pilot Plant Decontamination and Demobilization
After the second test ran, the pilot plant equipment was cleaned by DTC using water and
detergent, disassembled, and prepared for removal. All utilities were disconnected and the trailer was
hauled off site by DTC.
5.3 SAMPLING PROGRAM
The intent of the demonstration was to collect data that would demonstrate the ability of the
C-G Process to separate the PAB Oil site waste into its constituent solids, oil, and water components.
The following sections describe the specific sampling objectives and sampling point locations and
parameters.
5.3.1 Sampling Locations and Parameters
Sampling locations for solids, liquids, and gases are shown in Figure 5-3. Table 5-1 gives the
sampling and analysis schedule, including the blank run and test runs. These locations are
summarized as follows:
Predemonstration: Waste Pit Feedstocks. As described earlier, four 55-gallon drum
composites were developed from the waste pits. Each was sampled and analyzed for SOW content to
determine which drums would be used for the test run feedstocks. Screening analyses were also
conducted on these samples by DTC to assess suitability for the anticipated fluidization process. The
main purpose of these analyses was to assess the compatibility of the solvent and waste and to
determine if pretreatment was required. These consisted of simple "shake" tests contacting the wastes
with solvent.
Location 1: Feedstocks. This included the waste pit feedstocks as well as the inert solids
(benton.ite) used for the blank runs. The feedstocks were sampled from the mixer just prior to
transfer to the fluidizing tank, using a scoop spoon and stainless steel bucket. These samples were
analyzed for SOW, solvent (background), TPH, VOC, SVOC, metals, and ignitability (for hazardous
ID). The actual weight of the feedstock was measured directly using a calibrated platform scale.
40
-------
R»» Feed
HOI
L
\ ix-ioi / f"11
Of Out
IK-IOH Utlrt Scale
Stlteiil lukeup)
Rimnt
Siltiftl
Miilir^
Sal»mt htur* 01
Carbon
ClMSUf
tviporiiif Vacuua
insati
Rroceu
oodcaiiU
FVy t ITOtetS
'lK-|0?t nutf
FluldlilM lank
or
condensed
. .-Solvent
Jwv u*
Bee inter
Product
U1 Solvent J
Crindtf<£v£
PO-2 Uit
Lvapdfitv
frehfit
Uawqtt
It Of
Flit
bchiftgir
Solvent
*W
f¥«duc(
»iter„,
[Tub®
Solvent
Holding
link
afljtit-
Flumilno
lank
Desolventlier
Circuit
freftealer
F-SI3
Vapor
Oiiabcr
fiMwiaiu
Stew Condensate
Pu
UcUric
whrenlljer
III! 8jo«r
FluldifInf
link (Vap
solvent 1?
tfUO&er
Scrwbbtr — fa solvent 12er
Coolir k-in Circuit
JroAict Slirrf
link Agitator
Solvent Mirn
Steal or
a
Superheater
Centriluie
at ids
Collection
fruu
tiporatar
Circulation Puap
kfitflfyge
Circuit iwi
Product
Slurri
lank
Product Slirrj
Puap
>c rubber
Circulation
ftjap
, Crnirile
EH051 lank
Joitater
Centrifuge
H, minders
Feed hto
^4]N Stripping 6aj
Oesa rent
[Mpl apcllr
Central*
link
lie Lead
Seco*ered
olient Coo
Condensed
CeAiriti
hjaa
!T-Slif)
la
13)
Solvent vlll not be returned, Iresh solvent Nil) be used
Kith each eUracilon cycle.
Condensed vent solvent Mill be added to the centrate.
Process condensate and vapor condensate were eoablned for satpllng.
Solttnl
Figure 5-3 Flowsheet for the Mobile Pilot Plant Showing Sampling Locations
-------
TABLE 5 1. SUMMARY OF SAMPLE COLLECTION AND ANALYSIS
•t*.
¦'' tyfewm 9440$) 1;
W
0)
a)
w
(5)
- m
T, 1ft# >
% ^ jsssd;
f|,,H ¦¦
. ;¦ *iwww» ¦. ¦ ¦ ¦
¦a ?t. fv - 4:
CI
CI
Swi|lt4
s ¦
TMai
-
m 1? ^
LecutiM
M«Hk
R * t
* b C
riifiiw
» C
M$mo s/so x
Pre1*': Waste Pit
OS
4
sow
2
-
8
1. Feedstock (Raw
OS x
X
X
3
sow
2 6
i
16
Waste and Blank
(IB)
Solvent
2 6
-
16
Solids)""
(2 C)
TPH
2 6
2
18
-
voc
2 6
2
18
svoc
2 6
2
18
Melak
2 6
2
18
Ignitability
3
-
6
M/V/Q
1 1
-
-
1 a A.IJ Buck
s
1
sow
3
1
4
Solvent
3
1
4
TPH
3
2
S
voc
3
2
S
svoc
3
2
S
Metals
3
2
s
Igiutability
3
-
3
2 Solvent'" (Ficih)
0 x
1
Solvent
2
-
2
SVOC
2
-
2
Metals
2
-
2
3. Slurried Feedstock
OS
XXX
XXX
6
Solvent
3
•
18
SOW
3
-
IS
TPH
3
, -
It
M/V
'
-
-------
-------
TABLE S i.
SUMMARY OF SAMPLE COLLECTION AND ANALYSIS (CONTINUED)
.u
Ui
CfllUBB! (|A( BOtes)
U!
«)
yum
<»
" w /: i- i *f
CI
C1
Mafcte'*
« b e
i b c
Total
Cuintkw
PteWHtw
" ' !
B ^
:1 f;
w"> I *
fkf&ftfSD
illf
4. Ccnlrate
O x
XXX
XXX
7
(IB)
SOW
Solvent
TPH
M/V
Metals
2 J
2 3
2 3
1 1
1 J
I1*
2««
2»
22
22
26
12"
5. Ccniiifugc Cake
os
X X
X X
4
SOW
Solvent
3
3
1
14
14
6. Condensed W»kr
w *
X
X
3
(IB)
(2C)
Solve ni
TPH
V(JC
svoc
Mculs
Conventional
M/V
2 3
2 3
2 3
2 3
2 3
3
1 1
T"
T*
r«
2'"
2'"
10
12
12
12
12
10
7. Condensed Solvent
7a. Sciubber
O X
(> X
X
X
X
X
3
1
(IB)
(2C)
Solvent
TPH
Melala
M/V
SOW
2 3
2 3
2 3
1 1
2 3
I
2
2
10
12
12
a
8 Solid* PfiMlui-l
S *'•'
X
X
J
(IB)
SOW
Solvent
2 3
2 3
1
1
10
10
-------
TABLE 5-1. SUMMARY OK SAMPLE COLLECTION AND ANALYSIS (CONTINUED)
Cehinw (k« do«*)
(U
(J)
a>
M)
tt> P)
w
Run
#1
Cl
a
S—pio
<)A per Location
% *1$
v\
• ; -
Toui
UKibut
MMh
» b c
« k «
Sam pliant
ParmiMcn
B C
Mswsp stm
8 Solids Product
(2C)
TPH
2 3
2
12
VC K
2 3
2
II
SVOC
2 3
2
12
lynitalnlily
3
•
6
Metals
2 3
2
12
TCLP
3
|W
8
M/V
1 1
9 lll|> Bbllla"1
w
1
VI tc
1 1
-
3
It) f ield Uliinlb"
w
X
X
2
Sitl vc ill
¦
2
V(k:
1
-
2
SVOC
1
•
2
TPH
1
-
2
11 Equipment Blank*
w
X X
X
3
Salve nl
1 1
.
3
voc
1 1
-
3
SVOC
1 1
J
TPI1
1 1
-
3
12 Vent Gas (GAC)
S x
X
X
J
Solvent
1 2
¦
3
NOTKS
(1) S = Soil* (alter |m>c£«3ing)
OS = Oily (petroleum) and aulvcnl laden aoilt
O = Solvent and/or indigenous oil*
W = Ai|ueuus
GAC - Granular activated carbon
(2) Bl - Blank run
CI, CI a. I>, c <= E*lratiion/drjfiii|{ runs a, b and c for Teat Hum I and 2
-------
TABLE 5-1. SUMMARY OF SAMPLE COLLECTION AND ANALYSIS (CONTINUED)
(J)
(4)
Total sampling at this location The notations that occur below the total number arc the number associate J with the blank nin (B) and the teal runs (C).
Parameter Definitions
sow
-
Solids, oil, iihI water content by LXrau SliifL method (on-site)
Solvent
=
Carrier tolvciU by Carver-Greenfield Method (on site)
VOC
=
Volatile organica by Method 8240
SVOC
=
Semivolalilc acid and base neutral exiraciahlc organics by Metliod 8270
TPII
=
Total petroleum hydrocarbon by IK
McliiU
=
ICP scan for metals
Ignilahility
=
llaiardoui ID procedure
Tt'LF
=
Tonicity characteristic leaching proccdmc
Conventional
=
Conventional parameters: BOD, COD, TKN, Nil, N, SO,, TSS, |* 11. alldliiuly/uciJiiy. toial phosphorus
M/v/y
Mass, volume, and flow rate (if applicable) (on site)
(5)
(6)
(7)
(H)
(a)
(I.)
M
(J)
(O
(h)
(•)
Number of replicate samples taken in "sampling" (column 3). This total number is split (urtlioi to a blank ixiii (Bl) and test mn (CI, C2) As an example, three samples
were lakeen at Location I: one during the blank mn (Bl) and (wo during test mns (CI and C2).
One of the replicate samples during each C run was split three ways; two of the subsamples were spiked, the tiurd was analyzed as a replicate
One of the replicate samples duiing each C run was split two ways and analyzed in duplicate
Total number of analyses This is a siiiitmaiy of the sample analysis l« kj J ai each htcalion As an example. IcedMock VtK\ (IB x 2 reps) + (2C x 6 reps) * 2(MS/MSD * 2
mil*) — 18 analyses.
lour IceJsttick drums weie coiisIiik led be lore the demonstration. bach drum was analyzed in duplicate.
lieiilomle was uxd as the blank mn solids matrix.
Virgin solvent was analyzed in implicate
MS/MSI) and S/Sl) on sampling Irom Cla and C2u only
MS/MSD on samplings liom Cla only
Only the blank and first lest mn were analyzed for mclals.
Only one MS per lest run for bias collection
Tup blanks are shown for each mn, essentially equivalent lo one per sample shipment
One field blank for each blank and lest mn.
-------
Location 2: Solvent. The virgin solvent was sampled prior to the blank run, from a
randomly selected drum. This sample was analyzed for solvent (relative to standard), SVOC, and
metals to determine background levels of these compounds in the solvent. A dipper was used to
withdraw the sample from the drum.
Location 3: Slurried Feedstock. The fluidized feedstock/solvent mixture was sampled from
the fluidization tank recirculation pump discharge line. This was done after the "cold" slurry had
been recirculated for 10 to 15 minutes and before the mixture was heated. These samples were taken
for each extraction and analyzed for solvent, SOW, and TPH. The weight of solvent charged to the
system was measured.directly for each extraction.
Location 4: Centrate. The centrates from each extraction were sampled from the centrate
tank. This was done after the full batch had been centrifuged. The samples were drawn from a tap
downstream of the centrate pump (P-108, Figure 5-3), after which the tank contents were drained to
drums.
The centrate samples were analyzed for SOW content, solvent, and TPH to assess the
separation of oils from the solids, and the residual solids (fines) that were not recovered by the
centrifuge. Metals were also analyzed to assess their fate through the extraction process. The
centrate was discharged to tared 55-gallon drums, which were then weighed to determine the mass of
centrate removed.
Location 5: Centrifuge Cake. Centrifuge cake for the first and second extraction of each
test run was discharged through the deoiler chute and collected in a stainless steel 55-gallon drum.
The cake was actually a very thick slurry which was mixed with a stainless steel drum mixer. No
free liquids were visible in the centrifuge cake. Samples of the mixed cake were collected with a
dipper. During the third (final) extraction of each test run, the slurry was double centrifuged before
being sent to the deoiler. This procedure generated a true cake. A grab sample of the cake was
taken from the drum with a stainless steel spoon. The samples were analyzed for solvent and SOW
content; these data were used to determine the approximate solids separation efficiency of the
centrifuge.
46
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Location 6: Condensed Water. Condensates were collected at two points in the process,
the process condensate and the vapor condensate. During the first extraction step (and one
evaporation step in the blank run) all water was evaporated and condensed. Vapor losses at this point
were subsequently condensed (with other vents), as shown on Figure 5-3. The process condensate
(both aqueous and organic phases) was collected in the condensate holding tank throughout each test
run. The vapor condensate (both phases) was collected in a 30-gaJlon plastic container. The
condensates were manually split to aqueous and organic phases. Each phase was weighed, and like
phases of each condensate were composited to generate a total condensate sample for each phase.
The water condensate was then sampled via a dipper while the container contents were gently
stirred. The condensed water was analyzed for solvent and TPH to determine the loss of solvent and
indigenous petroleum hydrocarbons to the vapor phase. Similarly, VOC, SVOC, and metals analyses
were conducted. Conventional pollutants were also analyzed to determine subsequent treatment
requirements. These parameters include BOD, COD, total Kjeldahl nitrogen (TKN), ammonia
nitrogen (NH,-N), sulfate (S04), total suspended solids (TSS), pH, total phosphorus, alkalinity, and
acidity. The total condensed water weight was measured and recorded prior to sampling.
Location 7: Condensed Solvent. The condensed solvent, which was split from the total
system condensate, as described above, was sampled via a dipper while the drum contents were gently
stirred. The condensed solvent was analyzed for solvent, TPH, and metals. The total weight of the
condensed oil was measured and recorded prior to sampling.
Location 8: Solids Product. The final solids product from the desolventizer was collected
in a stainless steel drum under a nitrogen blanket. Once cooled, the drum contents were sampled
using a stainless steel spoon.
The final product was analyzed for SOW, solvent, and TPH to determine residual water,
solvent, and oil content. VOC and SVOC were measured to determine the extent to which indigenous
organics remained with the solids. The concentrations of metals were also determined. Ignitability
was measured to properly address hazardous identification requirements. Mass/volume and TCLP
measurements were also taken.
47
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Location 9; Trip Blanks. One trip blank per sample shipment was collected for VOCs. At
the laboratory, a sample bottle set was filled with organic-free (high pressure liquid chromatography
[HPLC]-grade) water and appropriate preservative for VOCs. This bottle was then shipped to the
field. The sampling crew shipped this bottle back to the laboratory unopened, along with the other
sample bottles from each run.
Location 10: Field Blanks. One field blank per run was collected for VOCs, SVOCs,
solvent, and TPH analyses to determine the extent of contamination from dust or other sources at the
Edison facility. A sample bottle was filled with HPLC-grade water and left open near the treatment
system during sample collection. At the end of sampling, this bottle was closed and added to the
sample inventory for shipment to the laboratory.
Location 11: Equipment Blanks. One equipment blank per blank run and test run was
collected for VOCs, SVOCs, solvent, and TPH analysis. At the laboratory, several 1-liter amber
glass bottles (identical to bottles for SVOC samples) were filled with HPLC-grade water and shipped
with the empty bottle set to the demonstration site. At the end of the blank run and test runs, the
HPLC-grade water was washed across decontaminated sampling equipment (stainless steel spoons,
spatulas, and dippers) into a stainless steel bucket. This water was then used to fill the equipment
blank bottle set. This procedure was used to identify the extent of any contamination attributable to
the sampling equipment as well as to atmospheric contamination.
Location 12: Vent Gas. All vent gases and vapors from the process were passed through a
granular activated carbon canister. At the end of a test run, the canister was removed and opened.
Sample thieves were used to extract core samples from the canister. These samples were analyzed for
solvent.
5.4 SAMPLE FREQUENCY DESIGN
Sampling frequency for demonstration plant studies must consider wastewater and process
stream variability. In a continuously operating process, a representative sample of all waste streams
can only be developed by collecting a continuous composite or a series of grab samples. In a batch
operating process, where wastewater and treatment products can be collected in their entirety, a single
48
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grab sample of a homogeneous mix of the materials can provide a proper characterization. The C-G
Process pilot plant was operated on a batch basis, minimizing the number of samples necessary to
characterize the waste streams and products. The scale of the pilot plant permitted manageable
quantities to be handled and mixed prior to sampling; therefore a single sample of the material was
sufficient for characterization.
Variability of sampling procedures and analytical techniques was considered by collecting
samples in triplicate from the total composite for the parameters to be measured at each sample
location. The exception to this was the raw feedstock, which was represented by six replicate
samples.
5.5 SAMPLING METHODS
The PRC SITE team collected samples at the eight locations in the C-G Process train.
Sampling methods conformed with SW-846 where applicable. Sampling methods and container
requirements are presented in Table 5-2. Section 5.3 discusses sampling procedures for each
location.
5.6 MONITORING POINTS AND OPERATING RANGES
This section discusses the process points which were monitored during the demonstration.
Monitoring points and measurements critical to the operation of the process were controlled during
process operation. Other monitoring points were for information and process analysis purposes only.
This discussion is limited to operational monitoring points used during the demonstration and which
are shown on Figure 5-* and Table 5-3.
Location A2 was the monitoring point for slurry flow from the fluidizing tank to the
evaporator preheat exchanger. Temperature and flow were monitored at this location. Steam
pressure was also monitored. Operating range for temperature is 130 to 250°F, depending on the
extraction phase. In the pilot unit, flow may range from 15 to 40 gallons per minute (gpm) and
steam supply may range from 0 to 50 pounds per square inch (psig). Temperature was not controlled
at this location.
49
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TABLE 5-2: SUMMARY OF SAMPLING METHODS AND CONTAINER REQUIREMENTS
(l) Feedstock Oily Solids Scoop (stainless steel) VOC Glass VOA Vial 2-4 or.
SVOC Glass Soils Jar 2-4 oz.
TPH Glass Soils Jar 1-4 oz.
Metals Glass Soils Jar 1-4 oz.
Solvent Glass Soils Jar 250 mL
SOW Glass Soils Jar 250 mL
(2) Solvent Oil Dipper (direct from SVOC Glass Jar 2-4 oz.
drums) Solvent Glass Jar 250 mL
Metals Glass Jar 1 L
(3) Slurried Oil/Solids Sample Tap off the Solvent Glass Soils Jar 250 mL
Feedstock Fluidization Pump SOW Glass Soils Jar 250 mL
TPH Glass Soils Jar 1-4 oz.
(4) Centrate Oil/Solids Sample Tap off the SOW Glass Soils Jar 250 mL
Centrate Pump Solvent Glass Soils Jar 250 mL
TPH Glass Soils Jar 1-4 oz.
Metals Glass Soils Jar 2-4 oz.
(5) Centrifuge Oil/Solids Scoop (from SOW Glass Soils Jar 250 mL
Cake centrifuge discharge) Solvent Glass Soils Jar 250 mL
(6) Condensed Aqueous Submerged Dipper VOC Glass VOA Vial 3-40 mL
Water (stirred drum) TPH Glass Jar 1 L
SVOC Glass Jar 2-1 L
Metals Glass Jar 1 L
Conventional Glass Jar 2-1 L
Solvent Glass Jar 250 mL
(7) Condensed Oil Submerged Dipper TPH Glass Jar 1 L
Solvent (stirred drum) Solvent Glass Jar 250 mL
Metals Glass Jar 1 L
(8) Solids Solids Scoop or Spoon SOW Glass Soils Jar 250 mL
Product Solvent Glass Soils Jar 250 mL
TPH Glass Soils Jar 1-4 oz.
VOC Glass VOA Vials 2-4 oz.
SVOC Glass Soils Jar 2-4 oz.
Igmtability Glass Soils Jar 1-4 oz.
Metals Glass Soils Jar 1-4 oz.
TCLP Glass Soils Jar 1-16 oz.
(12) Vent (GAC) Solids Thief Solvent Glass Soils Jar 250 mL
50
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te« Feed
a Out
\TX-IQI /
"1 MPS | Sludge Recirculation tap
Feed rapper
TK-I01H jlelQh Scilc
Solveot (Mkein)
urban
UftlSWr
ITQCCSS
Evaporator Vicuui
Condense
ft Qui
Solvent fetirfi HI
irotm
udensate
turn
Fluldlilnfl l«t
or
Condensed
Solvent
(rui
OtCtfltCT
Product
Solvent>
trlnder
Evaporator
fYefieat
Ei changer
Evmritor
failing nia
UchaMcr
__vni
Solvent
i>H0b| Holding
lank
Fluldltlng
lank
(tesoiventIter
Ci
ke
»(MI3
llcctrlc
Yipor
Oiaober
solvent tier
ill Blo«er
Fluldmng
lank Kiflp
Steaa Condensate
Solvent Retirn
^^53^ |
Centrlluge
Dtuas
>S0l*Cf>l | Iff
ruttrr
Server « .OrsolventUe
Caolrr UlllI Circuit
Superheater
Product Slirry
lank Agitator
•10
Situ or
vaporator
Circulation hip
Centrifuge
Circulation
Pvjao
&
¦TmisU
Product
Slxry
lank
Product Slirrj
Pom
Scrubber
Centrate
FTOSl lank
Agitator
Circulation
N) Cj linden
Centrifuge
Feed Ftao
I'-Suel
Healed SirIpplo u
Desolvent ler
Centrate
[Ml3
llecoveretf
Balvent Coole
MMoah
Product
Condensed
Solvent
Centrate
121
131
Solvent will not tie returned, fresh solvent *111 be used
Kith each extract ton cycle.
Condensed vent solvent will be added to the centrate.
Process condensate and vapor condensate Mere conblned lor saapllng.
Figure 5-4 Flowsheet for the Mobile Pilot Plant
Showing Monitoring locations
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TABLE 5-3. CARVER-GREENFIELD PROCESS MONITORING LOCATIONS
MwrnurcnuMt
DTC*
Notetfim
Operating ft«fe
Mt*tUorc4 During
E&rmnkm '
ABC
i: >SSii:: ; "i. W;
A2
Feed line slurry from Fluidiziog
Tank (TK-102) lo Evapora-
tor Preheat Exchanger (E-IOl)
Temperature
Prcbbure
How
Tl-I
PI 3
H 1
130 to iHffF (Extraction)
200 to 25(fF (Evaporation)
0 lo 50 pug
15 to 40 gpm
Y
N
N
Critical. Flow control neceaaarv
lo mainlaiii velocity in evaporator
A3
Steam PrcbMire Shell Side
Prchcater (E 101) and Evaporator
(E 102)
Picture
I'M
0 to 50 psig
Y
Y
Y
Control necea»ary to
miinuin temperature in
evaporator (E l 02)
AS
Slcain in Evaporator (E-102)
Temperature
Tl-J
250 u> 300'F
Y
N
N
Tl-3 monitor* condenaing ateam
temperature
A6
Process Vapor iri/from Vapor
Chamber (T-101)
Pressure
Temperature
PI 7
Tl 4
Aldkisjihciic lo lull vacuum
130 iu I80F (Exfraciion)
200 to 250*F (Evaporation)
Y
Y
Y
Critical. Temperature and
preaaure critical during
evaporation phase
A7
Process condensate between
ConJcnsci (E-103) and
Condensate Pol (M-l 13)
Temperature
Tl 5
< I30 F
Y
N
N
To ataure thai condeniinj it
occurring
AIO
Centrifuge feed between
circulation pump (P-118) and
feed pump (P-120)
Temperature
Tl 8
90 lo ISO'F (Extraction)
90 lo 250*F (Evaporation)
Y
Y
Y
Temperature Jrxjp between A2
and AIO ia due lo heat loaacs
through the proceaa
All
Between Cenirale Tank (TK-105)
and Cenirale Pump (P-108)
Temperature
Tl 9
90 lo I80*F (Extraction)
90 to 250*F (Evaporation)
Y
Y
Y
AI2
Vapor line from Dcaolveniizer
Superheater (E l II) to
Oe»o|venti/cr {M 108)
Temperature
TC 1
350 io 450'F
N
N
Y
Critical. Conlrai lit mm vimirr
alripping of reaidual oila
-------
TABLE 5 3. CARVER-GREENFIELD PROCESS MONITORING LOCATIONS (CONTINUED)
L«c4rtW"
IrffirttftcMtofi
Meamrcnuiit
- DTC** "
Operating Rwpi
Mnntorad During
CxtrattiMM r
w * ,
A 0
c
¦¦m :?.r
AI3
Off gas from Peaolvenlizer
(M 108)
Temperature
Ti 1
150 io 25(JPF
N N
Y
Critical (See Note lo A12)
AH
Oil gas from Dcxolvenli/cr
Scrubber (T-J06)
Temperature
Tl 12
(TC4)
200 to 275-F
N N
V
Critical Minimizes solvent losses
AI5
Gas between desolventi/er
jHuh^icr
200 t,. 275'F
N N
Y
AI6
Gas How fiom Desolvenlizcr Blower
(M HI)
Pressure
Flow
PI-15
FI-4
0 to 2 pvig
SO 1,. 200 >. fill
N N
Y
-
A17
Solids fmin Desolveutiicr
(M 1(18) to fioducl Drum
Temperature
Tl 14
150 in JSO'F
N N
Y
A1H
Circulating scrubber solvent
between pump (P- III) and
exchanger (t l 12)
Temperature
Tl 16
150 to 275"F
N N
Y
A19
Scrubber Solvent between
exchanger (E 112) and Desolventizcr
Scrubber (T-106)
Temperature
Tl 17
150 to 275"F
N N
Y
NOTKS:
(1)
(2)
(3)
Aa designated on Figure 5 4
DTC designation of monitoring point
Cntkal designation means control is important to piucesa.
-------
Location A3 was the monitoring point for steam pressure. This line supplied steam from the
boiler at the demonstration site. The operating range was set by the operating temperature of the
process and can range from 0 to 50 psig, depending on steam demand.
Location AS was located in the evaporator section. Temperature at this location was from
the shell, or steam side of the evaporator falling film heat exchanger. Temperature typically ranges
from 250 to 300°F. Pressure at this location was the shell side pressure and was similar to Location
A3.
Location A6 was the monitoring point for vapors generated in the evaporator. This
monitoring point was located on the line from the vapor chamber to the condensor. Temperature was
typically 200 to 26CPF and pressure 13 to 15 psig during the water extraction phase (hot extraction).
Temperature and pressure were not critical during cold extraction.
Location A7 was the monitoring point for the condensed vapors. The monitoring location
was on the line between the condensor and the condensate pot. The operating temperature was
< 130°F and was controlled by the flow and temperature of cooling water.
Location A10 is the monitoring point for slurry feed to the centrifuge. The monitoring point
was located on the line between the centrifuge circulation pump and the centrifuge feed pump. This
location was monitored for temperature only. Temperature at this stage of the process resulted from
the evaporator operating temperature and heat losses. The temperature'range during the first
extraction was 200 to 250°F. At this stage water was removed from the slurry. Temperature range
for the second and third extractions was approximately 130 to 180°F,
Location All was the monitoring point for centrate removed by the centrifuge. This location
was monitored for temperature only and was not controlled. The monitoring point was on the line
between the centrate tank and the centrate pump.
Location A12 was the monitoring point for the heated vapors and gases sweeping through the
desolventizer. The monitoring point was located on the line from the desolventizer superheater to the
desolventizer. Temperature was controlled to an operating range of 350 to 450°F by the electric
54
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preheaters. Temperature control at this point in the process-was critical to the removal of residual
levels of solvent from the centrifuge cake. The temperature range was determined based on
equipment shakedown operations.
Location A13 was the monitoring point for off-gases from the desolventizer on the line to the
desolventizer scrubber. Temperature was not controlled and was expected to be less than at Location
A12. The observed temperatures ranged from 150 to 250^. The temperature at this location
resulted from the heat loss through the deoiling process.
Location A14 was the monitoring point for off-gases from the desolventizer scrubber to the
circuit preheater. Temperature was expected to be slightly less than at Location A13. Temperature at
this stage of the process was critical in condensing solvent.
Location A15 was the monitoring point for vapors passing between the desolventizer circuit
preheater and the desolventizer blower.
Location A16 was the monitoring point for vapors passing between the discharge side of the
desolventizer blower and the superheater. Gas flow was measured at this point using a pitot tube and
pressure measurement.
Location A17 was the monitoring point for solids between the desolventizer and the product
solids drum. Heated gas was continually swept through the drum while product was generated.
Temperatures up to 300"F are typical at this location. This location was not critical to process
performance.
Locations A18 and A19 were the monitoring points for temperature on both sides of the
scrubber cooler. The cooler inlet was monitored at Location A18, and the outlet was monitored at
Location A19. Temperature range at both locations was expected to be 170 to 225°F.
55
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6.0 PERFORMANCE DATA AND EVALUATION
AnaJytical and performance data were gathered during the demonstration to serve as a basis
for evaluation of the process. These data were collected in conformance with the Demonstration Plan
and subsequent memoranda and evaluated with respect to the demonstration objectives stated in
Section 2.2.4. This section consists of the following subsections:
• Discussion of bench-scale treatability results which were referenced in the
Demonstration Plan as a basis for defining operating procedures
• Description of deviations made from the original Demonstration Plan
• Discussion of trial runs and consequent modifications to the operating procedures
• Description of operating conditions experienced during the demonstration
• Discussion of blank run results
• Characterization of feedstocks used for the test runs
• Discussion of analytical results with respect to demonstration objectives
• Presentation of material balances performed for the blank run and each test run
6.1 TREATABILITY TESTS
A sample of the pit waste from the PAB Oil site was sent to DTC for bench-scale treatability
analyses. DTC received the sample on July 23, 1990. The sample was somewhat "liquid" in that it
could be stirred, resuspending the solids. The breakdown of the sample was as follows:
Solids 29.5%
Water 29.1%
Oil 41.4%
An aliquot was centrifuged to determine if significant oil and solids/water separation could be
accomplished by centrifuging. This yielded the following results:
56
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Centrifuged Solids
(61 % of Total
Sample Volume)
Centrate Liquid
(39% of Total
Sample Volume)
Water
Solids
Oil
27.2
46.5
27.3
%
32.0 %
4.5 %
63.5 %
Because oil separation was not high, subsequent C-G Process treatment was done on the total feed,
three treatments were imposed:
(1) Sample was slurried in solvent and dried at the same time,
(2) Sample was extracted three times; the water was evaporated during the first
extraction.
(3) Sample was extracted three times; the water was evaporated during the third
extraction.
Five samples were submitted for VOC analysis (GC/MS Method 8240): the total raw sample,
the centrifuged solids, and the three treatment samples. The following compounds were detected:
Dry Final Product
Feed
Sample
Feed Sample
Centrifuge Solids
Treatment
1
Treatment
2
Treatment
3
Acetone (uglVLg)
3,200
ND
ND
ND
ND
Toluene (jig/Kg)
5,510
513
4.310
3,410
346
Ethylbcnzene (>g/Kg)
762
ND
ND
ND
ND
Total Xylene OigAcg)
3,040
ND
ND
ND
ND
ND = Not Detected
These results demonstrated that the third treatment was the most effective, possibly because
the adsorbed water in and on the solids minimized the adsorption of hydrocarbons by the solids. Pre-
drying the material apparently opens surfaces on the solids for adsorption of organics. Thus, the bulk
of the contaminants should be extracted before the solids are dried to increase the removal of the final
residual contaminants.
57
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Based on the treatability results, DTC planned for each test run to consist of three solvent
extractions, with drying during the last extraction. Additionally, the feedstock would be prepared to
have a solids content of approximately 50 percent, possibly within a range of 45 to 60 percent.
Pretreatment of wastes with higher "liquid" contents (by centrifugation, decanting, etc.) or by add-
back of dried solids during the fluidization step would yield this level. Pretreatment was not
demonstrated, since the purpose was to demonstrate the C-G Process itself.
6.2 DEVIATIONS FROM DEMONSTRATION PLAN
Several changes were made to the Demonstration Plan, due to logistical and scheduling
constraints and trial run results. A major deviation was to switch the demonstration from the PAB
Oil site to the EPA-Edison research facility. The third test run and the distillation step after each test
run were also eliminated due to scheduling constraints. In addition, several modifications were made
to the sampling and analysis plan and to the monitoring and operation protocols for the pilot plant.
6.2.1 Modifications to the Demonstration Plan Content
6.2.1.1 Change of Demonstration Site
The demonstration site was changed from the PAB Oil site to the EPA-Edison facility. This
was done mainly because delays, in construction of the pilot plant caused a potential conflict between
the site demonstration activities and EPA Region 6 remediation activities at the PAB Oil site. Severe
wet weather in Louisiana also contributed to the decision to transfer the demonstration to the EPA
facility in Edison, New Jersey.
6.2.1.2 Elimination of the Third Test Run
EPA eliminated the third test run due to scheduling constraints and lack of sufficient Isopar-L
supply. EPA Region 2 had requested that the demonstration be completed and the pilot plant shut
down by August 16. Sufficient quantities of Isopar-L would not have been available from the sole
source of the solvent, Exxon, for several weeks after the scheduled August 16 shutdown date. The
58
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second test run was completed on August 15, precluding a third test run, regardless of Isopar-L
supply considerations.
6.2.U Elimination of Distillation Step from Blank and Test Runs
The full-scale C-G Process incorporates a solvent distillation step to recover and recycle
carrier solvent and to concentrate the extracted indigenous oils for ultimate disposal. The pilot plant
was not equipped for, nor was there ever any intention of, demonstrating a complete separation of
indigenous oils from Isopar-L by multi-phase fractional distillation, as is typically used in full-scale
operations. Rather, the Demonstration Plan called for single-stage solvent distillation through the use
of the evaporator; the intent was to demonstrate, on a gross basis, that the Isopar-L could be
recovered for reuse. DTC maintains that distillation is a well developed technology and that
separation of the carrier solvent from indigenous oils is a routine application of the distillation
process. Due to the compressed schedule, the fact that the pilot plant distillation would not reflect a
full-scale operation, and that demonstration of distillation was not a primary objective, this element of
the Demonstration Plan was cancelled by mutual consent of the developer, PRC, and EPA.
6.2.2 Summary of Pilot Plant Shakedown and Trial Runs
Preliminary evaluations were conducted once the pilot plant was fully assembled, including
shakedown and pretest runs. A shakedown of all major unit operations was performed to check for
system leaks and proper operation of pumps and other equipment. Pretest runs were then conducted;
these identified specific problems relating to free water in the slurried mixture and specific changes to
how the feedstock would be fluidized in the solvent.
6.2.2.1 Pilot Plant System Shakedown
Pilot plant shakedown occurred during the latter part of July. Only Isopar-L and a clean
standard soils mixture (SSM) were added during shakedown. Each unit operation was tested for leaks
and the ability to process solids. The upper jacket of the desolventizer malfunctioned, discharging
heavy oil from the jacket to the solids in the unit. The whole system was cleaned and flushed with
Isopar-L to assure that all residues were out of the system.
59
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6.2.2.2
Trial Runs
A C-G Process system operated in a batch mode can be susceptible to process start-up
problems. These are often related to the free-water content of the waste material, the presence of
which frequently produces a gummy slurry when the feedstock is fluidized with the carrier solvent. If
carried into the process, this gummy material can cause clogging of pipes, pump failure, and system
shutdown.
In many commercial applications, recirculation of dried slurry to the fluidlzing tank absorbs
the free water and prevents the development of this gummy condition. If dried slurry is not available,
such as during start-up, a surfactant is added to stabilize the suspension in the slurry. The surfactant
is generally eliminated as dried slurry material is generated and becomes available as add-back.
At first, the unit was operated with a wetted SSM and solvent. The lines became plugged
with the gummy material described above. In the next series of tests, DTC used a surfactant with the
SSM to prevent the gummy condition during start-up. This produced a dry final product after
desolventization. A SOW analysis of the final product showed the presence of approximately 4
percent indigenous oil, an anomalous result. However, clean SSM, when analyzed by the SOW
procedure, was found to be oil-free. This led to the conclusion that the surfactant itself was being
detected as an oil. Based on this finding, surfactant was not used since it could compromise the test
run results.
A new run was then attempted (this had been planned as a blank run) on August 1, 1991.
Operational modifications were made, one of which was the use of bentonite as the solid matrix
instead of sand or silt, as planned and attempted with the earlier runs. Bentonite was chosen because
of its potentially higher water holding capacity. Additionally, since bentonite is a major component of
most drilling muds, it better simulated the PAB Oil waste solids. DTC did not use any surfactant
while charging the feed in the fluidizing tank. During processing, the line between the centrifuge
feed tanlr and the centrifuge became plugged with the gummy material. Despite repeated efforts to
clear the blockage, the gummy slurry could not be pumped to the centrifuge. The scrubber also
contained a blockage resulting from the slurry. Because of these problems, this run was terminated
and the system was flushed. It was determined that add-back would be needed to prevent the gummy
60
-------
condition. This and other changes made to the pilot plant operation plan are discussed in the next
section.
6.2.3 Changes Made to the Pilot Plant Operating and Monitoring Plan
6.2.3.1 Selection of the Evaporative Extraction Pass
DTC's bench-scale treatability studies indicated that most organics were removed when
evaporation occurred in the third extraction (Section 6.1). Therefore, the third extraction was
established as the evaporative phase.
During the pilot plant shakedown and initial attempts at the blank run, as discussed earlier, a
gummy substance formed when the waste was added to the solvent. DTC therefore switched the
evaporative extraction from the third pass to the first pass, removing the water immediately.
The evaporative drying pass for each run was also conducted under deep vacuum (22 inches
Hg) instead of slightly below (2 to 3 inches of water) atmospheric pressure, as originally planned.
The operating temperature was lowered to 210 to 220PF, accounting for a 40 to 50°F reduction in the
water boiling point due to deep vacuum. The intent was to promote more complete drying. This
change was made because the initial trial runs at low vacuum with a maximum temperature of 260°F
resulted in residual water (approximately 3 to 5 percent) in the solids. The second and third passes
were at lower temperatures and under slight vacuum, similar to those originally planned for the first
and second passes.
6.23.2 Operating Conditions of the Desolventizing Process
The desolventizing process strips residual solvent from the centrifuge cake, forming a dry,
solvent-free solids product. A stream of hot gas volatilizes and sweeps out the residual oils. This is
the last step in the C-G Process.
The initial temperature objectives stated in the Demonstration Plan were for inlet gases to be
275 to 350°F and outlet gases to be 225 to 350°F. A net temperature drop of 50°F was expected
61
-------
across the desolventizer. During a preliminary run, the upper heating jacket of the desolventizer
malfunctioned and had to be shut down for the remainder of the demonstration. This resulted in
higher heat losses than expected from the desolventizer. To maintain a high enough temperature in the
desolventizer to strip residual solvent, the desolventizer superheater had to be operated at a higher
temperature than originally specified in the Demonstration Plan.
6.2 J J Blank Run
Bentonite was used as the solid matrix for the blank run rather than sand, as originally
planned. This material better simulated the waste solids and had a higher holding capacity for water.
Distilled water was added to the bentonite to allow condensate to be generated in the process, thereby
"blanking" the system's condenser.
6.23.4 Water Heel
At startup of the first pass (evaporative pass) of each test run, a heel of 65 pounds of
deionized water was added to the condensate tank. This was necessary for accurate observation of the
sight glass level in the condensate tank during this pass. This initial volume of water was accounted
for in subsequent mass balance calculations.
6.2.3.5 Use of Add-Back Procedure
Add-back is a standard operating procedure in commercial systems. In many full scale C-G
Process units a surfactant is used in fluidization until sufficient dried (water removed) product is
produced to add back to the fluidization process. This dry add-back material absorbs free water from
the raw waste material, preventing the gummy condition described in Section 6.2.2.2. DTC
investigated and found a suitable surfactant; however, as discussed earlier, the surfactant was detected
in the final product as an indigenous oil by the SOW procedure. As such, it was not used for the
demonstration. Instead, a separate add-back material was used for the test runs. Because of the batch
nature of the operation, a dried feedstock could not be developed for subsequent add-back.
62
-------
The material used as add-back was bentonite, which comprises a major fraction of drilling
mud solids. The sand and silt fractions of EPA's Standard Soil Reference (SSR) were considered as
add-back; however, these materials had insufficient water holding capacity. Bentonite was added at a
dry solids to feed solids ratio of approximately 1:6; each test run was performed with approximately
185 pounds of dry solids, consisting of 25 pounds of bentonite and 160 pounds of feedstock solids.
These add-back solids were accounted for in subsequent mass balance calculations.
6.2.3.6 Oil/Water Separator
The oil/water separator (TK-107, Figure 4-1), was not used. Instead, organic and aqueous
condensates were collected in a drum, and the phases were manually separated with a separatory
funnel.
6.2.3.7 System Flushing
A flushing sequence was incorporated into each run. After centrifuging and the resultant
transfer of all solids to the dry side, fresh solvent was used to flush residual solids through the wet
side to the centrifuge. This allowed for more efficient recovery of the solids and effectively cleaned
the wet side operations before the next extraction pass.
6.2.3.8 Recycling of the Centrifuge Cake During the Third Extraction
Centrifuge cake was generated at the end of each extraction. The slurry was centrifuged once
in the first two extractions of each test run. This produced a cake with approximately 50 percent
solids, which was actually a slurry. Although suitable for return to the fluidizing tank, a higher
solids content was needed for efficient processing through the desolventizer. During the third
extraction, the centrifuge cake was collected and passed once more through the centrifuge before it
was discharged to the desolventizer.
63
-------
6.2.4 Modifications to the Sampling and Analysis Plan - * -
The sampling and analysis plan was revised because of the modifications to the pilot plant.
These changes are discussed in the following subsections.
6.2.4.1 Slurry Sampling
The slurried feedstock was sampled on the first pass after it was dried (evaporated). This
differed from the original plan, in which sampling was planned before heating.
6.2.4.2 Centrifuge Cake Sampling
The cake was sampled in the first and second extractions, as well as after the first centrifuge
pass of the third extraction. Due to the safety hazard created by the operating temperature (250 to
350°F) of the desolventizer, the centrifuge cake was not sampled during the second centrifuge pass of
the third extraction. The safety hazard was due to the hot gases (250°F) circulating through the
desolventizer and into the centrifuge chute.
6.2.43 Condensate Sampling
' The collection and sampling procedures for process condensates were revised. Evaporator
condensate was collected in the condensate tank during the extraction. After the evaporated slurry
was transferred to the centrifuge feed tank, the water and oil phases were manually separated into two
separate drams. The vapor condensate was collected in another container. Water and oil phases of
the vapor condensate were manually separated and composited with the water and oil phases of the
evaporator condensate before sampling.
6.2.4.4 Addition of Scrubber Liquid Sample
A new sampling location was added for the scrubber liquid from the desolventizer. The
scrubber solvent, after desolventization, was sampled and analyzed by the SOW procedure. This
64
-------
sample was needed to account for solids losses to the scrubber liquid, which were observed during the
initial shakedown runs.
6.2.4.5 Elimination of Distilled Solvent and Indigenous Oils Sampling
Distilled solvent and indigenous oils were to be sampled to demonstrate recovery of solvent
through distillation. These sampling locations were eliminated when the distillation step was
cancelled.
6.2.4.6 Elimination of Third Test Run Sampling
All sampling for the third test run was cancelled due to the cancellation of the test run itself.
6.3 OPERATING CONDITIONS
Certain operating conditions are critical to the performance of the C-G Process. These
conditions are related to the evaporative extraction pass and the desolventizing operation.
The evaporative extraction process was to operate at 200 to 250PF, under full vacuum, to
ensure complete removal of water, or drying of the slurry. Subsequent extractions were to operate at
atmospheric pressure and temperatures of 130 to 180PF. Temperature and pressure were not
considered critical after the slurry was dried.
Table 6-1 summarizes the critical operating conditions and objectives. The temperature and
pressure objectives of the evaporative extraction (Extraction A) for the blank run and both test runs
were met. The evaporator process vapor (Location A6) temperature was slightly lower than the
objectives. This was not a significant deviation from the objectives, since the slurry was already dry
and the slurry temperature (Location A2) was within the stated objectives.
65
-------
TABi.fc 61.
SUMMARY OF C RITICAL OI'liRAl INti DATA
Os
On
flpnrUm ffwm
MmAc IUm ¦ '
IMRmI
TtMt 9
t WlittWI:
¦3
:'a aif flyn
WSm
T«wfwntMr«
PV)
. i-fniwwt.:
<**«)
Tmjpwtwv
en
: ; From*
Wl>
en
tnmm*
W9mm*
A2
Recirculated Slurry
A
200 - 250
0 50
214
Atmospheric
201
Atmospheric
203
Almoiphcrk
through Evaporator
B
130 - 180
0 50
-
-
154
Atmospheric
152
Aunoipheric
C
130 - 180
0 - 50
•
153
Atmospheric
153
Atmoaphcric
A6
Evaporator Proccia
A
200 - 250
Vacuum
199
10 8
199
11.3
198
-10 9
Vapor
B
130 - 180
Atmospheric
-
94
Atmospheric
99
Atmosphcric
C
130 180
Atoto spheric
-
-
101
Atmospheric
99
Atmospheric
AI2
Vapor/Gas to
Dcsolveittiicr
C
350 - 450
-
395
-
454
-
445
All
Dcsolvcnti/ci Oil Ga»
c
150 250
•
191
-
184
219
-
AN
Similiter Gas
c
200 -275
-
198
161
-
169
•
-------
Table 6-1 also presents the revised temperature objectives for the desolventizer. These
objectives were met, but the low desolventizer off-gas temperatures, relative to the original objectives
(225 to 350^), may have contributed to slightly higher final product solvent concentrations.
The temperature objective of the scrubber gas (Location A14) was 200 to 275°F. This was to
assure quenching of the solvent vapor without condensing water. Condensed water in the scrubber
could result in blockages in the scrubber, which happened in the initial blank run attempt. The
temperature objectives were not critical for a completely dry slurry. Although the observed
temperatures during the demonstration were slightly lower than planned, this is not considered a
significant deviation since the slurry was already dry.
Appendix A summarizes all system monitoring data.
An equipment blank run was performed to characterize background contaminant levels and
identify materials contributed by the system. The pilot plant was newly constructed for the
demonstration. Several unit operations had been part of an earlier DTC pilot plant; however, all
piping was new. No waste material was charged to the system prior to the blank run. Only clean
inert materials such as the SSM silt and bentonite were used in the shakedown and pretest runs, as
well as solvent. Surfactant was also added in one of the pre-blank runs.
Fresh solvent was sampled from a random drum and analyzed for metals and solvent. The
following metals were detected:
6.4
RESULTS OF BLANK RUN
Aluminum
Boron
Chromium
Iroa
Nickel
<5.6 uglg
11.2 uglg
4.1 uglg
18.8 uglg
1.9 /ig/g
These results are all at or near detection limits, which ranged from 0.25 to 25 uglg.
67
-------
The blank run was conducted on August 4, 1991. It was similar to the test runs, except that
one extraction was performed instead of three. The feedstock for the blank run consisted of 153.5
pounds of bentonite, of which 16.21 pounds was absorbed water. An additional 11 pounds of water
was added after the bentonite was fluidized in 1,543 pounds of solvent. This yielded a feedstock with
a total water content of 16.5 percent and 83.5 percent solids. Section 6.4 describes the critical
operating conditions. AH monitoring data is presented in Appendix A. All sampling was conducted in
replicate.
Table 6-2 presents the analytical results for the blank run. The feedstock (bentonite) contained
near trace levels of six VOCs, the highest of which was toluene at 63.1 fxg/kg. The values denoted
with a less than sign (<) indicate that one of the replicate results was less than the detection limit. No
acid extractable SVOCs were detected, and six base/neutral extractables were detected. Only
bis(2-ethylhexyl)phthalate was detected in both replicates. This compound is a plastics component and
may have been due to contamination from plastic gloves or other plastic materials.
Several metals characteristic of bentonite were found in the blank feedstock solids. The solids
contained 10.57 percent water due to their hygroscopic characteristics. No indigenous oil, solvent, or
TPH was detected.
The centrate generated in the blank run was analyzed for metals, SOW, solvent, and TPH.
Organics were not determined due to matrix interferences. Metals concentrations were relatively low
as compared to the feedstock, suggesting that the metals remained partitioned to the bentonite solids.
This was confirmed by the metals results for the treated solids, which were essentially equivalent to
the feedstock results.
The centrate also contained 0.7 percent indigenous oil, as did the final product at 1.17
percent. The indigenous oil found in the blank run products may be attributable to residuals of
surfactant from pilot plant shakedown operations. The surfactant was detected as indigenous oil by the
SOW procedure.
68
-------
TABLE 6-2. CARVER-GREENFIELD PROCESS BLANK RUN AVERAGE ANALYSIS
DATA <"
Treat*i
Wad*-'"
Soiftat
" FwiMMt
Fwdrfock
Ctntratt
Sofidr
Coadnnt*
CoadanM
VOC
methylene chloride
<5.72
na
NA
<250
NA
(;ig/kg)
acetone
<35 8
NA
NA
3.775
NA
(wet wi)
tetnchloroeihene
<3.15
NA
NA
<250
NA
toluene
63 I
NA
NA
<250
NA
«thylbenzen«
<3.80
NA
NA
<250
NA
total xylene (o.m.pj
2.99
NA
NA
<250
NA
svoc
ND
NA
ND
ND
NA
acid ext
Gig/kg)
(wet wi)
SVOC
phenanthrene
<217.5
NA
<50.000
<50
NA
b/n exi
di-n-butyl phthalate
<218
NA
<50.000
<50
NA
Oig/kg)
bis(2-ethylhexyl)
NA
(wet wt)
phthalate
1.071.5
NA
<50.000
42.3
NA .
di-n-octvl phthalate
<273
NA
<50.000
<50
NA
2-methyl rupihalene
<603
NA
< 100,000
< 100
NA
Meiala
aluminum
9,850
<5.00
8525
3.32
<7.90
(Mi'g)
banum
64.5
<0.25
82.3
0.023
<2.50
(wet wt)
beryllium
1.46
<0.25
1 30
<0.005
<0.23
boron
22.2
< 10.
15 75
<0.33
<15.7
cadmium
o.«
<0.25
0.43
<0.005
<0.23
calcium
12.250
<25
11,150
3.23
<25
chromium
4 34
2.79
15 3
0 059
3.73
copper
2.55
0.55
2.37 .
<0.01
0.56
iron
13,800
11.05
12.550
2.86
15.23
lead
30.1
<2 5
27.35
<0.05
<2.5
magnesium
3305
<25
2.865
1.29
<25
nunganeM
_ 503.5
<0.25
455.5
0.067
<0.25
nickel
3 95
1.33
9 85
0.034
1.44
potassium
623.5
<50.0
771
0.50
<50
sodium
9.350
28.95
8.555
3.75
<27.3
strontium
217.5
<2.50
200.5
<0.055
<2.50
zinc
60.4
1.97
58.6
0.091
<0.50
SOW
solid*
87 7
<0 01
38.7
NA
NA
(%)
indigenous oil
<0.11
0.70
1.17
NA
NA
(by wt)
water
10.6
<0.01
0.10
NA
NA
Solvent
Isopar-L
<0 10
56.8
4.58
0.73
55 5
(%)
(by wt)
69
-------
TABLE 6-2. CARVER-GREENFIELD PROCESS BLANK RUN AVERAGE ANALYSIS
DATA (CONTINUED)"1
Treat ad
¦ Water •
¦ Solftot
CUs
PamaMar
Feedstock
Cantrata :
Solids
CoodeosaM
^ Cmtiimn ¦
TPH
toul petroleum
<10 0
1.170.000
131,000
137.5
1,060,000
hydrocartjon
(wet wi)
Conventional
pH
NA
NA
NA
7 05
NA
Polluunu
alkiluuty, toul
NA
NA
NA
4.10
NA
(mg/L)
jciduy, iot»l
NA
NA
NA
17.2
NA
BOD j
NA
NA
NA
34.8
NA
COD. dichroimte
NA
NA
NA
S77.5
NA
nttrogen, •mmonit
NA
NA
NA
<0.05
NA
nitrogen, Kjeldihl
NA
SA
NA
0.82
NA
>oiidi. suspended
NA
NA
SA
146.5
NA
sulfite
NA
NA
NA
<10.0
NA
"NA = Not analyxed
ND » No Compound Detected
b'n " B««e'ncutrtl
70
-------
The final product also contained 4.58 percent solvent. This relatively high level of solvent
was probably to be due to the centrifuge's inefficiency, which resulted in high solvent loads to the
desolventizer. For this reason, an additional pass through the centrifuge was incorporated into the test
runs after the third extraction.
The only organics detected in the water condensate were acetone (3,775 pg/kg) and
bis(2-ethylhexyl)phthalate (42.3 ng/kg). Acetone was not detected in the feedstock but was
occasionally used in sampling equipment decontamination. Bis(2-ethylhexyl)phthalate was found in the
feedstock, probably due to plastic gloves used in sample handling. All metals detected in the water
and oil condensates were at trace levels.
The solvent content of the centrate and condensed solvent appeared to be low. Both samples
should have been 100 percent solvent. The TPH values for centrate and condensate solvent suggest
that the solvent content was much higher than the reported result. This is discussed further in Section
6.11, which presents the material balance for the blank run.
The blank run results indicate that the equipment did not contaminate processing materials.
The more significant findings were (1) the presence of acetone and bis(2-ethylhexyl)phthalate in some
samples, probably due to sample handling and decontamination, and (2) detectable indigenous oil in
the centrate and on the final product, probably due to surfactant residuals in the system. Because the
level of contamination identified in the blank run is not considered significant, test run results were
not blank corrected.
6.5 FEEDSTOCK CHARACTERIZATION
The analyses used to characterize the feedstock included SOW, TPH, solvent, VOC, SVOC,
and metals. The principal waste characteristics, with respect to the primary objectives of the
demonstration, were the solids, oil, and water content. These results are presented in Table 6-3. The
two feedstocks were similar in solids content but differed in oil and water content. The feedstock for
the first test run was higher in oil content and lower in water content than the second test run. Both
71
-------
feedstocks were considered suitable for the C-G Process. Although they differed in oil and water
content, no changes in operations were required.
TABLE 6-3. COMPOSITION OF WASTE FEEDS
Test Rub No.
Solids <%)
Oil (%)
Water (%>
(By Wt.)
(By Wt.)
(By Wt)
1
52.35
17.48
21.75
2
52.44
7.24
34.77
Tables 6-4 and 6-5 present the average analytical results for the feedstock in Test Runs 1 and
2, respectively. For sample values less than a detection limit, the detection limit was used for
averaging. These tables will be referred to in subsequent discussions regarding treatment
performance. The complete feedstock characterization, including the results of the six replicates, is
presented in Appendix B.
In the feedstock for Test Run 1, xylene was the only organic compound (VOC or SVOC)
found above detection limits. Toluene and ethylbenzene (VOCs), and phenanthrene and
2-methylnaphthalene (SVOCs), were present but at less than the detection limits.
In the feedstock for Test Run 2, only ethylbenzene and toluene were found above detection
limits. As with Test Run 1, several organics were present but at less than the detection limits. These
included benzene (VOC) and phenanthrene, 2-methylnaphthalene, and naphthalene (SVOCs).
The most significant metals in both feedstocks were aluminum, barium, calcium, iron, and
magnesium. TPH levels ranged from 80,000 to 150,000 mg/kg, confirming the high oil levels
indicated by the SOW results. The feedstocks had no detectable solvent and had ignitability levels
greater than 100*C.
72
-------
TABLE 6-4. CARVER-GREENFIELD PROCESS AVERAGES KOR TEST RUN I"'
RmI PradacM
ParwHen
Urat$
ttack
Slnnied
: feedstock i
' Coiirale '¦
CarfriAige
Trautai
Solids
CtadL' '
CmI.
''' A
B
c
A ¦
B
"" "A
¦fig
c
V(>C
loluciu:
clhylbeiucuc
Mai xylene (o.m,j>)
acetone
2 huunonc
(wcl wl)
546
993
3.658
<5,000
<2 500
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<250
<250
<250
4.927
1 067
NA
NA
NA
NA
NA
SV(K? - acid cxlrJciaMc
phciH>l
(wcl W|)
<- 100.000
NA
NA
NA
NA
NA
NA
NA
NA
NA
<660
<203
NA
SV(>C - li/n cxUjcIjMc
phciuiillirciic
2 uiclhyliiaiililli.ilciu:
iMtjitioiouc
l»is(2 clhyllicxyl)|iltiliulalc
ili » twlyl phlhalalc
(wo! wl)
15,950
26, IH3
< 50,000
< 50.000
< 50.000
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
257
<-660
< 364
592
<321
«. 250
< 5(H)
<250
<250
<250
NA
NA
NA
NA
NA
aluminum
antimony
haiiom
Ixrylliuin
lioion
cadmium
calcium
chromium
cobali
copper
iron
lead
magnesium
nuingancttc
0'b's)
(wcl wl)
10,663
<50
2990
0 831
<24 7
0 578
2,13$
25 4
7 44
16.4
13.570
41 0
1.517
373
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
24 4
<5 0
7 3
<0 50
<20
<0 50
<50
<10
<5 0
<10
40 5
<5 0
<5 0
1 55
3.452
<5.0
904.6
<0 58
<20
<0 50
<723
8 61
<5 94
<6 2
3,998
< 16 2
<453
138
79 1
<5 0
10 9
<0 50
<20
<0 50
<50
< 1 46
<5 0
<10
78 0
<5.0
<50
3 05
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
16,833
<50
3,193
1 37
<20
<0 5
5,243
412
14 8
26 4
20,333
46 1
2,460
695
2 61
<0 052
0 0382
<0 0050
<0 20
<0 0050
4 28
<0 0103
<0 050
<0010
2 68
<0 050
1 085
0 093
11 43
<5 0
<0 50
<0 50
<20
<0 50
<50
<1 0
<50
<10
<5 0
<5 0
<50
<0 50
-------
TABLE 6-4. CARVER-GREENFIELD PROCESS AVERAGES FOR TEST RUN 1 (CONTINUED)"'
f
fatal Product
¦ill
Sbnkd
Treated
CmmL "
ComI.
ParanHen
Uafo
Feedstock
Cent rale
Cak*
Sofida
Wm«
...
m§mm
A
B
c
' A "
B
. . C: . "
A
"¦ B '
c
Mcul*
(ft't)
;
HHiJylitJcmjfn
(wel wl)
<5 0
NA
NA
NA
<5 0
<5 0
<5 0
NA
NA
NA
43 3
<0 050
<5 0
nickel
13.3
NA
NA
NA
<2 0
<6 86
2 19
NA
NA
NA
287
<0 0384
<2 0
potassium
485
NA
NA
NA
<50
<308
<50
NA
NA
NA
1310
<0 56
<50
MkllUIII
135
NA
NA
NA
<50
<73
<50
NA
NA
NA
2103
3 05
<50
ktloitlilllll
6-15
NA
NA
NA
<5 0
<22 9
<5 0
NA
NA
NA
125
0 0576
<5 0
vanadium
24 3
NA
NA
NA
<5 0
<113
<5 0
NA
NA
NA
28 0
<0 050
<5.0
zinc
160
NA
NA
NA
1 82
50 86
2 34
NA
NA
NA
145
0 192
<10
sow
(*)
boliii.s
(l.y wi)
52 35
10 54
8 17
8 89
0 12
Oil
<0 11
58 64
57 44
57 68
¥6 42
NA
NA
indigenous «>il
17 48
10 83
0.45
0 30
8 35
0 94
0 33
4 90
2 47
2 16
1 43
NA
NA
WJlCf
21 75
<0 1
<0 1
<0.1
<0 1
<0 1
<0.1
<0.1
<0 1
<0 1
<0 1
NA
NA
Solvent
<*)
Isopai L
(by wl)
<0.1
75 18
82 06
90 23
89 55
100 29
98 02
36 02
42 44
41 33
0 88
0 900
96 07
TTII
Oig/g)
(wcl Wl)
146.830
NA
NA
NA
999,670
998,670
103,130
NA
NA
NA
7,910
1,440
952,670
Ignilahilily
'C
> 100
94 2
Conventional Pollutanu
,.n
(nig/L)
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
4 57
NA
alkalinity, lolal
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<2 0
NA
acidily, lolal
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
36 5
NA
BOD,
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
76
NA
COD, diclirouulc
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
1,193
NA
nitrogen, ammonia
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<0 050
NA
mitogen, Kjtldahl
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
0 535
NA
aolida, suspended
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
82 3
NA
vultalc
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
10 0
NA
"'NA = nol analyzed
©
-------
TABLE 6 5. CARVER GREENFIELD PROCESS AVERAGES FOR TEST RUN 2
M hodxti
Panmetcn
U"M*
Jtod-
Stanitad -
Feedstock
Cotftfgft' '
Cartftfoge
Sainfc '
CM.
W«Mr
A.
'¦ a
c
A
' : B
e
A
C :
x
vac
Oig/kg)
hctt/citc
(wcl wl)
1,076
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<250
NA
InluClkl
1,046
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<250
NA
clhylhoik/cuc
1,887
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<250
NA
total xylene («» in J»)
8,873
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<250
NA
a^cl.iuc
<5,000
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
2,280
NA
2-buiJiiuiic
<2,500
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<395 7
NA
SVOC - aciil cMiacuWc
U-s'm
phemd
(wcl wl)
ND
NA
NA
NA
NA
NA
NA
NA
NA
NA
ND
ND
NA
SV(lC l»/n cxliiiciablc
Ms'iK)
8.127
NA
NA,
NA
NA
NA
NA
NA
NA
NA
< 1.65(1
<50
NA
2 metltyJiiapittluikiic
(wcl wl)
49,150
NA
NA
NA
NA
NA
NA
NA
NA
NA
2,317
< 100
NA
luptilhalcuc
< 28,420
NA
NA
NA
NA
NA
NA
NA
NA
NA
1,055
<50
NA
Im->(2 clliylhc*yl)|tliiliaUlc
<50,000
NA
NA
NA
NA
NA
NA
NA
NA
NA
1,407
<196 3
NA
di it Imlyl ptiilulalc
< 50,000
NA
NA
NA
NA
NA
NA
NA
NA
NA
< 1.650
<20 1
NA
McuU
U'B'f)
ahiiniiiiiiii
(wcl wl)
7,352
NA
NA
NA
24 77
19 43
19 97
NA
NA
NA
8,6(17
13 33
<9 94
iMiuim
576
NA
NA
NA
40 53
32 07
32 87
NA
NA
NA
3.173
<0.50
<0.50
hcryllmnt
0 70
NA
NA
NA
<0.50
<0 50
<0.50
NA
NA
NA
112
<0 50
<0 50
boron
<21 93
NA
NA
NA
<20
<20
<20
NA
NA
NA
<20
<20
<24 33
cadmium
400
NA
NA
NA
<0.50
<0.50
<0 50
NA
NA
NA
5 55
<0 50
<0.50
calcium
7,785
NA
NA
NA
<50
<50
<50
NA
NA
NA
12,033
<52 37
<48.27
chromium
139.5
NA
NA
NA
1 54
<0,95
<1.07
NA
NA
NA
318
<1.0
<10
cohail
9 41
NA
NA
NA
<5 0
<5 0
<5 0
NA
NA
NA
13
<50
<5 0
copper
88 5
NA
NA
NA
<1.35
< 1
<1
NA
NA
NA
107
<10
<10
iron
20,733
NA
NA
NA
65,30
33 93
32 *7
NA
NA
NA
36,433
<6 46
<5 0
lead
206
NA
NA
NA
<5.0
<5 0
<5 0
NA
NA
NA
248
<5 0
<5.0
magncaium
1,252
NA
NA
NA
<50
<50
<50
NA
NA
NA
1,927
<50
<50
manganese
276
NA
NA
NA
1 12
0 64
<0 76
NA
NA
NA
505
<0 50
<0 50
molybdenum
25 4
NA
NA
NA
<5 0
<5 0
<5 0
NA
NA
NA
49
<5 0
<5.0
-------
TABLE 6 5. CARVER GREENFIELD PROCESS AVERAGES FOR TEST RUN 2 (CONTINUED)
HuI Product*
Piramrten
Wu
flock
Startied ...v
FeetfahxJf
Castrate
CeatriAuM
CmM
Tmuri '
Sofi*
CwA
Water
Solvent
A
T: B ' i'
•c-
A
B
" e
A
B
c
Mcial*
(w's)
(lickcl
(wcl wl)
2« 8
NA
NA
NA
<2 0
<2 0
<2 0
NA
NA
NA
146
<2 0
<2 0
[M>4u*MUIU
74*
NA
NA
NA
<5 0
• SO
<50
NA
NA
NA
969
<50
<50
blHillMII
600
NA
NA
NA
<50
<52 57
<51 57
NA
NA
NA
2,310
67 97
<5J 7J
Mioiilaiiii
271
NA
NA
NA
<5 0
<5 0
<%U
NA
NA
NA
378
< SO
<50
VUlUilmnl
22 0
NA
NA
NA
<5 0
<5 0
<5 0
NA
NA
NA
21 J
<5 0
<5 0
/iiit-
1.01J
NA
NA
NA
6 76
2 60
< 1.94
NA
NA
NA
1,153
< 1 0
< 1 21
SOW
<*>
Solid*
(by wi)
52.44
It 26
9 13
9.16
<0 12
<0 1
0 15
68 19
64 35
66.69
98 Jl
NA
NA
iriiJi{'ctii m.v oil
7 24
5 89
0.36
0 20
6 61
0 79
0 10
J 64
1 26
I 06
0 85
NA
NA
W4ICI
i4 77
<0 1
<01
<0 1
<0.1
<0 1
<0 1
<0 1
<0 1
<0 1
<0 1
NA
NA
St'fvciU
<*)
Iw.|>ai L
(by wl)
< 4) i
78 53
91 84
9 j 16
87 24
100 64
102 JO
26 40
J1 55
Jl 23
0 99
<0 1
99 70
Mil
(fe'si
(wcl Wl)
N9..1H0
NA
NA
NA
952.J30
964.670
1,010,000
NA
NA
NA
6,620
313
923,110
l^jui jluliiy
•c
> MIO
NA
NA
NA
NA
NA
NA
NA
NA
NA
>100
NA
NA
t'oiivciHumal Pollutdnlb
P'«
(mg/L-)
NA
NA
NA
NA
NA
NA
NA
NA
NA
na
NA
6 82
NA
alkalinity, l«»aal
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<1 40
NA
¦sillily, loul
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
310
NA
BOD,
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
12 7
NA
COD, ilkhruiiuile
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
395
NA
mirugcn, •mmtuua
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<0 05
NA
nitrogen, Kjclddhl
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<0 2
NA
wlida, guspeniied
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Na
70 33
NA
•ulftic
(injj/l.)
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
1000
NA
ND = ih» tttntfMHtiHl*
NA - iuii analy/cd
-------
6.6 SEPARATION OF SOLIDS, OIL, AND WATER MATRICES BY THE CARVER-
GREENFIELD PROCESS
The primary objective of the demonstration was to evaluate the process' ability to separate
petroleum based hydrocarbon contaminated soil into its constituent solids, oil, and water
fractions. This objective was met by interpreting the results of the SOW, TPH, and solvent analyses.
Tables 6-4 and 6-5 present the SOW, solvent, and TPH results for both test runs. The results
are shown as averages of several replicate samples for each sample location and are presented left to
right in the order in which the process is operated. The three extractions are denoted as A, B and C
for the slurried feedstock, centrate, and centrifuge cake results.
In Test Run 1 the SOW analysis indicated that the feedstock consisted of 52.35 percent solids,
17.48 percent indigenous oil, and 21.75 percent water. The TPH result for the feedstock averaged
146,833 fig/g or 14.68 percent by weight. A comparison of the TPH result to the indigenous oil result
suggests that some materials are detected as indigenous oils but not detected as TPH. This
characteristic is important when interpreting the final product results, as discussed later in this
section. No Isopar-L was detected in the feedstock.
The most significant results for the slurried feedstock (after solvent addition/fluidization) were
for the water and indigenous oil. The SOW analysis showed that effectively all the water was
removed in the first extraction, confirming the observation that all the water condensate was collected
during the first extraction. Most of the indigenous oil was also extracted to the solvent phase in the
first extraction. The indigenous oil concentration went from 10.83 percent in the first extraction to
0.45 and 0.30 percent in the second and third extractions, respectively. This was confirmed by the
indigenous oil results for the centrate; the first extraction contained 8.35 percent indigenous oil while
the centrate from the subsequent two extractions contained 0.94 and 0.33 percent, indicating that most
of the oil was extracted in the first pass.
The feedstock for Test Run 2 was similar in solids content to Test Run I but differed in oil
and water content, as shown in Table 6-6. The slurried feedstock and centrate results indicated that,
11
-------
similar to Test Run 1, all of the water and most of the indigenous oil was removed in the first
extraction.
The significance of the indigenous oil removal efficiency in the first extraction is shown in
Table 6-6, which is an excerption of indigenous oil and solids data from Tables 6-4 and 6-5. The
ratio of indigenous oil to solids (gig) decreases through each extraction to the final product. Of the
indigenous oil extracted, 78.1 and 65.9 percent was removed in the first extraction of Test Runs 1
and 2, respectively. Indigenous oil removal diminished with each subsequent extraction; however, it
also apparently increased slightly through the desolventization process (Extraction C to the final
product). This is probably due to the higher operating temperature and vaporization in the
desolventizer (350 to 450°F) in comparison to the extractions (150 to 250°F).
TABLE 6-6. OIL REMOVAL EFFICIENCY OF EXTRACTIONS
Test Run 17". f"-.
Tefit Rub I
Sample
Location
Indigenous
Oil/Solid
fe/B>
Fraetioa ot
Total
Indigenous
00 Removed
<*>
Indigenous
Oil/Solid
Fraction of
Total
Indigenous
Oil Removed
W
Feedstock
0.334
.
0.138
-
Extraction A
0.084
78.1
0,053
65.9
Extraction B
0.043
12.8
0.020
25.6.
Extraction C
0.037
1.88
0,016
3.1
Final Product
0,014
7.29
0.009
5.4
The indigenous oil consists of TPHs and other material detected as oil by the SOW procedure
but not measurable by the TPH procedure. These materials may be polar organics or surfactants
which are soluble in toluene (SOW procedure) but are retained on silica gel (TPH procedure). As
TPH is the most commonly regulated parameter used with regard to oil contamination, oil removals
through the C-G Process were developed both in terms of oil determined by the SOW procedure and
by TPH analysis. Since the bulk of the residual oil measured in the final solids product was Isopar-L,
oil removal efficiency is also expressed as indigenous TPH. Indigenous TPH removal is a calculated
value (initial feed TPH minus final product TPH minus final product Isopar-L), which estimates the
quantity of TPH originating in the waste feed that remains on the final solids product. The
78
-------
calculation must be made because Isopar-L is detected by the TPH procedure. Table 6-7 presents
estimated oil removal efficiencies.
TABLE 6-7. INDIGENOUS OIL AND
TPH REMOVALS
Oil Removal Efficiency (%}
. .TestRob.'
Indigenous
Indigenous*
Number
Oil
TPH
TPH
1
91.8
94.6
>99 9
2
88.3
92.6
>99 9
'Calculated Value
Indigenous oil removals are lower than indigenous TPH removals due to toluene soluble
organics (SOW procedure) which are not detected in the TPH procedure. Indigenous TPH removal
was over 99.9 percent for both test runs. TPH removals were 94.6 and 92.6 percent for Test Runs 1
and 2, respectively.
6.7 FATE OF METALS THROUGH THE CARVER-GREENFIELD PROCESS
The C-G Process is not represented to have any metals fixation capacity. Metals could either
be retained on the solids, or dissolve into the aqueous and oil phases in the slurry. Several metals
were detected in the feedstock, the most significant of which were aluminum, barium, calcium, iron,
magnesium, sodium, potassium, and zinc (all greater than 500 /tg/g wet weight).
Very few metals were detected in the centrate and condensed oil. Those detected were found
at relatively low levels in comparison to the feedstock. Metals in the water condensate were found at
low levels. The final product results indicate that most metals in the feedstock were retained in the
final solids product.
Table 6-8 presents the calculated results (on a dry weight basis) for the major metals and the
calculated percent retained in the final solids product. For several metals, more than 80 percent of the
feedstock' metals content was retained on the final solids product. In two instances, barium in Test
Run 1 and aluminum in Test Run 2, the recovery was approximately 60 percent.
79
-------
TABLE 6-8. SUMMARY OF SIGNIFICANT METALS
(DRY WEIGHT BASIS)
Feedstock
Final Solids
Product
Retained la
Final Solids
Product
Test Raa I
Test Rua 2
Test Run I:
Test Rub 2
Test Rua I
Test Run 2
(titR>
Wr>
:V X';: W
m
Aluminum
20,369
14,023
17,458
8,754
86
62
Barium
5,711
1.099
3,312
3,228
58
294
-------
solvent may be retained in the recycled solvent and actually reduce solvent make-up requirements.
Additionally, these may also be retained in the residual solids in proportion to the solvent which is
retained.
The presence of indigenous oil and Isopar-L in the samples (even at residual levels) interfered
with the detection of VOCs, and SVOCs, requiring sample dilution. This increased the method
detection limits, precluding quantitative tracking of specific organics through the process.
Table 6-9 summarizes the detected VOC and SVOC compounds in the feedstock, final solids
product, and condensed water. In both test runs, the VOC compounds detected in the feedstock were
not found in the condensed water. Due to the elevated detection limits, these compounds could not be
measured in the final solids product.
TABLE 6-9. SUMMARY OF VOC AND SVOC RESULTS
Test Rati
Test Run 2
Ha*f
Caedented
Ffaal
Condcosed
Feedstock
Protect
Water
Feedstock
Product
Water
Parameter
(NCkf)
WW
wu
VOC
benzene
<1,230
<125.000
<250
1.076
<230
toluene
546
<125,000
<250
1,046
<250
ethylbenzene
993
<125,000
<250
1,887
<250
loul xylene
3,658
<125,000
<250
8.873
<250
acetone
<5,000
<500.000
4,927
<5,000
2,280
2-buUnone
<2,500
<250,000
1,067
<2,500
<396
SVOC - b/n emncubles
phenanihrene
15,950
257
<250
8,127
<1,650
<50
2-meihyi Mpduiene
<26,183
<660
<500
49,150
2,317
<100
lupthaicne
<50,000
<364
<250
<28,417
1,055
<50
bi»(2-eliiyU>exyl)phthalit£
<50,000
592
<250
<50,000
1,407
<196
di-n-butyl phihelelr
<50,000
<321
<250
<50,000
<1,650
<20
Two VOCs, acetone and 2-butanone, were found in the condensed water at levels below the
detection limit for the feedstock. Acetone was also found in the blank run water condensate.
Several SVOCs were found in the feedstock. These compounds were also in the final
product, although at significantly reduced levels. This indicates that the process removes organics
from the solid and water phases to the solvent oil phase, which is consistent with expectations and
81
-------
developer claims. The.heavier organics (such as the polyaromatic hydrocarbons [PAHs] and
phthalates) would probably be retained in the separated indigenous oils fraction after distillation.
6.9 TCLP ANALYSIS OF FINAL PRODUCT
TCLP tests were performed on the final solids product from both test runs. Appendix B
contains a complete summary of the TCLP results, including the appropriate RCRA TC regulatory
criteria. TCLP results indicate that the final solids product in Test Runs 1 and 2 was not a RCRA
characteristic waste. The dry solids product does not leach metals, VOCs, or SVOCs above the
RCRA regulatory limits.
The only elements detected in the leachate were barium and silver. Silver was detected only
slightly above the detection limit in the final product leachate of Test Run 2.
When solids fractions increase from 50 percent in the feedstock to 98 percent in the final
product, a proportional increase in metals in the final solids product should be expected, presuming
the metals stay bound to the solids. A comparable increase in the metals concentration of the TCLP
extract could also be expected. This concentration effect could be a consideration in selecting the
C-G Process. The process could produce a hazardous material, with respect to TCLP metal levels,
from a nonhazardous raw waste with significant metals content.
6.10 SUMMARY OF RESIDUALS CHARACTERISTICS
The residuals generated from the C-G Process comprise the final dry solids product, the
separated water and oil phases, the vapor phase, and spent solvent.
The final solids product was a dry powder similar to bentonite in appearance. Values for all
organics (VOCs and SVOCs) and metals were below the RCRA TC Rule limits for characteristic
hazardous wastes. TCLP results for the final solids product of Test Runs 1 and 2 also indicated that
the process does not leach metals, VOCs, or SVOCs above the RCRA regulatory limits. Residual
TPH levels were at near trace concentrations, indicating that the final solids product would be suitable
for land disposal.
82
-------
The water product from Test Runs 1 and 2 was a clear liquid with a strong odor, with low
suspended solids and BOD, but high COD levels. TPH analysis results correlated well with the COD
analysis results in both test runs, suggesting that most of the COD was related to Isopar-L and lighter
organics in the water product. Acetone and 2-butanone were detected at trace levels. No other
VOCs or SVOCs were detected. Metals analyses also showed only trace levels. The characteristics of
the water product were similar to dilute municipal wastewater. The waters also complied with the
OCPSF industrial categorical discharge limits with respect to metals and organics concentrations.
The condensed solvent product was a clear liquid in both test runs. VOCs and SVOCs were
not analyzed due to excessive detection limits in the solvent matrix. Metals analysis indicated that
most metals were below detection limits. The condensed solvent was mostly Isopar-L and hence could
be recycled as carrier solvent in the C-G Process.
Although most of the vapors produced were condensed, some escaped to the vent. These
vapors were passed through a canister filled with activated carbon. Solvent analysis of the activated
carbon showed approximately 5 to 10 percent Isopar-L on carbon.
Centrate produced in both test runs was a dark liquid with strong odor. The analyses of
centrates from both runs showed relatively higher indigenous oil and TPH levels in the first extraction
centrate in both test runs. The indigenous oil and TPH levels decreased sharply in the subsequent
extractions, indicating that most indigenous oil was removed in the first extraction. Solvent analysis
of the centrate showed approximately 87 to 89 percent Isopar-L in the first extraction centrate
produced in the two test runs. Second and third extraction centrates showed Isopar-L levels above 98
percent. Due to lack of time and other problems, the final distillation step demonstrating the
separation of carrier oil (solvent) from the indigenous oil was cancelled. Therefore, the
characteristics of the final indigenous oil product and solvent produced after distillation are not
known. However, the centrate should be easily split by fractional distillation to its constituent heavy
oil and light oil (Isopar-L) components, allowing cost-effective recycling of the recovered solvent and
more efficient disposal of the indigenous oil fraction.
83
-------
6.11 MATERIAL BALANCES
Laboratory results and mass and volume measurements of materials charged to and removed
from the system were used to construct material balances around the system. Two types of balances
were developed. Gross material balances were performed for solids, oil, water, and solvent to
evaluate the quality of the laboratory results and mass and volume measurements. Material balances
for specific analytical parameters (specific metals and indigenous oil) were performed to qualitatively
determine the fate of these constituents through the process.
Figure 6-1 presents a simple schematic of the material balance around the C-G Process.
Process inputs include feedstock and solvent. These materials are charged to the process regardless of
batch or continuous operation.
Process additions are materials which were charged specifically for the needs of the
demonstration. The need for add-back has been previously discussed. Scrubber oil is generally a one-
time addition for a continuously operated system; however, under batch mode this was charged and
removed in the blank run and each test run. Flushing oil was used to flush out residuals in the system
after each run was completed. Isopar-L was used for both the scrubber and flushing inputs. Water
was added to the condensate tank as a tank heel to provide a visible level in the tank sight glass.
Water was also added to provide a vacuum seal on the condensate line.
In a continuously operated process with solvent recovery, the only material outputs are
indigenous oil, condensed water, product solids, and vapors. In a batch operated process without
solvent recovery, as used in the demonstration, the centrate included the solvent and most of the
extracted indigenous oil. The resulting duel phase condensate was manually split to organic and
aqueous phases.
-------
Process
Inputs -
oo
LA
Process
Additions
o
n v vu. >1
Carver-
Greenfield
Process
v"? vQ. vO VCP ^ ^
Process
Outputs
Figure 6-1 Components ol Material Balance Around the Carver-Greenfield Process
(Batch Operation)
-------
6.11.1
Gross Material Balance
Gross material balances were performed for the blank run and Test Runs 1 and 2. Total
quantities charged and removed were based on direct weight measurements. The component
quantities were estimated from these weights and the SOW and solvent analyses.
The gross material balance for the blank run is presented in Table 6-10. A total of 2,141
pounds of material was charged to the system, and the sum of recovered materials was 2,070 pounds.
On a total materials basis, 96 percent of the materials charged were recovered. By a similar approach,
on a constituent basis, 103 percent of the solids, 89 percent of the water, and 60 percent of the
solvent/oil was recovered.
The low solvent/oil recovery is probably due to an anomalous solvent analysis for the
centrate. The solvent result for the blank run centrate was 56.8 percent solvent. The centrate,
especially in the blank run, should be virtually 100 percent solvent. A check on the solvent result can
be made by subtracting the solids and water components from the total centrate quantity. This
approach suggests that the total oil component is 1,559 pounds rather than 896 pounds, resulting in 95
percent material recovery rather than 60 percent. The apparent solvent analysis error is attributed to
sampling and analytical errors.
The gross material balances for Test Runs 1 and 2 are summarized on Tables 6-11 and 6-12,
respectively. More than 5,400 pounds of materials were charged to the system in each test run. Of
the totals, more than 96 percent was accounted for in recovered materials. On a constituent basis, 80
percent of the solids, 107 percent of the water, and 96 percent of the oil charged to the system were
recovered in Test Run 1. Similarly, 79 percent of the solids, 95 percent of the water, and 97 percent
of the oil charged to the system was recovered in Test Run 2. These results suggest that the
measurement techniques and analytical methods sufficiently characterized the movement of materials
through the process. The results also indicate no significant losses or contributions to the process
occurred which were not incorporated into the material balance.
86
-------
TABLE 6-10. GROSS MATERIAL BALANCE FOR BLANK RUN
Components
Total
Quantity
Solids
Water
Total Oil»
(lbs)
0b»>
(lbs)
(It*)
Materials Charged
Bentonite
Feed
153.50
134.56
16.21
0.00
To Deoiler
11.00
9.64
1.16
0.00
Solvent/Oil
Solvent to Fluidization Tank
1,543.25
NA
NA
1,543.25
Scrubber Charge
145.25
NA
NA
145.25
Wet End Flush
97.75
NA
NA
97.75
Dry End Flush
110.00
NA
NA
110.00
Water
Condensate Tank Heel
66.75
NA
66.75^'
0.00
Vapor Condensate Line Seal
2.20
NA
2.20(b'
0.00
Water added to Fluidization
11.00
NA
11.00,bl
0.00
Total Charged
2,140.70
144.20
97.32
1,896.25
Materials Recovered
Centra te
1,558.75
0.00
0.00
895.97""
Condensed Water
87.50
NA
86.86'°
0.64
Condensed Solvent
54.50
NA
NA
30.26
Scrubber Liquor
201.00
0.20
0.00
200.80
Final Product
164.00
145.45
0.00
9.43
Final Product Sampling
4.16
3.69
0.00
0.24
Vent Gas (GAC)
0.52
NA
NA
0.52
Total Recovered
2,070.43
149.34
86.86
1,137.86""
Percentage Recovered
96.72
103.57
89.25
60.01""
"Calculated as sum of indigenous oii and solvent
^'Assumed 100% water
''Calculated as total quantity minus solvent
d,Poor oil recovery is due to low solvent results. By substituting the total quantity added (1,558.75) for
Total Oil, closure improves to 98.38%. This is a valid approach since the SOW analysis
indicated 0.00% solids and water in the centFate.
NA = Not analyzed
Note: Values below detection limit counted as zero tor mass balance
87
-------
TABLE 6-11. GROSS MATERIAL BALANCE FOR TEST RUN 1
Components
Total
Quantity
Solids
Water
Total OUw
(lbs)
(lbs)
(lbs)
(lbs)
Materials Charged
Feed
314.00
164.44
68.30
54.86
Solvent
Extraction A
1,698.25
NA
NA
1,698.25
Extraction B
1,694.60
NA
NA
1,694.60
Extraction C
1,628.25
NA
NA
1,628.25
Scrubber Charge
161.50
NA
NA
161.50
Bentonite
Add Back
25.00
21.92
2.64
0.00
To Deoiler
10.50
9.20
1.11
0.00
Water
Condensate Tank Heel
58.00
NA
ss.oo0"
NA
Vapor Condensate Line Seal
2.20
NA
2.20
-------
TABLE 6-12 GROSS MATERIAL BALANCE FOR TEST RUN 2
Components
Total
Quantity
Solids
Water
Total Oilw
(Jbs>
(lbs)
Obs)
0l»)
Material* Charged
Feed
333.50
174.89
115.72
24.21
Solvent
Extraction A
1,760.25
NA
NA
1,760.25
Extraction B
1,413.00
NA
NA
1,413.00
Extraction C
1,676.75
NA
NA
1,676.75
Scrubber Charge
160.00
NA
NA
160.00
Bentonite
Add Back
25.00
21.92
2.64
0.00
To Deoiler
10.00
8.77
1.06
0.00
Water
Condensate Tank Heel
68.25
NA
68.25*'
NA
Vapor Condensate Line Seal
2.20
NA
2.20
0.00
Condensed Solvent
207.50
NA
NA
206.88
Scrubber Liquor
180.25
0.18
0.00
180.07
Final Product
141.25
138.86
0.00
2.60
Deoiler Residual
10.00
9.83
0.00
0.18
Final Product Sampling
11.29
11.10
0.00
0.21
Vent Gas (GAC)
16.58
NA
NA
16.58
Total Recovered
5,253.12
162.36
181.25
4,889.21
Percentage Recovered
96.41
78.98
95.46
97.12
"'Calculated as sum of indigenous oil and solvent
MAssumed 100% water
(clCalculated as total quantity minus solvent
NA = Not analyzed
Note:' Values below detection limit counted as zero for mass balance
89
-------
6.11.2
Material Balance of Selected Parameters
Based on the closure of the gross material balance, a balance of selected analytical parameters
was performed. This was done to qualitatively determine the fate of specific metals and indigenous
oils through the process. Balances of specific organics (VOC and SVOC) could not be performed due
to matrix interferences. The detailed balances could only be done on a qualitative basis because the
distillation step was cancelled. This change made full characterization of the centrates necessary to
quantify materials extracted from the waste. Solvent recovery, if demonstrated, would have otherwise
reduced the centrates to their solvent and indigenous oil fractions.
The total mass of centrate dominates the balances. When this is coupled with the accuracy
limits of the analytical procedures, the computed masses can be exaggerated, suggesting a significant
gain in material. For this reason, the detailed material balances provide only a qualitative estimate of
the fate of the materials.
6.11.2.1 Indigenous Oil
Table 6-13 presents the balance for indigenous oil for both test runs. In Test Run 1, 54.86
pounds of indigenous oil were charged to the system while an apparent 152.27 pounds were
recovered. This results in 278 percent recovery. Despite this imbalance, it is apparent that 98 percent
of the recovered indigenous oil was extracted into the centrate. Of the oil extracted, 85 percent was
removed in the first extraction. The indigenous oil fraction of the centrate is on the order of 0.5
percent, by weight, so that any analytical deviation from true levels (particularly given the precision
of the test procedures in this matrix), will result in exaggerated over- (or under-) quantification.
Test Run 2 exhibited very similar results with respect to oil removal. The apparent material
recovery was greater than in Test Run 1 (462 percent). The analysis suggests that greater than 98
percent of the recovered indigenous oil was extracted into the centrates. Of this, 86 percent was
removed in the first extraction. Both test runs indicate that most of the oil was removed in the first
extraction. This is consistent with conclusions drawn from reviewing the sample characteristics
discussed in Section 6.6.
90
-------
TABLE 6-13. MATERIAL BALANCE ON INDIGENOUS OIL FOR
CARVER-GREENFIELD PROCESS DEMONSTRATION
Indigenous Oil (lbs)
Test Rub I
Test Run 2
Obs)
(lbs)
Materials Charged
Feedstock
54.86
24.21
Beatoaite
0.00
0.00
Total Charged
54.86
24.21
Materials Recovered
Centrate
Extraction A
129.82
94.27
Extraction B
14.99
10.83
Extraction C
5.23
5.12
Scrubber Liquor
0.00
0.18
Final Product
1.87
1.20
Deoiler Residue
0.20
0.09
Final Product Sampling
0.17
0.10
Total Recovered
152.27
111.78
Percentage Recovered
278
462
Note: Values below detection limit counted as zero for mass balance
6.11.2.2 Balance of Selected Metals
Material balances were performed for five metals which were present in significant quantities
(>500 tiglg) in the feedstock: aluminum, barium, calcium, iron, and magnesium. Table 6-14
presents the balance for Test Run 1. Total metal recovery for Test Run 1 ranged from 80.77 percent
for magnesium to 248 percent for aluminum. Extraction B results for aluminum, barium, and iron
were at elevated levels as compared to the first and third extraction. This is believed to contribute to
the apparent excessive recoveries for these metals. If the metals are assumed to be nonexistent in
Extraction B centrate, recoveries improve to 83 percent, 56 percent, and 79 percent, respectively.
This approach to the metals balance suggests that after three extractions, 40 to 100 percent of the
metals remain partitioned to the solids.
91
-------
TABLE 6-14. MASS BALANCE ON METALS FOR TEST RUN 1
Aluminum
Barium
Calcium
Iron
MagoeshHv
:n;>: (g)
(g)
Materials Charged
Feed
1,518.74
425.87
304.09
1,932.35
216.07
Materials Recovered
Centrate
Extraction A
17.20
5.15
0.00
28.55
0.00
Extraction B
2,497.26
654.41
0.00
2,892.25
0.00
Extraction C
56.82
7.83
0.00
56.03
0.00
Condensed Water
0.17
0.17
0.28
0.17
0.07
Condensed Solvent
0.79
0.79
0.00
0.00
0.00
Final Product
996.43
189.01
310.36
1203.61
145.62
Deoiler Residual
106.90
20.28
33.30
129.12
15.62
Final Product Sampling
90.33
17.13
28.13
109.11
13.20
Total Recovered
3,765.88
894.76
372.07
4,418.84
174.51
Percentage Recovered
247.96'"
210.10*"
122.35
228.68"'
80.77
'"Extraction B centrate results seem anomalous when compared to Extractions A and C. If these
metals are assumed to be nonexistent in Centrate B, recoveries improve to 83% (aluminum),
56% (barium), and 75% (iron).
Note: Values below detection limit counted as zero for mass balance
A similar balance for Test Run 2 exhibits similar results with respect to the partitioning of the
metals to the solids and their resistance to extraction. Table 6-15 presents the metals balance for Test
Run 2. The barium result appears low compared to Test Run 1. This anomaly appears to elevate the
recovery of barium. If the feedstock barium concentration is corrected using the Test Run 1 result,
barium recovery improves to 77 percent. These results suggest that 45 to 74 percent of metals remain
partitioned to the solids. The partitioning is summarized as follows:
Percent of Metal Remaining with Solids After Three Extractions
Aluminum
Barium
Calcium
Iron
Magnesium
Test Run 1
66
44
100
62
67
Test Run 2
50
45
66
74
65
92
-------
TABLE 6-15. MASS BALANCE ON METALS FOR TEST RUN 2
Aluminum
Bariran
Cakhna
Iron
Magnesium
(l)
(g>
m
Materials Charged
Feed
1,112.13
87.1 lw
1,177.68
3,136.40
189.35
Materials Recovered
Centra te
Extraction A
15.86
25,94
0.00
41.80
0.00
Extraction B
12.24
20.20
0.00
21.37
0.00
Extraction C
15.44
25.42
0.00
25.42
0.00
Condensed Water
1.10
0.00
0.00
0.00
0.00
Condensed Solvent
0.00
0.00
0.00
0.00
0.00
Final Product
551.44
203.32
770.97
2,334.30
123.44
Deoiler Residual
39.04
14.39
54.58
165.26
8.74
Final Product Sampling
44.08
16.25
61.62
186.58
9.87
Total Recovered
679.19
305.53
887.17
2,774.73
142.05
Percentage Recovered
61.07
350.75
75.33
88.47
75.02
(,iBelieved to be erroneous due to low barium result. If the result for Test Run 1 is substituted
(2,990 jiglg wet weight) and applied to the quantity of feed, charged, the mass of barium charged
increases to 453.3 g, improving recovery to 77%.
Note: Values below detection limit counted as zero for mass balance
93
-------
7.0 QUALITY ASSURANCE/QUALITY CONTROL
The approved QAPjP is described in the Demonstration Plan and associated memoranda. The
overall QA objective was to develop sampling and analytical data of known quality in support of the
demonstration objectives. The QA/QC data were evaluated with respect to the QA objectives defined
in the QAPjP. QA objectives for the liquid sample matrix are presented in Table 7-1, while Table
7-2 presents the objectives for the solid and slurry matrices. Evaluation of the QC data encompassed
several elements:
• Adherence to sample holding time limits before analysis
• Acceptability of blank results (method, field, equipment, TCLP, equipment, and trip
blanks)
• Results of reference standards analyses (reference spikes, laboratory control samples)
relative to acceptance limits
• Analysis of laboratory duplicates relative to established precision limits
• Matrix spike/matrix spike duplicate analysis results within acceptance limits
• Detection limits of various analyses
• Compliance with calibration requirements
• Completeness of analytical reporting
The following sections discuss the analytical methods used, sample holding times, matrix
spikes and spike duplicates, laboratory duplicates, reference standards, blanks, calibration, and
detection limits.
7.1 ANALYTICAL METHODS
The only analytical procedures used in this demonstration which were not EPA-approved were
those for SOW and solvent. Solvent was analyzed using a GC procedure developed by DTC. The
SOW analysis was conducted using a modified ASTM Dean-Stark procedure, provided by DTC.
DTC has used both procedures as process control tests. These methods are described in Appendix C
of this report, as modified and demonstrated for this demonstration. Method development work
94
-------
TABLE 7-1. QA OBJECTIVES FOR
LIQUID SAMPLE MATRIX*
Analytical
- * - - - -- ¦» .
NWQRBVI
Prteim
"''Aeearacy:?-:;.:;.
fywipMnii H
Grwp
' T&rkmctw
IWeraac*
Unto
(WO)
(~JtowafyV
(**
Oil»
Solvent
DTC"
%
50
O
O
NO
90
Petroleum
MCA WW 418.1®
mg/L
45
61 - 147
90
Hydrocarbons
Organic*
Volaliici
SW846/8240"1
Mg/L
30"'
D-234'"
90
Semivolatiles
SW846/8270"1
*g'L
50"'
D-2301"
90
Metals
ICP
SW846/6010"'
mg/L
30
80 • 120
90
TCLP
40 CFR'8
Orgamcs
SW846/8240/8270"'
mg/L
90
Metals
SW846/60101"
mg/L
-------
TABLE 7r2. QA OBJECTIVES FOR SOLID AND SLURRY MATRICES*
MessureBeot
::, precisioa
Accuracy
- Group
ParaneMr
¦ ¦ Rtf«r*nt» . ¦'
Units
ftee6*«fy)
Oili
Solver*
DTC"
%
30
75 - 125
90
SOW"'
ASTM 9S-7Q;
%
Solid IS
95 ¦ 103
90
DTC/HQI
Oil 20
74-118
90
modified procedure'"
Water 20
88 - 117
90
Petroleum
SMEWW5520 D,EW
mg/Kg
30
56 - 130
90
Hydrocarbons
Organic*
Volatile*
SW846/824051
*»g/Kg
30'«
D-234®
90
Semivoiatiles
SW8 46/8270"
ng'Kg
50""
D-230"1
90
Metals
ICP
SW846/60I0"
mg/Kg
30
80 - 120
90
NOTES
<»
GC Method developed by DTC, tee Appendix C.
(2)
Precision and accuracy (relative percent difference) are shown for each of the three component*.
(3)
Solids/Oil/Water (SOW). This is a modified Dean-Stark procedure used by DTC and modified by HydroQuaJ.
See Appendix C.
(4)
Standard Methods, 17th edition, 1989.
(S)
Test Methoda for Evaluating Solid Waste, EPA, 3rd edition, November 1986.
(6)
MS/MSD Analysis encompasses maximum range of all spike compounds.
•
Feedstock, indigenous organics/oil, treated solids, solvent, GAC and solvent slurried materials.
included demonstrating the applicability of the procedures to the matrices encountered in the
demonstration and development of QA/QC criteria.
The only procedural deviation from the Demonstration Plan was associated with the TPH
analysis. A sample preparation step was incorporated to remove free water and produce a non-flowing
solid. Standard Method 5520 D,E was used for oil and slurry matrices. Approximately 20 grams of a
homogenized sample was mixed with the dehydrating agent, followed by soxhlet extraction. The
sample was then analyzed according to EPA Method 418.1, as originally intended.
Minor modifications were made to the GC procedure for solvent analysis and to the SOW
procedure to account for the presence of very fine solids in the waste feed. A filtration step was
added to the GC procedure to prevent these particles from blinding the column. Similarly, a
96
-------
centrifuging step prior to vacuum filtration was added to the SOW procedure to enhance the filtration
rate and reduce the required analysis time.
During the laboratory QA audit, a concern was raised regarding metals recovery of the
digestion procedure (Method 6019, acid digestion) for matrices containing high levels of oil. It was
noted that the aqueous metal spikes recovery, even if satisfactory, might not adequately indicate metal
recovery in an oil matrix. To check this, three metals (barium, iron, and aluminum) were added as
organometallic spikes to selected samples of centrate and solvent. Organometallic spike recoveries
ranged from 99 to 117 percent for the centrate samples and 101 to 112 percent for the solvent
samples. These results complied with the QA objectives for metals (Tables 7-1 and 7-2) and
suggested that sample digestion by Method 6019 was satisfactory.
7.2 SAMPLE HOLDING TIMES
Tables 7-3, 7-4, and 7-5 list the dates of sample collection, preparation, and analysis for the
blank run and Test Runs 1 and 2, respectively. All holding times for metals and VOC analyses were
met. For the SVOC analyses, all holding times were met with the exception of the feedstock samples
of Test Run 1 which were analyzed one day outside of the targeted maximum holding time. Holding
times for BOD and pH analyses in Test Runs 1 and 2 and for TSS analysis in Test Run 2 were not
met. Holding times for other conventional parameters were met. Targeted holding times for the
TPH analyses were not met because of difficulties with the matrices and changes in the methodology
for sample preparation.
Considering the volume of analytical work, most holding times were met. Other than the
TPH analyses, only a very small fraction of samples were analyzed outside their respective holding
times. The primary reason for holding time difficulties for the TPH analyses was that the laboratory
procedure planned in the QAPjP was changed as a result of the laboratory audit, causing the analysis
to be delayed. Matrix difficulties with several of the high solvent samples also contributed to these
delays.
97
-------
TABLE 7-3. DATES OF SAMPLE COLLECTION, PREPARATION,
AND ANALYSIS - BLANK RUN
¦ ¦ T::T;:r-;;;:D:V ^
Preparation/
Holding
Coflactm
Extraction
Aaaferir
Aaafcrt* -
Time
Data
Date
Data
Waste Feed
VOC
14 dayt
8/4/91
-
8/19/91
n
SVOC (BateVNeutril Ext.)
7 dayt
8/4/91
8/7/91
8/13/91
y
SVOC (Acid Ext.)
7 dayi
8/4/91
8/7/91
8/13/91
y
Meult
6 month!
8/4/91
-
8/15-9/3/91
y
TPH
28 dayt
8/4/91
-
9/9/91
n
Freth Solvent
Meult
6 months
8/1/91
-
8/15-9/3/91
y
Centrile
Meuli
6 months
8/4/91
-
8/15-9/30/91
y
Water Condensate
pH
Immediate
8/4/91
-
8/6/91
n
Toul Alkalinity
14 days
8/4/91
-
8/13/91
y
Total Acidity
14 days
8/4/91
-
8/14/91
y
BOD,
48 hours
8/4/91
-
8/7/91
n
COD
28 days
8/4/91
-
8/9-8/12791
y
NH,-N
28 dayt
8/4/91
-
8/13/91
y
TKN
28 dayt
8/4/91
-
8/15/91
y
TPH
7 dayt
8/4/91
-
9/9/91
n
TSS
7 dayt
8/4/91
-
8/10/91
y
Sulfate
7 dayt
8/4/91
-
V16/91
n
Meuli
6 months
3/4/91
-
8/14-8/21/91
y
VOC
14 days
8/4/91
-
8/17/91
y
SVOC (Acid Ext.)
7 days
8/4/91
8/8/91
8/13/91
y
SVOC fBase/Neutnl)
7 days
8/4/91
8/8/91
8/13/91
y
Solvent Condensate
TPH
28 days
8/4/91
-
12/16/91
n
Meuli
6 months
8/4/91
-
8/15-9/3/91
y
Treated Solids
SVOC (BaaeV Neutral)
7 dayt
8/5/91
8/8/91
8/14/91
y
SVOC
(Acid Ext.)
7 dayt
8/5/91
8/8/91
8/14/91
y
Meult
6 months
8/5/91
-
8/15-9/3/91
y
TPH
28 davt
8/5'91
9/9/91
n
Trip Blank
VOC
14 days
. 8/191
••
8/13/91
y
Equipment Blank
TPH
28 dayt
8/5/91
-
8/13/91
y
voc
14 days
S'5/91
-
8/13/91
y
SVOC (Base/Neutral Ext.)
7 days
8/5/91
8/8/91
8/13/91
y
SVOC (Acid Exi.)
7 dayt
8/5/91
8/8/91
8/13/91
y
98
-------
TABLE 7-4, DATES OF SAMPLE COLLECTION,
PREPARATION, AND ANALYSIS - TEST RUN 1
- Prep«r*ti-
Wade Feed
voc
• Samples 1-6
14 daya
8/5/91
-
8/18/91
i
svoc
(Ba»e/Neuu»l Ext.)
- Samplea 1-4
7 daya
8/5/91
3/13/91
3/17/91
n
- Samplea 5-6
7 days
8/5/91
8/13/91
8/18/91
n
svoc
(Acid Ext.)
• Simplei 1-4
7 dayi
8/5/91
8/13/91
8/17/91
n
- Samplea S-6
7 daya
8/5/91
8/13/91
8/18/91
n
Meula
6 months
8/5/91
-
8/1J-9/3/91
y
TPH
28 daya
8/5/91
•
9/11/91
n
Central*
TPH
• Extric. A
13 daya
8/5'91
-•
11/7/91
a
• Extric. B
23 days
8/6/91
--
'.1/7/91
tx
- Extrac. C
28 days
8/9/91
..
11/7/91
n
Meula
• Exilic, A
6 months
8/5/91
-
8/23-9/30/91
y
• Extrac. B
6 months
8/6/91
-
8/28/91
y
- Extrac. C
6 months
8/9/91
-
8/28/91
y
Water Condensate
pH
Immediate
8/9/91
-
8/12/91
n
Tout Alkalinity
14 days
8/9/91
-
8/19/91
y
Total Acidity
14 days
8/9/91
-
8/14/91
y
BOD,
48 hours
8/9/91
-
8/21/91
n
COD
- Cond. 1
28 days
8/9/9!
--
8/12/91
y
- Cond. 2
28 days
8/9/91
--
8/12/91
y
NH,-N
28 days
8/9/91
--
8/13/91
y
TKN
28 daya .
8/9/91
-
8/15/91
y
TPH
7 dayi
8/9/91
_
9/9/91
*
TSS
7 daya
8/9/91
-
8/16/91
y
Sulfate
7 days
8/9/91
-
8/16/91
y
Meula
6 months
8/9'91
••
8/19/91
y
VOC
14 day*
8/9/91
--
8/17/91
y
SVOC
(Acid Ext.)
7 Jay*
8/9/91
8-13-91
8/16/91
y
SVOC
(Bate/Neutral Ext.)
7 days
3/9/91
< 13.91
S-M6/91
¥
99
-------
TABLE 7-4. DATES OF SAMPLE COLLECTION,
PREPARATION, AND ANALYSIS - TEST RUN 1 (CONTINUED)
SftspW
Ajiajyte
Hofcfaf
Tin*
CoWMtfan
Dat*
Preparation/
Extrteticn
D*t»
Aaatysb
Dat*
Hefc&ng Urn*
Mtl
Solvent Condensate
TPH
28 dayi
8/9/91
-
11/21/91
n
Meuli
6 month!
8/9/91
-
8/28/91
y
Treated Solidi
SVOC
(Baac/NeutrtJ Ext.)
7 dayi
8/9/91
8/15/91
8/27/91
y
svoc
(Acid Exl.)
7 dayi
8/9/91
8/15/91
8/27/91
y
Melait
6 monihi
8/9/91
-
8/28/91
y
TPH
28 days
8/9/91
-
10/16/91
n
Thp Blank
VOC
14 days
8/9/91
-
8/16/91
y
Field Blank
TPH
28 dayi
8/9/91
-
9/9/91
n
VOC
14 dayi
8/9/91
-
8/16/91
y
svoc
CBaie/Neutnl Ext.)
7 dayi
8/9/91
8/13/91
8/17/91
y
svoc
(Acid Ext.)
7 davi
8/9/91
8/13/91
8/17/91
y
Equipment Blank
TPH
28 davi
8/9/91
-
9/9/91
n
VOC
14 davi
8/9/91
-
8/19/91
y
svoc
(Baie/Neutral Ext.)
7 davi
8/9/91
8/13/91
8/14/91
y
SVOC
(Acid Ext.)
7 davi
OO
8/13/91
8/14/91
y
100
-------
TABLE 7-5. DATES OF SAMPLE COLLECTION,
PREPARATION, AND ANALYSIS • TEST RUN 2
fntwiW
$**XU
tfaiding
CoUectJoa
Ertraetfa*
Auijrafe -
' Aoatyf* -
Taw
Date
Date
Dai*
ishi
Watt Feed
voc
-Sample 1
14 dayi
8/12/91
-
8/24/91
y
•Simple! 2-6
14 dayi
8/12/91
-
8/25/91
y
SVOC
(Baw/Neulral Ext.)
7 dayt
8/12/91
8/15/91
8/22/91
y
SVOC
(Acid Ext.)
7 dayi
8/12/91
8/15/91
8/22/91
Metala
6 monthi
8/12/91
-
8/23-9/30/91
y
TPH
28 davi
8/12/91
-
9/11/91
n
Centrite
TPH
- Extrac. A
28 dayi
8/12-8/15/91
-
11/14-12/5/91
n
- Extrac. B
28 dayi
8/13/91
-
11/14/91
n
¦ Extnc. C
28 davi
8/15/91
-
11/14-12/5/91
n
Metali
- Extnc. A
6 months
8/12-8/15/91
-
9/4-26/91
y
- Extrac. B
6 months
8/13/91
-
9/4-26/91
y
- Extrac. C
6 monihi
8/15/91
-
9/4-26/91
y
Water Condeniate
PH
Immediate
8/15/91
-
8/19/91
n
Toul Alkalinity
14 day!
8/15/91
-
8/27/91
y
Toul Acidity
14 day!
8/15/91
8/27/91
y
BOD,
48 houn
8/15/91
-
8/21-29/91
a
COD
- Cond. 1
28 dayi
8/15/91
-
8/22/91
y
- Cond. 2
28 dayt
8/15/91
-
8/22/91
y
- Cond. 3
28 day!
8/15/91
-
9/9/91
y
NH,-N
28 day!
8/15/91
-
8/20/91
y
TKN
28 dayi
8/15/91
-
8/23/91
y
TPH
7 dayi
8/15/91
- •
9/9/91
n
TSS
7 dayi
8/15/91
-
9/5/91
n
Sulfate
7 dayi
8/15/91
-
8/27/91
a
Metali
6 monthi
8/15/91
-
9-4-26/91
y
VOC
14 dayi
8/15/91
-
9/27-28/91
n
SVOC
(Acid Ext.)
SVOC
7 davi
3/15/91
-
9/5/91
n
(Baie/Neutril Ext.)
Solvent Condensate
TPH
2S Jayi
8/15/91
-
11/21/91
n
Meult
6 monih!
8/15/91
-
9'6/91
y
101
-------
TABLE 7-5. DATES OF SAMPLE COLLECTION,
PREPARATION, AND ANALYSIS ¦ TEST RUN 2 (CONTINUED)
asssssa
Preparation^; *
Roldhg T&m
Stuapiaf
MS**
Collection
Extrvtias
Auijrsta
Vfc*
Aaaiytt
-
Dat#
Datt
Dal*
Treated Solid »
SVOC
(B»k< Neutrtl Ext.)
7 dayt
8/15/91
8/26/91
9/9/91
n
SVOC
(Acid Ea.)
7 day*
1/15/91
8/26/91
9/9/91
n
Meuli
6 monihi
8/15/91
-
9/4-26/91
y
TPH
28 dayi
8/15/91
-
10/16/91
n
Trip Blank
voc
14 diyi
8/15/91
-
8/28/91
y
Field Blank
TPH
Zi days
8/15'91
-
9'9/91
¥
VOC
14 day»
8/15/91
-
8/28/91
y
SVOC
(B»a«/Neulrtl Ext )
7 dayt
8/15/91
8/22/91
9/4/91
y
SVOC
/Acid Ext.)
7 dayt
8/15/91
8/22/91
9/4/91
y
Equipment Blank
TPH
28 dayt
8/15/91
-
9/9/91
V
VOC
14 d*y»
8/15/91
-
8/28/91
y
SVOC
(Baje'Neutnl Ext.)
7 diyi
8/15/91
8/22/91
9/4/91
y
SVOC
(Acid Ext.)
7 days
8/15/91
8/22/91
9/4/91
y
102
-------
7 J MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERIES
Matrix spike and matrix spike duplicates were analyzed for VOCs, SVOCs, metals, TPH, and
conventional parameters. Results of these analyses are presented in Appendix D.
All matrix spike recoveries (50 of 50) for VOC analyses were within QC limits. All surrogate
spike recoveries (189 of 189) were also within QC limits. For SVOC analysis, 99 of 110 spike
recoveries were within precision limits. Similarly, 242 of 270 matrix spikes for metals analysis, 9 of
15 for TPH analysis, and 10 of 12 for conventional parameters were within QC limits. The relatively
poor spike recovery for TPH was primarily due to the nature of the samples. Samples containing
high solvent/oil levels such as the centrate and feedstock could not be sufficiently spiked, resulting in
poor spike recovery. Table 7-6 summarizes completeness for matrix spike and matrix spike duplicate
results. Sample analysis results for which the spikes were outside QC limits were considered
estimates and were flagged accordingly.
7.4 LABORATORY DUPLICATES
Results of duplicate analyses are presented in Appendix D. At least one sample of each
sample matrix (waste feed, slurry, centrate, centrifuge cake, treated solids, condensed water, vent gas
[GAC], and condensed solvent) from Test Runs 1 and 2 was analyzed in duplicate. The precision
objectives for different analytes and sample matrices are summarized in Tables 7-1 and 7-2.
All duplicate results for VOC analysis (25 of 25) and TPH analysis (11 of 11) were within
QC precision limits. For SVOC analyses, 42 out of 55 duplicates were within precision limits.
Similarly, 236 out of 241 duplicates for metals analysis, 13 out of 15 duplicates for conventional
parameters, 23 out of 25 duplicates for solvent analysis, and 17 out of 18 duplicates for SOW analysis
were within precision limits. Data outside of the QC limits were flagged as such. Table 7-6
summarizes the duplicate results and associated completeness.
103
-------
TABLE 7-6. SUMMARY OF QA/QC RESULTS FOR MATRIX
SPIKE, DUPLICATE ANALYSIS, AND REFERENCE STANDARDS
MSMSD
Dupikflit
Mv«M»Sl«dinl
"
PvrmKteiv •
Cawjrfy*'
Cmplri«ten^ .
Awityvrf"
CawiV
CwnpteaKW**
P
Cow
Volatile Organic!
so
50
100
25
25
100
67
67
100
Scmivolalik Organic*
no
99
90
55
42
76
55
55
100
Mclal»
27(1
242
9(1
241
236
9J
320
298
93
Tuul Petroleum llydiocafhoii
15
9
60
II
II
100
II
II
100
Solvent
-
-
-
25
21
92
31
31
100
SOW
-
IS
17
94
19
19
100
ClMIVeillMMIill FafJiih-'UTS
12
10
Si
IS
IJ
87
41
41
100
NOTES
"'Number of uniplcs aiuly/ed for particular (JA parameter!
"'Number of analyse:) complying with the relevant QC criteria
"'I'en tillage of QA results complying willi llic it
hlive QC criteria
-------
7.5
REFERENCE STANDARDS
Reference standards recoveries for each batch of samples indicate the accuracy for that
particular batch or matrix. Acceptable QC limits for accuracy for different analyses and sample
matrices are given in Tables 7-1 and 7-2. QC limits for accuracy were checked using reference spike
recoveries for VOC and SVOC analyses. All reference spike recoveries for VOC analysis (67 of 67)
and SVOC analysis (55 of 55) were within QC limits. Laboratory control samples (LCS) were run for
metals, TPH, solvent, SOW, and conventional parameters to check QC accuracy limits. All LCSs for
TPH (11 of 11), solvent (31 of 31), and conventional parameters (41 of 41) were within QC
acceptance limits. Similarly, 298 out of 320 LCSs for metal analysis and 19 out of 19 LCSs for
SOW analysis were within control limits. Table 7-6 summarizes QC results for the reference
standards.
7.6 FIELD AND EQUIPMENT BLANKS
Field and equipment blanks were analyzed for VOCs, SVOCs, solvent, and TPH in each test
run. A trip blank was also analyzed for VOCs in each test run. Equipment blank results did not
indicate any contamination of VOCs, SVOCs, solvent, or TPH.
Chloroform was detected in the Test Run 2 trip blank. Trace levels of methylene chloride
and chloroform were also detected in the Test Run 2 field blanks. No VOCs were detected in the
Test Run 1 field blank. SVOCs were not detected in any field blank. TPH analysis showed trace
levels in the field blanks for Test Runs 1 and 2, and trace solvent levels were noted in the Test Run 2
field blank.
7.7 METHOD BLANKS
The method blanks for VOCs, SVOCs, and metal analyses were also non-detectable. At least
one blank was analyzed for solvent and SOW each day. Trace solvent was detected in two blanks;
similarly, trace levels of indigenous oil were detected in three blanks run for SOW analysis.
105
-------
Three method blanks for TPH analysis indicated trace level contamination. This was not
considered significant since the TPH levels in the associated samples were high. Similarly, traces of
ammonia were detected in two method blanks; the associated samples were all measured at less than
detection for ammonia. All other conventional analyte method blanks showed no contamination.
7.8 LABORATORY INSTRUMENT CALIBRATION
The laboratory's instrument calibration requirements for this project are stated in the
Demonstration Plan (PRC, 1991). All initial and continuing calibration verifications were done. All
data were analyzed under compliant calibrations. All continuing calibration and tuning criteria were
met.
7.9 DETECTION LIMITS
Detection limits for analytes varied depending on sample matrices. These are summarized in
Tables 7-7, 7-8, 7-9, and 7-10 for metals, VOC, SVOC (acid extractable), and SVOC (base/neutral
extractable), respectively.
The presence of Isopar-L in samples caused matrix interferences for the organics analyses,
requiring dilution in some samples and elevating the detection limits. Matrix interferences in water
condensate samples required dilutions which raised reported detection limits 5 to SO times above the
method practical quantitation limits (PQLs) for VOC analysis. Similarly, matrix interferences in
the feedstock samples for both test runs caused a need for dilutions. This raised reported detection
limits 250 times above method PQLs for VOCs.
Matrix interferences caused by Isopar-L in SVOC analyses required dilutions in treated solids
samples of the blank run and Test Run 2, feedstock samples of Test Runs 1 and 2, and water
condensate samples. This raised reported detection limits 10 to 300 times above the method PQLs for
these samples.
106
-------
TABLE 7-7. RANGE OF DETECTION LIMITS FOR METALS
o
—i
Feedstock :
Um/g) (wrt yrt)
Ffaul So&b Product
tag/g)(wetwtf
oa»
dVeik, Central, Cukbted)
0
W«tw
. CaadMMale .
• V - •
Meiab
fQL
MDL Range
PQL
MDt, Kange
MBL lUngft
kjl
Aluminum
0.100
100
0 100
10 0
0.100
100
o too
010-10.0
Aniimoiiy
0050
5 0
0.050
5 0
0.050
5 0
0 050
0.05-0.50
Arsenic
0.500
50.0
0.500
50.0
0.500
50 0
0.500
0 50-50 0
Barium
0 0050
0 5
0.0050
0 5
0 0050
,0 5
0.0050
0 0050 0 50
ikiylliuin
o.ooso
1)5
0.0050
1)5
0 0050
0 5
0 005
0 0050 0 50
Buitui
0 200
20 0
0 200
20.0
0 200
20.0
0.200
0 200-20 0
Cadmium *
0.0050
0.5
0.0050
0.5
0 0050
0.5
0 0050
0 005-0 50
Calcium
0 500
50 0
0.500
50.0
0.500
50 0
0 500
0 50 50 0
I'liroiiiiimi
0 010
1.0
0.010
10
0 010
1 0
0 010
0 010 1 0
Coltall
0 050
5 0
0 050
5 0
0.050
5 0
0.050
0 05 5 0
Cupper
0.010
l.u
0 010
1 0
0 010
1 0
0010
0.01-1 0
lion
0 050
5 0
0 050
5.0
0 050
5 0
0 050
0.05 5 0
Lead
0 050
5 0
0.050
5 0
0 050
5 0
0.050
005 5 0
Mjgitcsnxii
0.500
50 0
0.500
50 0
0.500
50 0
0 500
0 50-500
Manganese
0.005
0.5
0.005
0 5
0 005
0.5
0.0050
0.00S-0.5
Molybdenum
0 050
5 0
0050
5.0
0.050
5 0
0 050
0 05-5.0
Nickel
0 020
2 0
0 020
2.0
0 020
2 0
0 020
0 02 2 0
Potassium
0.500
50 0
0.500
50 0
0 500
50 0
0 500
0.5-50.0
Selenium
0.500
50,0
0 500
50 0
0.500
50.0
0 500
0.5 50 00
Strontium
0.500
500
0 500
50 0
0.500
$00
0 500
0 5 50 0
Suiiium
0 500
500
0.500
50 0
0.500
50 0
0.500
0 5 50.0
Thallium
0 050
5 0
0.050
5.0
0050
5 0
0 050
0 05 5 0
Vanatliuiu
0 050
5 0
0.050
5 0
0 050
5 0
0,050
0 05-5 0
Zinc
0.010
10
0.010
10
0.010
10
0010
0 01 1.0
-------
TABLE 7-8. RANGE OF DETECTION LIMITS FOR VOLATILE ORGANICS
'o
voc*
Feedstock
G«Ag>
Water .
CmwfHitttg
tflt/L}
PQL
MDL Range
PQL
MDL Rufc
Chlorome thane
5
1,250
5
250
Bromomeihane
5
1.250
5
250
Vinyl Chloride
5
1,250
5
250
Chlorocthane
S
1,250.
5
250
Methylene Chloride
S
1,250
5
250
Acetone
20
5,000
20
1,000
Ctrbon Disulfide
10
2,500
10
500
T nchlarofluoromeihine
5
1,250
5
250
Vinyl Aceuie
10
2,500
10
500
I.l-Diehloroethane
5
1,250
5
250
irana-l ,2-Dichloroethene
5
1,250
5
250
:i»-l ,2-Dichloroeihene
5
1.250'
5
250
Chloroform
5
1.250
5
250
2-Buunone
10
2,500
10
500
1,2-DichIoroe thane
5
1,250
5
250
1.1.1 -T richloroethane
5
1.250
5
250
Carbon Tetrachloride
5
1,250
5
250
Bromodichloro methane
5
1.250
5
250
1,2-Dichloropropane
5
1.250
5
250
1,3-Diehloropropene (Trans)
5
1.250
5 •
250
Trichloroethene
5
1.250
5
250
Dibromochloromethane
5
1,250
5
250 "
1,1,2-Trichloroe thane
5
1,250
5
250
Benzene
5
1,250
5
250
1,3-Dichloropropene(Cis)
5
1.250
5
250
Bromoform
5
1.250
5
250
4-Methyl-2-penun
-------
TABLE 7 9. R VN(IE OF DKTEC TION LIMITS FOR SEMI VOLATILE OKGANICS ACID
EXTRACTABLES
Watfr
feedstock
Ha»l Solids Product
Cood canto
0ini«:iltyl|>liciM>t
330
100,000
330
660 3,300
10
10 500
2,4 Diililoioplicito]
330
100,000
330
660 3,300
10
10 500
4 CJiiorn-3 mciliyJjthcjtol
330
100,000
330
660 3,300
10
10 500
2,4.6-TiicIiIaruplicnol
330
100,000
330
660 3,300
10
10 500
2.4 Diiiiiiopliciiid
660
200,000
660
1,320 6.600
20
20 1,000
4Niiiuj»ltc»io|
660
200,000
660
1,320 6,600
20
20 1,000
2 Miihyl 4,6 tlmuiopluiiol
660
200,000
660
1,320 6,600
20
20 1,000
IViiI.k JitiMophciiol
660
200,000
660
1,320 6,600
20
20 1,000
2-Mciliyl|*Iicno|
330
100,000
330
660 3,300
10
10 500
4-Mclliyl|iliciu>I
330
100,000
330
660 3,300
10
10 500
Bcn/oic Acid
1650
500,000
1650
3,300 16,500
50
50 2,500
2,4,!>Tiiihlufi>j)hcm>i
330
100,000
330
660-3,300
10
10-500
-------
TABLE 7-10. RANGE OE DETECTION LIMITS FOR SEMI VOLATILE ORGAN1CS-
BASE/NEUTRAL EXTRACTABLES
Feedstock
0^/Vk) (w«t wt)
' Final SoM* FwAict
Otg/VftHwM wt)
Co
Wirttr
Kkwttto
$VOC
: pQL
MDL Range
PQL
MDL Range
POL
MDL tUag»
N - N iiiosodimcihyUmine
16$
50,000
165
330-1,650
5
5-250
tiis(2-LliK>roelhyl) cihcr
165
50,000
165
330 1,650
5
5 250
1 ..l-Dichlorobcn/ejie
I6S
50,000
165
330 1,650
5
5 250
1,4-Dichloroi>t:ti/cfi£
I6S
50,000
165
330 1,650
5
5 250
I.J DicMnrohcii/cuc
165
50,000
165
330 1,650
5
5-250
Uis(2-chloroisnpropy() elite r
165
50,000
165
330 1,650
5
5 250
N Niliosn Di li propylamine
165
50,(MX)
165
330 1.650
5
5-250
llcxachloiticlliaiic
165
5(1.000
165
330 1,650
5
5 250
NiIimIicii/cdc
165
50,000
165
330 1,650
5
5 250
l.sojiliojonc
165
50,000
165
330 1,650
5
5 250
Ui.s(-2-cliloi«>clhoxy)mclliaue
165
50,000
165
330 1,650
5
5 250
i .2.4 TiiLhloioben/cnc
165
50,000
165
330-1,650
5
5-250
Naphthalene
165
50,000
165
330 1,650
5
5 250
llcxachlorobuladicne
165
50,(XX)
165
330-1,650
5
5-250
llexuchloroeyelopeiiladiene
165
50,000
165
330 1,650
5
5-250
2-ChloronaphiltAleiie
165
50,000
165
330 1,650
5
5-250
Dimethyl phlhalule
165
50.000
165
330-1,650
5
5-250
Acenaphlhyleiie
165
50,000
165
330 1,650
5-250
Acenaphihene
165
50,000
165
330-1,650
5
5-250
2,4 Diiiitrololuene
165
50,000
165
330 1.650
5
5-250
2,6- Diiiitrololuene
165
50,000
165
330-1,650
5
5 250
-------
TABLE 7-10. RANGE OE DETECTION LIMITS FOR SEMIVOLATILE ORGANICS-
BASE/NEIJTRAL EXTRACTABLES (CONTINUED)
W#tfr
*
F««d&(ocli
Final Solids Product
Coadanule
Ojg/kg> (wet w()
WU
svoc
POL
MDL Range
FQL
MDL Range
PQL
MDL Rftnge
Diethyl phihalatc
165
50,000
165
J JO 1,650
5
5-250
4-ChIoroj>hs:nyi phenyl ether
165
50,000
165
330 I 650
5
5 250
Fliimciic
165
50,000
165
J30 1,650
5
5 250
1 2 DipJicnylhyilia/Hie
165
50,000
165
J JO 1,650
5
5 250
NNiUoioJij)licnyIjniiuc
165
50,000
165
J JO 1,650
5
5 250
4 UitMnophcnyl phcaylclhcr
165
50,000
165
J JO 1,650
5
5 250
Hcxaclilitmhca/ciic
165
50.0(H)
lf.5
JJO 1,650
5
5 250
I'lunuiiiiiiciic
165
50,000
165
J JO 1,650
5
5-250
Aiilhuccnc
165
50,000
165
JJO 1,650
5
5 250
Di II luilyl phlliablc
165
50.000
165
JJO 1,650
5
5 250
Bcii/iiliiic
1,650
500,(K)0
1,650
3,300 16,500
50
50 2500
Miiurunlhcnc
165
50,000
165
JJO 1,650
5
5-250
Py teiic
165
50,000
165
JJO 1,650
5
5-250
Butyl l»cii/.yl jthlhalaie
165
50,000
165
J JO-1,650
5
5-250
JJ'DivhlurobcuzuJme
165
50,000
165
JJO 1.650
5
5 250
Ek i i£o (a) a i iih r a c c nc
165
50,000
165
J JO-1,650
5
5 250
Bi»(2 clliyihcxyOiihthalalc
165
50.0M
165
JJO 1,650
5
5-250
Chrysciic
16$
50,000
165
JJO 1,650
5
5-250
D» H-otlyl phthalatc
165
50,000
165
3 JO 1,650
5
5 250
Beii/.i>(b)lluoraiuhcnc
165
50,000
165
3J0 1,650
5
5-250
Bcii/u(k)(1ii4>ian(hciic
165
50,000
165
JJO 1,650
5
5 250
-------
TABLE 7-10.
RANGE OK DETECTION LIMITS FOR SEMI VOLATILE ORCANICS
BASE/NEUTRAL EXTRACTABLES (CONTINUED)
to
I'eedtlock
KuuJ Solid* Product
'' CoodatutMe
(jtg (wet wt)
btg/lt«) (wet wl)
' "
*/u
$VOC
1"0L
MDL Runge
fQi-
: MDL Range
PQL
MDL fUkage
Bcn/o(a)pyrcnc
165
50,000
165
330-1,650
5
5 250
Jiidcn«i(!.2,3 ir4J)|»crylv'iw
I6S
50,000
165
330 1,650
s
5 250
Ucn/yl Akohol
660
200,0
660
1,320 6,600
20
20-1.000
A < hl
-------
7.10 QUALITY ASSURANCE CONCLUSIONS
Overall, the QA objectives for the C-G SITE demonstration were met. Some data required
qualifications, as indicated by associated QC measurements; however, most of the data met QA/QC
acceptance limits and are appropriate for use. The demonstration data discussed in this report and the
AAR (EPA, 1992), are sufficiently documented and of known quality.
113
-------
8.0 COST OF DEMONSTRATION
The cost (rounded to the nearest $100) of conducting the C-G Process demonstration was
approximately $872,400. This cost includes site characterization, collection and transporting the
drilling mud waste to the Edison facility, demonstration planning, demonstration field work, chemical
analyses, and report preparation. EPA costs for labor and travel are not included in this cost
breakdown.
8.1 EPA SITE CONTRACTOR COSTS
Each SITE demonstration consists of two phases. Phase I is for planning, and Phase II is for
the actual demonstration. Activities during each phase and their associated costs are presented below.
Phase I costs are actual costs incurred before the demonstration; Phase II costs include actual costs
plus estimates for labor to complete the TER and AAR.
8.1.1 Phase I: Planning
Phase I activities included the following:
• Site sampling and treatability testing
• Sampling and analysis plan development
• Demonstration Plan development
• Site subcontractor procurement
Costs for Phase I are summarized below by cost category:
114
-------
Labor $ 85,300
Equipment and supplies 2,200
Travel 4.700
TOTAL $ 92,200
8.1.2 Phase II: Demonstration
Phase II activities included the following:
• Site preparation, mobilization, and demobilization
• Waste handling and transportation
• Sample collection and field oversight
• Chemical analysis (field and off-site)
• Report preparation
• Demonstration waste disposal
Costa for Phase II are summarized below by cost category:
Labor $751,000
Equipment and supplies 8,200
Travel 9,000
Waste disposal 12.000
TOTAL $780,200
115
-------
REFERENCES
American Society for Testing and Materials (ASTM), 1991. Methods Published Annually by
the American Society of Testing and Materials.
PRC Environmental Management, Inc. (PRC), 1991. Demonstration Plan for the Carver-
Greenfield SITE Demonstration. Prepared by the PRC SITE Team for the Superftind
Innovative Technology Evaluation Program.
United States Environmental Protection Agency (EPA), 1979. Methods for the Chemical
Analysis of Water and Wastes, EPA-600/4-79-020, Revised March 1983,
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio, U.S.
Environmental Protection Agency (EPA), and subsequent EPA-600/4 Technical
Additions.
United States Environmental Protection Agency (EPA), 1986. Test Methods for Evaluating
Solid Waste, Volumes IA-IC and subsequent revisions: Laboratory Manual
Physical/Chemical Methods; and Volume II: Field Manual, Physical/Chemical
Methods, SW-846, Third Edition, Office of Solid Waste, Document Control No.
955-001-00000-1.
United States Environmental Protection Agency (EPA), 1992. Applications Analysis Report -
Dehydro-Tech Corporation - The Carver Greenfield Process. Prepared by the PRC
SITE Team for the Superfund Innovative Technology Evaluation Program,
EPA/540/XX-92/XXXX (to be published).
116
-------
LIST OF APPENDICES
A. MONITORING DATA
B. SUMMARY OF ANALYTICAL RESULTS
C. ANALYTICAL PROCEDURES FOR SOW AND SOLVENT
D. QUALITY CONTROL/QUALITY ASSURANCE DATA
E. EQUIPMENT CALIBRATION DOCUMENTATION
-------
APPENDIX A
DEMONSTRATION MONITORING DATA
• Blank Runs
• Test Run 1
• Test Run 2
-------
OPERATING CONDITIONS LOG SHEET
CARVER-GREENFIELD SITE DEMONSTRATION
Date:
Test Run:
8/4/91
Blank Run
Note: Only 1 extraction was performed for the Blank Run
Extraction Number
1st
2nd
3rd
Location
Notation
Parameter
1.
3_ -± 2_ 3_ X •
2_
1. .
A2
FI-1
Flow (Ibs/min)
664
665
675
PI-3
TI-1
Pressure (psig)
Temperature (°F)
Time
ATM
213
1137
ATM
212
1233
ATM
217
1320
A3
PI-4
Pressure (psig)
Time
A5
TI-3
Temperature (°F)
Time
217
1137
217
1233
206
1320
A6
PI-7
TI-4
Pressure (inches Hg)
Temperature (°F)
Time
-22
199
1137
-22
203
1233
-22
196
1320
A7
TI-5
Temperature (°F)
Time
103
1137
105
1233
109
1320
A-1
-------
OrnRAiirsG CuinDITiuinS Luu SHum
CARVER-GREENFIELD SITE DEMONSTRATION
(Continued)
Date:
Test Run:
8/4/91
Blank Run
Extraction Number
1st
2nd 3rd
Location
Notation
Parameter
X
JL 1
JL
X JL X X J_ _L
A10
TI-6
Temperature (°F)
Time
184
1454
179
1550
179
1717
— — —
A12
TC-1
Temperature (°F)
Time
396
1454
394
1350
394
1753
— — — —
A13
Till
Temperature (°F)
Time
206
1454
186
1550
182
1711
— — —
A14
T-12
TC4
Temperature (°F)
Time
195
1454
194
1550
204
1711
A15
TI-13
TC2
Temperature (°F)
Time
198
1454
188
1550
196
1711
A16
PI-15
FI 4
Pressure (psig)
Flow (psig)
Time
0.5
0.5
1454
0.58
0.57
1550
0.67
0.65
1711
— — — — —
A17 TI-14 Temperature (°F) 218 238 237
Time 1454 1550 1711
-------
OrfcRA'l iinG CuinDITiuinS Luu SHtsci
CARVER-GREENFIELD SITE DEMONSTRATION
(Continued)
Date: 8/4/91
Test Run: Blank Run
Extraction Number
1st 2nd 3rd
Location Notation Parameter 1 2 3 1 2 3 1 2 3
A18 Tl-16 Temperature (°F) 129 192 128 _
Time 1454 1550 1711
A19 TI-17 Temperature (°F) 188 192 183
Time 1454 1550 1711
-------
OPERATING CONDITIONS LOG SHEET
CARVER-GREENFIELD SITE DEMONSTRATION
Date:
Test Run:
8/5/91 to 8/8/91
#1
Extraction Number
1st
2nd
3rd
Location
Notation
Parameter
1
2
3
1
2 3
1
2
3
A2
FI-1
Flow (Ibs/min)
650
535
551
569
560
588
594
592
PI-3
Pressure (psig)
ATM
ATM
ATM
ATM
ATM
ATM
ATM
ATM
TI-1
Temperature (°F)
191
206
207
151
156
153
153
153
Time
1200
1305
1330
1435
1443
1050
1100
1106
A3 PI-4 Pressure (psig) 25 30 30 0 0_ 0 0 0
Time 1220 1305 1330 1435 1443 1050 1100 1106
A 5
TI-3
Temperature (°F)
Time
207
1200
210
1305
210
1330
210
1435
173
1443
194
1050
166
1100
155
1106
A6
PI-7
TI-4
Pressure (inches Hg)
Temperature (°F)
Time
-23
196
1220
-22
199
1305
-23
202
1330
ATM
93
1435
ATM
95
1443
ATM
99
1050
ATM
101
1100
ATM
123
1106
A7
TI-5
Temperature (°F)
Time
94
1200
101
1305
102
1330
94
1435
95
1443
97
1050
97
1100
96
1106
A-4
-------
ur ER/\ i iNG cuWDI i .uNS i>vju S111 :i^T
CARVER-GREENFIELD SITE DEMONSTRATION
(Continued)
Date:
Test Run:
8/5/91 to 8/8/91
#1
Extraction Number
1st
2nd
3rd
Location
Notation Parameter
J_
_2_
J_ 2.
J_
2_
A10
TI-6 Temperature (°F)
Time
136
1330
134
1455
124
1553
143 137 127
1530 1750 1915
142
1130
140
1330
124
1555
A12
TC-1 Temperature (°F)
Time
396
394
394
466
1430
451
1634
446
1830
A13
TI-11 Temperature (°F)
174
181
197
Time
/
1430
1634
1830
A14
T-12 Temperature (°F)
TC4 Time
158
1430
167
1634
160
1830
A15
TI-13 Temperature (°F)
TC2 Time
153
1430
160
1634
158
1830
A16
PI-15 Pressure (psig)
FI-4 Flow (psig)
Time
0.5
0.5
1430
0.5
0.8
1634
0.6
0.6
1830
A17
TI-14 Temperature (°F)
Time
187
1430
231
1634
245
1830
A-5
-------
V>1 iERa m
-------
OPERATING CONDITIONS LOG SHEET
CARVER GREENFIELD SITE DEMONSTRATION
Date: 8/12/91 to 8/15/91
Test Run: #2
Extraction Number
1st
2nd
3rd
Location
Notation
Parameter
X
2.
X
2_
X
X
2_
x
A2
FI-1
Flow (Ibs/min)
635
633
577
578
584
589
579
593
595
PI-3
Pressure (psig)
ATM
ATM
ATM
ATM
ATM
ATM
ATM
ATM
ATM
Ti-1
Temperature (°F)
203
204
203
151
153
152
152
153
153
Time
1326
1406
1426
1318
1323
1333
1052
1058
1105
A3
PI-4
Pressure (psig)
36
38
34
0
0
0
0
0
0
Time
1326
1406
1426
1318
1323
1333
1052
1058
1105
A5
TI-3
Temperature (°F)
210
210
211
206
182
166
207
177
162
Time
1326
1406
1426
1318
1323
1333
1052
1058
1105
A6
PI-7
Pressure (inches Hg)
-22.6
-22
-23
ATM
ATM
ATM
ATM
ATM
ATM
Tl-4
Temperature (°F)
194
199
200
96
99
101
96
99
101
Time
1220
1305
1330
1435
1443
1050
1100
1106
A7
TI-5
Temperature (°F)
103
104
105
94
94_
94
92
92
93
Time
1326
1406
1426
1318
1333
1333
1052
1058
1105
A-7
-------
OrcRA i iinG CuixOIl i^inS Luu SHciii
CARVER-GREENFIELD SITE DEMONSTRATION
(Continued)
Date: 8/12/91 to 8/15/91
Test Run; #2
Extraction Number
1st
2nd
3rd
Location
Notation
Parameter
x
1_
3_
X
2_
y
_L
1_
_3_
A10
TI-6
Temperature (°F)
Time
151
1318
152
1333
152
1335
151
1344
151
1440
139
1615
15
1052
153
1058
153
1105
A12
TC-1
Temperature (°F)
Time
—
440
1445
450
1250
446
1432
A13
Till
Temperature (°F)
Time
214
1145
217
1250
227
1431
A14
T-12
TC4
Temperature (°F)
Time
•
—
164
1145
170
1250
173
1432
A15
TI-13
TC2
Temperature (°F)
Time
—
—
—
159
1145
165
1250
169
1432
A16
PI-15
FI-4
Pressure (psig)
Flow (psig)
Time
' —
0.56
0.56
1430
0.63
0.70
1250
0.58
0.58
1432
A-8
-------
L/« i_RA ni^iG CvjiiDIl A Wi
CARVER-GREENFIELD SITE DEMONSTRATION
(Continued)
Date: 8/12/91 to 8/15/91
Test Run: #2
Extraction Number .
[st 2nd 3rd '
Location Notation Parameter X_2_JLXJLJ__L-1_JL
A 1'7 TI-14 Temperature (°F) J78_ 218 236
Time 1145 1250 1432
A18 TI-16 Temperature (°F) 178 178 179
Time 1145 1250 1432
A19 TI-17 Temperature (°F) VJ1_ 178 179
Time 1145 1250 1432
A-9
-------
APPENDIX A
MONITORING DATA
• Blank Runs
• Test Run 1
• Test Run 2
-------
APPENDIX B
SUMMARY OF ANALYTICAL RESULTS
DATA AND QUALITY CONTROL QUALIFIERS
TEST RUN 1
Bl-A Feedstock
Bl-B Slurried Feedstock, Centrate and Centrifuge Cake
Bl-C Treated Solids
Bl-D Treated Solids TCLP
Bl-E Water Condensate
Bl-F Solvent Condensate
TEST RUN 2
Feedstock
Slurried Feedstock, Centrate and Centrifuge Cake
Treated Solids
Treated Solids TCLP
Water Condensate
Solvent Condensate
BLANK RUN
B3-A Feedstock
B3-B Centrate
B3-C Treated Solids
B3-D Water Condensate
B3-E Solvent Condensate
B3-F Fresh Solvent
B2-A
B2-B
B2-C
B2-D
B2-E
B2-F
-------
DATA AND QUALITY CONTROL QUALIFIERS
U • Indicates compound was analyzed for but was not observed at a quantifiable
concentration
J - Indicates an estimated value below the method detection limit.
J - Sub-Qualifiers - Indicates an estimated value due to failure of QA/QC requirements.
(Used in conjunction with J and/or QC page or chronology):
S - Surrogate recoveries outside of control limits.
St - Surrogate recoveries outside of control limits; analysis repeated; same
results obtained; matrix interferences suspected.
M - Matrix spike and /or matrix spike duplicate outside control limits.
Mt - Same as M. Organic reference spike acceptable, matrix interference
suspected or inorganic repeat analysis still unacceptable,
r - Laboratory replicates outside of laboratory advisory limits,
h - Holding time exceeded for analysis,
t - Matrix interferences unsuspected,
p - Grab samples composited in laboratory.
B Indicates that the analyte was found in the associated laboratory or field blank.
B - Qualifiers (Used in conjunction with B);
1 - Contamination in laboratory or method blank,
e - Contamination in equipment blank
t - Contamination in trip blank,
f - Contamination in field filtration blank,
d - Contamination level elevated by dilution factor.
Additional QC and DATA Qualifiers:
Not detectable
No sample
Not analyzed.
Spiked recovery cannot be determined; sample value >4 times spike
concentration
Outside laboratory acceptance limits (Blanks spikes, Ref. spikes)
No limits currently established.
See attached data.
Insufficient sample to re-analyze
Surrogate standard diluted out.
Sample re-analyzed outside of holding time.
Unable to perform analysis due to sample matrix.
Results confirmed via repeat analysis.
ND
NS
NA
V
+ +
• +
• •
I
D
R
UP
RC
B-L
-------
TABLE Bl-A: CARVER-GREENFIELD PROCESS: TEST RUN 1
FEEDSTOCK
Parameter!
Units
SI
S2
S3
S4
S5
S6
VOC
toluene
(w'kg)
5851
4701
6201
545 1
573 1
4801
eihylbenzene
(wet wt)
883 1
965 1
10901
11001
935 1
983 1
total xylene (o,tn,p)
3480
3710
3870
3730
3500
3660
SVOC - scid extracubles
none
(m^g)
All analyses below detectable limits
(wet wt)
SVOC - base neutral extracubles
phenanthrene
100
>100
>100
B-2
-------
TABLE BI B CARVER GREENFIELD PROCESS: TEST RUN i
SLURRIED FEEDSTOCK SLURRIED FEEDSTOCK SLURRIED FEEDSTOCK
EXTRACT A EXTRACT B EXTRACT C
Parameter* Units SI S2 S3 SI S2 S3 SI SI S3
SOW
solids (*) 10.92 10.45 1024 8 32 7 83 8 36 8 55 9 26 8.85
indigenous oil (by wt) 9.78 12.13 10.59 0.64 0.17 0.55 0.15 0.41 0.35
water 0 IU 0 1U 0.1U 0.1U 0.IU 0 IU 0 1U 0.1U 0.1U
Solvenl
Isopar-L (%) (by wt) 77.59 73.04 74.91 75.49 87.33 83 35 92 15 91.61 86.94
CENTRATE CENTRATE CENTRATE
EXTRACT A EXTRACTB EXTRACT C
Parameters Units SI S2 S3 SI S2 S3 SI S2 S3
McUll
aluminum
(Mglg)
20.3 IM
21.8 JM
31.1 IM
135 IM
10100 IM
122 IM
41.7 IM
95.5 IM
100 JM
barium
(wet wt)
2.64
4.53
14.6
21 5
2670
22.4
5.43
13.5
13.9
beryllium
0.50 U
0.50 U
0.50 U
0.50 U
0.75
0.50 U
0 .50 U
0.50 U
0.50 U
calcium
50 U
SOU
50 U
50 U
2070
SO V
SOU
SOU
SOU
chromium
1.0 U
1.0 U
1.0 U
2.31
21.8
1.72
1.0 U
1.70
1.68
cobalt
5.0 U
SOU
5.0U
SOU
7.82
5.0 U
SOU
SOU
SOU
cupper
1.0 U
1.0 U
1.0 V
1.0 V
16.5
1.0 U
1.0 u
1.0 U
1.0 U
iron
38 2
32.4
50.8
157
11700
137
40,6
96.4
97.1
lead
5 .0 U
SOU
SOU
SOU
38 7
SOU
S.O U
5.0 U
SO U
magnesium
SOU
50 U
SOU
SOU
1260
50 U
50 U
50 U
SOU
manganese
1.09
1.27
2.29
6.32
404
6.25
1.57
3.76
3.83
nickel
2 04
2.0 U
2.0 U
2.68
15.9
2 .0 U
1.96
2.0 U
2.60
polasaium
SOU
50 U
50 U
SOU
824
50 U
SOU
50 U
SOU
sodium
SOU
50 U
SOU
50 U
120
SOU
SOU
50 U
50 U
strontium
5 0U!
5.0 U
5.0 U
5 .0 U
588
SOU
5.0 U
5.0 U
5.0 U
vanadium
5.0U
5.0 U
5.0 U
SOU
23,8
SOU
SOU
5.0 U
5.0 U
zinc
2.53
1.29
1.64
5.64
142
4.9S
2,67
1.82
2.54
-------
TABLE BI B CARVER GREENFIELD PROCESS: TEST RUN I
SOW
¦olidt
(*)
<0.1
0.12
0.15
0 18
0.05
0.10
<0.1
<0 1
0.12
indigenous oil
(by wl)
5.72
9.43
9.89
0.95
t.15
0.71
0.32
0.33
0.35
water
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
Solvent
laopar-L
(%) (by wl)
89.30
89.62
89.74
99.75
100.20
100.92
98.34
97.35
98.36
TPH
(jtglg)
loul
(wel wl)
1100000
952000
947000
959000
1060000
977000
1030000
844000
1220000
CENTRIFUGE CAKE
CENTRIFUGE CAKE
CENTRIFUGE CAKE
EXTRACT A
EXTRACT B
EXTRACT C
Parameters
Uniu
SI
S2
S3
SI
S2
S3
SI
S2
S3
SOW
solids
(%)
58.92
58.69
58.30
57 23
57.75
57.34
57.42
57.74
57.89
indigenous oil
(by wl)
4.22
4.68
5,80
1.18
2 76
3 46
2.33
2 69
1.47
water
<0.1
<0.1
<0 1
<01
<0.1
<0.1
<0.1
<0 1
<0.1
Solvent
Isopar-L
(%) (by wt)
36.40
36 57
35.08
42.59
42.73
42.01
40,96
42.69
40.34
B-4
-------
TABLE Bl-C: CARVER-GREENFIELD PROCESS: TEST RUN 1
TREATED SOLIDS
Parameters
Units
SI
S2
S3
S4
VOC
none
(pg/kg)
Not analyzed
(wet wt)
SVOC - acid extnctables
none
All analyses below detectable limits
(wet wt)
SVOC - base neutral extractables
isophorone
(Mg'kg)
433
330 U
330 U
phetianthrcne
(wet wt)
303 J
225 J
244 1
bia(2-ethylhexyl) phthalate
760
492
523
di-n-octyl phthalate
302)
330 U
330 U
Metals
aluminum
(Mg/g)
18500
15500
16500
barium
(wet wt)
2850
3520
3210
beryllium
1.41
1.31
1.39
calcium
5300
5130
5300
chromium
437
402
398
cobalt
15.4
14.7
14.2
copper
27.0
25.9
26.3
iron
21100
19400
20500
lead,
46.0
45.9
46.5
magnesium
2670 It
2310 It
2400 It
manganese
703
689
693
molybdenum
47.9
45.0
37.1
nickel
300
283
278
potassium
1430IM
1210 IM
1290 IM
sodium
2080
2100
2130
strontium
126
124
124
vanadium
32.6
25.6
25.7
zinc
146
144
146
SOW
aolida
(*)
96.72
95.92
96.61
96.99
indigenous oil
(by wt)
1.30
1.50
1.33
1.58
water
0.1U
0.1U
0.1U
0.1U
Solvent
Isopar-L
(%) (by wt)
0.97
0.74
0.92
1.07
TPH
total
(ji g'g)
10300
6710
6710
(wet wt)
Ignitability (°C)
90.9
95.9
95.9
B-5
-------
TABLE BI D CARVER-GREENFIELD PROCES TEST RUN I
TCLP: TREATED SOLIDS
Treated 1
Treated 2
Treated 3
%
%
%
Parameters
Units
Biased
Unbiased
Recovered
Biased
Unbiased
Recovered
Biased
Unbiased
Recovered
VOC
benzene
50 U
50 U
95
50 U
SOU
102
50 U
50 U
94
carbon tetrachloride
(MS")
50 U
SOU
95
50 U
sou
100
SOU
50 U
94
chlorobenzene
SOU
50 U
96
50 U
sou
106
SO U
50 U
94
chloroform
50 U
50 U
96
50 U
50 U
100
50 U
50 U
95
1,2-dichloroethane
SOU
SOU
93
50 U
sou
97
50 U
SO U
106
1,1-dichloroethene
50 U
50 U
97
50 U
50 U
92
50 U
50 U
102
methyl ethyl ketone
100 U
100 U
70
100 U
100 u
79
100 U
100 U
77
letrachloroethene
SOU
50 U
97
SOU
50 U
101
50 U
50 U
87
trichloroethene
50 U
50 U
94
50 U
50 U
100
107
94.1
88
vinyl chloride.
50 U
50 U
101
50 U
50 U
94
50 U
50 U
102
SVOC - acid exiraciatsles
in t p-cresol
(P&H)
100 U
100 U
JJ
100 u
100 U
33
100 U
100 U
39
u-eiesol
100 u
100 u
37
100 u
100 u
38
100 U
100 U
46
pcnuchlocophcnol
200 U
200 U
62
200 U
200 U
72
200 U
200 U
60
2,4,5-trichIorophenol
100 U
100 U
52
100 u
100 U
58
100U
100 U
51
2,4,6-triehIoropheno
100 u
100 u
56
100 u
100 u
62
100 U
100 U
58
SVOC - base neutral extractables
1.4 dichlorobenzenc
(pe'n
50 U
50 U
38
50 U
sou
45
SOU
SO U
49
2.4 dimtrotoluene
SO U
50 U
52
SOU
sou
55
SOU
50 U
58
he xachlorobenzene
50 U
50 U
54
SO U
so u
51
50 U
50 U
60
hexadiloroethane
50 U
50 U
36
50 U
50 U
44
SOU
50 U
47
nitrobenzene
SO u
50 U
49
SOU
50 U
58
SOU
50 U
64
pyridine
100 u
100 U
30
100 u ,
too u
29
100 U
100 U
33
hcxachlt>ro-l ,3-buladieiie
sou
SOU
39
sou
sou
37
50 U
50 U
51
B-6
-------
-------
TABLE BID: CARVER-GREENFIELD PROCES: TEST RUN I
TCI.P: TREATED SOLIDS
Treated I
Treated 2
Treated 3
%
%
%
Parameter*
Units
Biased
Unbiased
Recovered
Biased
Unbiased
Recovered
Biased
Unbiased
Recovered
vlclals
1
arsenic
(mg/l)
0.50 0
0.50 U
no
0.50 U
0.50 U
106
0.50 U
0.50 U
109
barium
1.15
1.15
101
1 22
1.20
98
1.17
1.17
102
cadmium
0,10 U
0.10 U
111
0.10U
0 10 U
105
0.I0U
0.10 U
110
chromium
0.I0U
0.10U
10?
0 I0U
0 10 U
102
0.10 U
0.10 U
108
lead
0.10 U
0 10 U
107
0 10 U
0.10 U
102
0 10 U
0.10 U
106
mercury
0.0020 U
0.0020 U
83
0.0020 U
0 0020 U
61
0 .0020 U
0.0020 U
61
selenium
0.50 U
0.50 U
103
0.50 U
0 50 U
93
0.50 U
0.50 U
105
silver
0.10 U
0.10 U
75
0.10U
0.10 U
94
0 258
0.190
74
B-7
-------
TABLE Bl-E: CARVER-GREENFIELD PROCESS: TEST RUN 1
WATER CONDENSATE
Parameters
Units
SI
S2
S3
VOC
acetone
(Mg/1)
4790
5110
4880
2-bulanone (MEK)
1020
1110
1070
SVOC - acid exlractables
phenol
(Mg/0
55.01
54 0 J
500 U
SVOC - base neutral extractables
none
(w/i)
All analyses below detectable limits
Metals
aluminum
(mg/1)
3.05 Jr
3.13 Jr
1.66 Jr
antimony
0.0545
0 050 U
0.050 U
barium
0.0404
0.0388
0.0354
calcium
4.37
4 30
4.18
chromium
0.010 UJ
0.010 UJr
0.0109 J
iron
2.38
3.84
1.82
magnesium
1.20
1.14
0.915
manganese
0.0946
0.0959
0.0894
nickel
0.0200 UJ
0.0519 Jr
0.0432 J
potassium
0.50 U
0.693
0.50 U
sodium
3 .32 JMt
3 .14 JMt
2.70 JMt
strontium
0.0600
0.0573
0.0556
zinc
0.184
0.199
0.194
Solvent
bopar-L
(%) (by wt)
0.84
1.15
0.71
TPH
total
(mg/1)
976
. 2100
1250
Conventional
PH
4.59
4 64
4.47
alkalinity, total
(mg/1)
2.0 U
2.0 U
2.0 U
acidity, total
36.0
37.5
36.0
BODj
70 R
75 R
84 R
COD, dichromate
1040
1310
1230 JMt
nitrogen, ammooia
0.050 U
0.050 U
0.050 U
nitrogen, Kjeldahl
0.787
0.438
0.379
solids, suspended
78.6
91 8
76.5
sulfate
10.0 U
10.0 U
10.0 U
B-8
-------
TABLE Ct-F: CARVER-GREENFIELD PROCESS. TEST RUN 1
SOLVENT CONDENSATE
Name Unita SI S2 S3
Meula
aluminum (Mg'g) 13.3 9,90
(wet wt)
Solvenl
bop«r-L (%) (by wt) 100.55 99,79 87.87
TPH
low! . (Jig/g) 1000000 915000 943000
(wet wt)
B-9
-------
TABLE B2-A: CARVER-GREENFIELD PROCESS: TEST RUN 2
FEEDSTOCK
Parameters
Unit*
SI
S2
S3
S4
S5
S6
VOC
benzene
O^kg)
1250 U
688 J
1250 U
1250 U
1230 U
766 J
toluene
(wet wt)
763 I
803 J
1150 J
1130 J
1210 J
1220 J
ethbenzene
1860
1960
2060
1510
2140
1790
total xylene (o.m.p)
8820
9000
9270
7870
10000
8280
SVOC - acid extractables
none
(Mg/kg)
All analyses below detectable limits
(wet wl)
SVOC - base neutral extractables
phenanthrene
(Mg/kg)
11000 J
11500 J
12100 J
1090 J
1070 J
12000 J
2-cnethyl naphthalene
(wet wt)
45500 J
50900
55800
36600 J
48800
57300
napthalene
50000 U
17600 J
17500 J
50000 U
16200 J
19200 J
Metala
aluminum
(MS'S)
7380
7150
7100
7230
7610
7640
barium
(wet wt)
653
688
666
450
520
478
beryllium
0.65
0.63
0.73
0.79
0.74
0.68
boron
31.6
20 U
20 U
20 U
20 U
20 U
cadmium
3.90 JM
4.10 JM
4.07 JM
4.01 JM
3 .82 JM
4 .12 JM
calcium
8000
7630
7570
7980
7840
7690
chromium
140
138
137
140
141
141
cobalt
9.15
8.89
10.0
9.54
9.33
9.52
copper
83.8
87 2
87.8
93.7
92.2
86.3
iron
20000
19300
19700
25 500
19800
20100
lead
207
196
208
205
213
202
magnesium
1260
1190
1230
1300
1260
1270
manganese
266
264
284
285 .
276
281
molybdenum
23.8
24.8
26.4
26.8
25.6
24.7
nickel
20.6
19.7
19.7
20.7
21.9
22.4
potassium
711 JM
726 JM
707 JM
778 JM
785 JM
776 JM
sodium
609 Jl
579 Jt
597 It
622 Jt
607 Jt
581 Jl
strontium
261
236
279
286
298
264
vanadium
21.5
20.8
22.6
22.2
22.4
22.7
zinc
1000
1030
990
1030
1020
1010
SOW
solids
(*)
52.31
53.00
-52.69
52.06
52.08
52 50
indigenous oil
(by wt)
7.37
7.78
7.05
6.51
7.69
7.03
water
36.62
34.95
34.07
34.74
33.63
34.61
Solvent
Isopar-L
(%) (by wt)
0.1U
- 0.IU
0.1U
0.1U
0.1U
0.10
TPH
total
(Mi/g)
79200
78600
94900
82500
103000
98100
Ignitability (°C)
>100
>100
>100
B-LO
-------
TABLE B2-B: CARVER-GREENFIELD PROCESS: TEST RUN 2
SLURRIED FEEDSTOCK
SLURRIED FEEDSTOCK
SLURRIED FEEDSTOCK
EXTRACT A
EXTRACTS
EXTRACTC
Parameters
Units
SI
S2
S3
SI
S2
S3
SI
S2
S3
SOW
solids
(%)
12.27
10.54
10.96
9,52
8.92
8.95
9.07
8.40
10.02
indigenous oil
(by wi)
3.36
8 27
6 05
0 43
028
0.38
0.17
0.25
0.17
water
O.IU
0.1U
0 IU
0.1U
0.1U
O.IU
O.IU
O.IU
O.IU
Solvent
Isopar-L
(*) (by wt)
78.01
75.80
81 78
91.57
92.72
91 23
94.89
92 63
91.9S
.
CENTRATE
CENTRATE
CENTRATE
EXTRACT A
EXTRACT B
EXTRACTC
Parameters
Units
SI
S2
S3
SI
S2
S3
SI
S2
S3
Metals
aluminum
(fg'g)
23 1
40.9
10.3
13.8
24,4
20,1
10 0 U
32.0
17.9.
barium
(wet wt)
46 I
57.9
17.6
40 8
27.8
27.6
13 6
54 7
30.3
chromium
1.63
1.98
1.0
1.0 U
0.895
0.957
I0U
1.22
10 U
copper
1 46
1.58
1.0 U
1.0 U
1.0 U
1 OU
1.0 U
1.0 U
1.0 U
iron
70.1
97.3
28,5
26.6
39.5
35,7
13 4
55 2
30.0
manganese
1.27
1.58
0.52
0.50
0.70
072
0 50 U
1.15
0.63
sodium
SOU
50 U
50 U
49 8
57.3
50.6
50 U
SOU
54.7
zinc
7.33
10.1
2.85
2.18
2.89
2.74
I.0U
3.07
1.74
SOW
,
solids
(%)
0.1U
0.16
0.1U
0.1U
O.IU
0.1U
O.IU
0 16
0.18
indigenous oil
(by wt)
7.59
5.83
6.42
0.75
1.03
0.59
0,24
0.41
0.25
water
0.1U
0 IU
0.1U
O.IU
0 IU
0 IU
0 IU
O.IU
O.IU
Solvent
Isopar-L
(%) (by wt)
88.52
88 32
84 87
99.67
99.97
102,29
101.97
100.59
104 33
B-l 1
-------
TABLE B2-B: CARVER-GREENFIELD PROCESS; TEST RUN 2
TPH
total 0»g/g) 901000 926000 1030000 1050000 917000 927000 1110000 920000 1000000
(wci wt)
CENTRIFUGE CAKE CENTRIFUGE CAKE CENTRIFUGE CAKE
EXTRACT A EXTRACT B EXTRACT C
Parameters Unit* SI • S2 S3 SI S2 S3 SI S2 S3
SOW
solids (*) 68.13 67.52 68.93 60.76 65.82 66.46 66 57 66.82 66.68
indigenous oil (by wt) 2.80 4.33 3 .79 0.94 158 1.27 1.17 1.08 0 94
water 0.1U O.IU 0.IU 0 1U 0.1U 0.1U 0.1U 0.1U 0.1U
——— j— 1
Solvent
Isopar-L (*) (by wt) 26.69 26,31 26.19 31.64 31 34 31.67 30 63 31.71 31.36
B-12
-------
TABLE B2-C: CARVER-OREENFIELD PROCESS: TEST RUN 2
TREATED SOLIDS
Name
Units
SI
S2
S3
S4
VOC
Wt)
svoc - acid exlractablea
none
Og/kg)
All analyses below detectable limits
(wet wt)
SVOC - base neutral extractables
2-melhyl naphthalene
O^g/kg)
1760
2660
2530
napthalene
(wet wt)
957 J
1250 J
957 J
bis(2-ethylhexyl) phthalate
1150 J
1460 J
1610 J
Metals
aluminum
(Mg/g)
9170
9570
7080
barium
(wet wt)
2470
5230
1820 Jr
beryllium
1.16
1.17
1.02
cadmium
5.66
5 49
5.50
calcium
12200
11700
12200
chromium
307
312
336
cobalt
13.4
13.3
13.0
copper
119
104
99.0
iron
38400
36100
34800
lead
254
252
239
magnesium
1990 JM
1870 JM
1920 JM
manganese
523
492
501
molybdenum
48.9
51.5
46 5
nickel
140
143
154 Jr
potassium
1030 JM
956 JM
922 JM
sodium
2290
2290
2350
strontium
390
412 '
332
vanadium
23.5
20.7
19.6
zinc
1150
1130
1180
SOW
solida
(*)
98.58
98.28
95.34
101.03
indigenous oil
(by wt)
1.18
0.84
0.69
0.68
water
0.1U
0.1U
0.1U
0.1U
Solvent
Iaopar-L
(%) (by wt)
1.12 .
I 02
0.90
0.90
TPH
total
(m's)
3840
8130
7880
(wet wt)
Ignitability (°C)
>100
>100
> 100
B — 13
-------
TABLE B2-D:
CARVER-GREENFIELD PROCESS TEST RUN 2
TCLP:
TREATED SOLIDS
Treated 1
Treated 2
Treated 3
*
*
*
Parameters
Uniu
Biased
Unbiased
Recovered
Biased
Unbiased Recovered
Biased
Unbiased
Recovered
VOC
benzene
Oig/1)
SOU
SOU
102
SOU
so U
86
SOU
SOU
96
carbon tetrachloride
SOU
50 U
99
SOU
50 U
88
50 U
50 U
92
chlorobenzenc
SOU
50 U
103
50 U
50 U
85
50 U
50 U
96
chloroform
SOU
SOU
104
SOU
50 U
86
50 U
SOU
99
1,2-dichIoroethane
SOU
50 U
106
50 U
SOU
87
50 U
50 U
96
1,1-dichloruelhcne
SOU
50 U
114
50 U
SOU
86
SO U
50 U
102
methyl elhyl ketone
100 u
100 U
71
100 U
100 U
74
100 U
100 U
117
lelraehloroelhene
sou
SOU
101
SOU
SOU
82
SOU
SOU
102
trichloroethene
sou
50 U
99
SOU
SOU
87
SOU
SOU
95
vinyl chloride
20 U
20 U
115
20 U
20 U
82
20 U
20 U
99
SVOC - acid extracubles
m tp-
-------
TABLE B2 D CARVER-GREENFIELD PROCESS; TEST RUN 2
TCLP: TREATED SOLODS
Treated 1
Treated 2
Treated 3
*
*
%
Parameters
UmUi
Biased
Unbiased
Recovered
Biased
Unbiased
Recovered
Biased
Unbiased
Recovered
cadmium
(mg/l)
o.ioo u
0 .100 U
85
0.100U
0.100 U
84
0.100U
O.IOOU
84
chromium
0.100U
0 .100 U
83
0 .100 U
0 .100 U
84
0.100 U
0 100 U
85
lead
0.100 u
0 .100 U
86
0.100U
0.100 U
86
0.100 U
0.100 U
87
mercury
0.0020 U
0.0020 U
$5
0.0020 U
0.0020 U
53
0,0020 U
0,0020 U
59
•elenium
0.500 U
0.500 U
79
0.500 U
0.500 U
84
0.500 U
0,500 U
85
silver
0 10 u
0.10U
58
0.100U
0.10 U
68
0 10 U
0.10 U
58
B-15
-------
TABLE B2-E:
WATER CONDENSATE
Parameter*
Uniu
SI
S2
S3
VOC
acetone
(ug/l)
1560
3130
1150
2-buUnone (MEK)
500 U
500 U
187
SVOC - acid extracubles
none
(ug/l)
All arulysea below detectable limiu
SVOC - base neutral extriclables
di-n-butyl phlhalate
(ug/l)
5 U
5.3
50 U
bis(2-ethylhexyl) phlhalate
62.1
78.7
448
Melals
aluminum
(mg/l)
16.8
12.7
10.5
calcium
57.1
50 U
SOU
iron
9.38
5 .0 U
5.0 U
sodium
83.1
60.8
60.0
Solvent
Isopar-L
($)(by wt)
0.1U
0.1U
0.1U
TPH
toul
(mg/l)
267
627
104
Conventional
PH
(mg/l)
7.15
7.07
6.25
alkalinity, toul
4.1
4.1
2.0 U
acidity, total
28
36
29
BODj
10.4 R
11.6 R
16 R
COD, dichromate
66.0
174
944 JMt
nitrogen, ammonia
0.050 U
0.050 U
0.050 U
nitrogen, Kjeldahl
0.204
0.20 U
0.20 U
solids, suspended
75 .0 R
63.0 R
73.0 R
sulfate
10.0 U
10.0 U
10.0 U
B-16
-------
TABLE B2-F: CARVER-GREENFIELD PROCESS: TEST RUN 2
Parameters
Units
SI
SOLVENT CONDENSATE
S2
S3
Metals
aluminum
boron
calcium
sodium
Zinc
(M' 8)
(wet wt)
10.0 U
32.9
46.3 U
53.7
1.0 U
9.82
20 U
50 U
57.5
1.0 U
10.0 u
20 U
SOU
50 U
1.63
Solvent
Isopar-L.
(%) (by wt)
99.74
97.74
101.62
TPH
total
(wet wt)
927000
980000
863000
B-17
-------
TABLE B3-A;
CARVER-GREENFIELD PROCESS; BLANK RUN
FEEDSTOCK
Parameters
Units
SI
S2
VOC
methylene chloride
6.43
5 U
acetone
(wet wt)
20 U
51.6
tetrachJoroethene
1,29
5 U
toluene
80.2
46.0
ethylbenzene
2.60
5 U
total xylene (o,m,p)
3.92
2.05
SVOC - acid exiractables
none
All analyiea below detectable limits
(wet wt)
SVOC - base neutral extractable*
phenamhrene
f)
330 U
105 JS
di-n-butyl phthalate
(wet wt)
330 U
106 JS
bia(2-ethylhe*yl) phthalate
333
1810 IS
di-n-octyl phthalate
330 U
216 IS
2-methyl napthalene
660 U
546 JS
Metala
aluminum
(Mg'g)
10600
9100
barium
(wet wt)
61.5
67.5
beryllium
1.45
1.46
boron
28.6
15.8
cadmium
0.468
0.460
calcium
12100
12400
chromium
4.01
4.66
copper
2,50
2.60
iron
13800
13800
lead
30.0
30.2
magnesium
3390
3220
manganese
507
500
nickel
3,73
4.16
potassium
615
632
sodium
9250
9450
strontium
214
221
zinc
59.7
61.0
SOW
•olidi
(*)
86.20
89.12
indigenous oil
(by wt)
0.11
0.1U
water
12.35
8.78
Solvent
Isopar-L
(%) (by wt)
0.1U
0.1U
TPH
total
Wr)
10.0 u
10.0 u
(wet wt)
B-18
-------
TABLE B3-B. CARVER-GREENFIELD PROCESS: BLANK RUN
Parameters
UniU
CENTRATE
SI
S2
Meuls
chromium
iron
nickel
sodium
zinc
(Mglg)
(wet wt)
2.68
10.6
1.30
25 U
0.50 U
2.90
11.5
1.35
32.9
3.44
SOW
solidi
indigenous oil
water
<%)
(by wt)
0.1U
0.45
0.1U
0.1U
0.94
0 1U
Solvent
Isopar-L
(*) (by wt)
70.22
43.37
TPH
total
(wet wt)
1210000
1130000
B-19
-------
TABLE B3-C: CARVER-GREENFIELD PROCESS: BLANK RUN
TREATED SOLIDS
Parameters
Units
SI
S2
VOC
none
AJ1 analyses below detectable limits
SVOC - acid extractables
none
0«/kg)
All analyses below detectable limits
(wet wt)
SVOC - base neutral extractables
none
(pg/kg)
All analysea below detectable limits
(wet wt)
Metala
aluminum
(Mg'g)
8150
8900
barium
(wet wt)
78
86.6
beryllium
1.28
1..32
boron
16.8
14.7
cadmium
0.420
0.442
calcium
11100
11200
chromium
16.0
14.6
copper
2.45
2.29
iron
12400
12700
lead
27.2
27.5
magnesium
2810
2920
manganese
448
463
nickel
9.50
10.2
potassium
779
763
sodium
8400
8710
strontium
197
204
zinc
59.5
57.7
sow
solids
(*)
88.97
88.40
indigenous oil
(by wt)
1.36
0.98
water
0.1U
0.1U
Solvent
Uopar-L
(%) (by wt)
3.94
5.22
TPH
total
(Mi's)
145000
117000
(wet wt)
B-20
-------
TABLE B3-D: CARVER-GREENFIELD PROCESS. BLANK RUN
WATER CONDENSATE
Parameter!
Units
SI
S2
voc
acetone
(Mg'O
3730
3820
SVOC - acid extractables
none
Og/I)
Ail analyses below detectable limits
SVOC - base neutral extractables
bis(2-ethylhexyl) phthalate
(pg/l)
5.77
78.9
Metals
aluminum
(mg/1)
4.00 Jr
2.63 Jt
barium
0 0242
0.0211
boron
0.20 U
0.466
calcium
3.68
2.78
chromium
0.0665
0.051
iron
3.62
2.10
magnesium
1.49
1.09
manganese
0.0786 Jt
0.0561 Jt
nickel
0.037Jr
0.0305 Jr
sodium
4.26
3.23
strontium
0.0605
0.050 U
zinc
0.114
0.0687
Solvent
Isopar-L
(%) (by wt)
1.00
0 46
TPH
total
(mg/1)
250
25.0
Conventionals
pH
(mg/1)
7.19
6.91
alkalinity, total
4.1
4.1
acidity, total
16 4
17.9
BODj
34.3
35.3
COD, dichromate
235
1520
nitrogen, ammonia
0 050 U
0.050 U
nitrogen,, Kjedahl
0.948
0.695
solids, suspended
188
105
sulfate
10.0 U
10.0 U
B-21
-------
TABLE B3-E: CARVER-GREENFIELD PROCESS: BLANK RUN
SOLVENT CONDENSATE
SI
S2
10.8 Jr
10 U
4.33
16.8
1.72
25 U
5.0 UJr
21.4
3.12
13.7
1.16
29.6
77.61
33.44
1030000
1090000
Parameter*
Unit*
Metals
aluminum
boron
chromium
iron
nickel
sodium
Ob's)
(wet wt)
Solvent
bopar-L
TPH
total
(%) (by wt)
Og'g)
(wet wt)
B-22
-------
TABLE B3-F: CARVER-GREENFIELD PROCESS
SOLVENT
Parameters
Uniu
SI
S2
Metals
aluminum
boron
chromium
iron
nickel
(Ws)
(wel wt)
5.12
12.2
4.69
23.6
2.12
5.0 U
10 U
3 53
13.9
1.67
Solvent
bopar-L
(%) (by wt)
101.93
82.04
B-23
-------
APPENDIX C
ANALYTICAL PROCEDURES FOR SOW AND SOLVENT
Solids/Oil/Water (SOW)
GC Solvent
-------
ANALYTICAL PROCEDURE FOR SOLID/OIL/VATER CONTENT
OF SOLIDS, LIQUIDS AND SLURRIES
GENERAL DISCUSSION
The Carver Greenfield process is a means of separating sol id-liquid
mixtures into three product streams: a clean dry solid; a water product
substantially free of solids and organics; and a concentrated mixture of
extracted organics. The extracted organics, generally referred to as
indigenous oils, are extracted into a hydrocarbon based solvent (carrier oil).
As the feed mixture is processed, oil and water are removed. The feed mixture
is processed from an oily wet semi-solid or slurry to a clean dry solid
product, ' The solid, oil and water content of the feed and products are
important parameters in assessing the performance of the process. The
analytical procedure discussed herein has been developed to quantify these
parameters in feed mixtures, and the intermediate and final products.
The method is based on ASTM Method #D95-70 and AOCS Ca 29-45. These
procedures are commonly used to quantify the solid and water content of crude
oils. Dehydro-Tech Corporation has modified these procedures to address the
analytical needs of the Carver Greenfield process. The differences in the
application of the procedure are caused by differences in the characteristics
of the samples being analyzed. The ASTM procedure was based on the analysis of
oils contaminated with small quantities of solids and water. Dehydro-Tech's
application of the procedure is for the analysis of solids contaminated with
oil and water.
The procedure is basically a solvent extraction/distillation procedure,
similar to the Carver Greenfield process itself. The sample is mixed with
toluene, which extracts the indigenous oils from the solid phase and develops
an azeotrope with water. The mixture is distilled, producing a two phase
distillate (water and toluene). Toluene is refluxed back to the distillation
flask, while distillation is continued to strip all water from the sample.
When water distillation is completed, the solids and toluene mixture remaining
C-I
-------
in the distillation flask is filtered. The filtrate (toluene with indigenous
oils) is set aside and the solids are reslurried with fresh toluene for a
second extraction. Multiple extractions are performed to ensure complete
removal of the indigenous oils. After all extractions are complete the
recovered filtrates are composited and distilled to strip the toluene from the
indigenous oil. The extracted solids and the residual toluene/indigenous oil
mixture remaining in the distillation flask are dried in a vacuum oven to
remove the final traces of toluene. Solids and indigenous oil content are
determined by direct weight; water content is determined indirectly by
subtracting the combined weight of the indigenous oil and solids from the total
sample weight. The results are reported on a weight percent basis.
HydroQual assessed and refined the procedure for the Carver Greenfield
process demonstration at the PAB Oil Site. The objective of the refined
procedure was to optimize the time required for analysis while still retaining
the maximum degree of precision and accuracy. The time consuming steps of the
procedure are the multiple extractions and the time required for drying in the
vacuum oven. Two extractions were found to be sufficient for removal of water
and indigenous oils in samples similar in character to those which will be
encountered at the PAB Oil site. Additionally, a drying time of 75 minutes for
extracted solids and 60 minutes for oil was found to be sufficient in reaching
a constant final weight for samples sizes ranging from 15 to 50 grams (wet
weight). The typical sample size was approximately 25 grams (wet weight).
APPARATUS
The apparatus used in this procedure is similar to the Dean Stark
distillation apparatus. This consists of a heater, distillation vessel, reflux
condenser, and a graduated receiver. Figure 1 shows a typical assembly of the
distillation equipment. Support equipment includes a multiple-place variable
temperature hot plate; vacuum oven; electronic balance; vacuum pump, manifold
and flask; Buchner funnel; centrifuge and filter paper.
C-2
-------
500 ML. Wid* Mogtfi
Clou Ettraction Flak
FIGURE 1. ASSEMBLY OF DEAN STARK DISTILLATION APPARATUS
C-4
-------
The distillation flask is a 500 raL wide mouth flat bottomed round glass
flask. A 300 mm straight water-cooled glass condenser is used for condensing
water and solvent vapors. A graduated valved glass burette with a reflux tube
is used to collect stripped water and toluene. Cork stoppers are used for
joining the glassware. Ground-glass joints should not be used due to their
tendency to trap solids, which makes it difficult to obtain a proper seal and
also makes quantifiable transfers difficult.
The distillation must be done in a ventilated hood. Filtration equipment
and the vacuum oven should also be located in a vented hood. The vacuum pump
for the vacuum oven should be operated continuously when samples are being
dried. The vent valve should be opened slightly to permit air to sweep through
the oven while still maintaining full vacuum. This is done to keep toluene
vapors from accumulating in the oven.
REAGENTS
A suitable solvent for this procedure must be insoluble in water and water
insoluble in the solvent. It should also have a boiling point between 75 and
150°C. Normally any hydrocarbon fulfilling this criteria can be used as a
solvent-carrier, such as technical-grade toluene, xylene and petroleum
distillate. The choice of solvent-carrier can also be dependent on the
characteristics of the indigenous oil present in the material. The preferred
solvent for this application is toluene, which forms a minimum boiling
azeotrope with water at about 80aC.
PROCEDURE
Sample Preparation
Some of the samples analyzed by this procedure have a tendency to separate
into solid, oil and water phases. Ideally a separate sample, weighing
approximately 25 gm and representative of the whole, should be taken and
C-5
-------
reserved for analysis. After the entire sample is transferred to the
distillation flask, the sample container should be flushed with a portion of
the toluene to be added for the first extraction. This will ensure recovery of
residual solids, oil, and water adhering to the walls of the container.
The sample should be homogenous and well mixed in the toluene before the
analysis is started. Large clumps of solids should be broken and the sample
should be well mixed into the toluene before the first extraction is started.
Sample Size
The appropriate sample size to be used for analysis is determined by solids
content of the sample. Larger sample sizes are required for materials with
lower solids contents. Recommended sample sizes, based on the solids content
are given below:
Solids Content Recommended Sample Size
(percent)
1 - 10 100
10 - 20 50
20 - 50 25
50 - 100 15
Typical sample size for samples encountered in the Carver Greenfield
demonstration will be approximately 25 g. Sample size should not exceed 50 g
without re-evaluating the number of extractions required and identifying the
required drying time,
Standardization
To determine the accuracy of the method it is necessary to run standards
having a known quantity of solids, oil and water. The standards should be
representative of the samples to be encountered during the demonstration.
C-6
-------
The standards are prepared by mixing known quantities of solids, oil, and
water. For this application of the procedure, barite and bentonite were used
as the solids matrix. Their selection is based on their common use in drilling
muds, which comprised a major component of the contents of the waste pits at
the PAB Oil site. Solids should be water-free before the standard is
formulated to ensure that the recorded weight is of dry solids. To ensure
this, the solids should be dried at 105 to 110°C and cooled in a desicator.
Motor oil was used to simulate indigenous oil in the formulation of the
standards. The basis of its selection is its high boiling point and viscosity.
The standards are prepared individually because it is difficult to ensure
that a bulk standard is homogeneously mixed. Each standard is prepared by
accurately weighing (0.01 g sensitivity) the components to a tared distillation
flask. The mixture is then allowed to stand for approximately 12 hours to
allow the solids to absorb the oil and water.
Procedure
1. Measure an appropriate amount of sample and transfer it carefully to
the tared distillation flask. Refer to the recommendations given
earlier for selecting the size of sample. Record the sample weight.
2. Add 150 mL of technical-grade toluene in a tared distillation flask,
mix it with the sample and start heating the distillation flask.
Water and toluene will co-distill and condense in the condenser.
Water will be collected in the graduated receiver and toluene will
overflow back to the distillation flask.
3. Stop heating the distillation flask after 30 minutes. Disconnect and
allow the flask and receiver to cool to room temperature. Record
volume of water recovered.
C-7
-------
4. Transfer the liquid contents of the extraction flask to centrifuge
tubes. The liquid is centrifuged for about eight minutes at 2500 to
3000 rpm.
5. Decant the supernatant from the centrifuge tube and filter it through
a Buchner funnel and a tared filter paper (Whatman if2) at full vacuum.
The mixture of indigenous oil, carrier oil and toluene will pass
through the filter paper and collect in the filter flask. Reserve
this filtrate. This completes the first extraction.
6. Carefully recover the solids from the filter paper and transfer them
back to the distillation flask for another extraction (retain the
filter paper). Add 60 mL of fresh toluene to the distillation flask
and thoroughly mix it with the solids using a spatula to break the
agglomerates of partially dried solids. Boil the contents of the
distillation flask for about five minutes. Disconnect and allow the
flask and liquid receiver to cool to room temperature. Centrifuge and
then filter the decanted supernatant using a fresh tared filter paper
and reserve the filtrate. This completes the second extraction.
7. Carefully recover the solids with the filter paper. Break any
agglomerates of solids remaining in the flask using a spatula. Place
the filter papers from the first and second extractions, and the flask
containing the solids in a vacuum oven at 250°F and full vacuum.
After 50 minutes take out the flask from the oven and again break any
agglomerates of partially dried solids. Place the flask back in the
oven for an additional 25 minutes. Cool the flask and filter papers
to room temperature in a dessicator. Weight the flask and filter
papers. Subtract the tare weights of the distillation flask and
filter papers and record the sum of both as the weight of solids.
8. Transfer the toluene and oil mixture collected from both the
extractions and filtrations into a tared 500 mL distillation flask.
Heat the flask until all the toluene and carrier oil are distilled
C-8
-------
over and Che production of distillate stops. Place the distillation
flask in the vacuum oven at 250°F and full vacuum for at least 60
minutes. Cool the flask to room temperature in a dessicator. Weight
the flask. Subtract the tare weight of the distillation flask and
record as the weight of indigenous oil.
% Water- - Volume of water x 100
Sample Wt
X Solids - Solids Wt x 100
Sample Wt
X indigenous Oil - Indigenous Oil Wt x 100
Sample Wt
FREQUENCY OF QAPP PROCEDURE FOR SOW ANALYSIS:
SOW analyses will be conducted each day, using a six-place assembly. First
test run each day will test four samples, one sample duplicate and one
standard. Rest of the runs will test five samples plus one sample duplicate.
QAPP ACCEPTANCE CRITERIA AND CORRECTIVE ACTION FOR SOW ANALYSIS:
CALCULATIONS
COMPONENTS
PRECISION
(RPD)
ACCURACY
(% RECOVERY) CORRECTIVE ACTION
Solid
Oil
Water
15
20
20
95 - 103
74 - 118
88 - 117
Repeat the analysis. If the
reanalysis yields acceptable
results, only those will be
reported. If acceptable results
are not obtained on reanalysis,
both sets of data will be reported
with a note stating the problem
C-9
-------
ANALYTICAL PROCEDURE FOR THE SOLVENT (ISOPAR-L) CONTENT
DETERMINATION OF SOLIDS, LIQUIDS AND SLURRIES
GENERAL
The analytical procedure discussed herein has been developed to quantify
the solvent (Isopar-L) present in feed mixtures, and the intermediate and final
products of the Carver Greenfield (C-G) process. The method is based on the
Dehydro-Tech Corporation (DTC)'s analytical method # CGP-6E, CGP-6F, and CGP-
15.
The procedure requires the use of a Gas Chromatograph consisting of a FID
detector and a six foot long stainless steel column with 10% OV-101 on
chromosorb 60/80 packing. One drop of tetradecane(C14) is added to the sample.
This is followed by the addition of carbon disulfide. In samples containing
water soluble solids, water is also added in addition to carbon disulfide.
Isopar-L and tetradecane are extracted in the carbon disulfide solution by
vigorous shaking. The mixture is then centrifuged and supernatant, containing
carbon disulfide is separated and injected into gas chromatograph. The
quantity of solvent (Isopar-L), on weight percent basis, is calculated assuming
that response of Isopar-L is equal to the response of Tetradecane(C14),
The General Testing Corporation (GTC) evaluated the above procedure to
analyze Isopar-L and recommended few modifications to the original procedure to
improve the chromatography of peaks in Isopar-L and to prevent the saturation
of the column and detector. Lowering the column temperature to 150°C was found
to improve the chromatography of Isopar-L peaks, GTC also observed that for
the samples containing greater than 5X Isopar-L, the dilution of carbon
disulfide extract prevents the saturation of column and detector.
C-10
-------
APPARATUS
The apparatus used in this procedure includes a Gas Chromatograph (GC), a
FID detector, a column with 102 OV-101 on Chromosorb G packing and an
integrator. Gas Chromatographic conditions for hydroextracted solids are
summarized below:
Column
Column Packing
Oven Temp.
Rate of Heating
Injection Port. Temp.
Detector_
Detector Port. Temp
Carrier Gas
Carrier Flow
Hydrogen (FID)
Air (FID)
Sample Injection
6' long, 1/8" ID, Stainless Steel
10X 0V-101 on Chromosorb 60/80
150°C (for initial 22 minutes), 300°C (for
final 20 minutes)
25°C per minute
200°C
FID
300°C
Nitrogen, UPC Grade
20 mL/min.
25 mL/min.
200 mL/min.
1 uL
Gas Chromatograph and integrator used to develop this procedure were of
Hewlett Packard make (model # HP 5890A and HP 3392A respectively).
REAGENTS
Reagents used in this procedure are Tetradecane(C14) and carbon disulfide.
Tetradecane is used as an internal standard. Carbon disulfide is required to
extract the Tetradecane (C14) and Isopar-L from the sample.
C-U
-------
STANDARDIZATION
To determine the accuracy of the method it is necessary to run standards
having a known quantity of solvent. The standards should be representative of
the samples to be encountered during the demonstration of the C-G process. The
standards are prepared by mixing known quantities of Isopar-L and tetradecane
in carbon disulfide. Each standard is prepared by accurately weighing (0.0001
g. sensitivity) the components to a tared VOC vial and the vials are
immediately sealed with the cap.
PROCEDURE
1. Measure accurately approximately 2 to 5 gms. of sample into a tared 40 ml
VOC vial.
2. Add one drop of Tetradecane (C14) and re-weigh. Record the weight.
3. Add 10 ml. of Carbon Disulfide. In the samples containing water soluble
solids, also add 10 ml of water.
4. Shake the mixture vigorously to extract the Isopar-L and Tetradecane in the
Carbon Disulfide.
5. Centrifuge and carefully pipette (or decant off) the supernatant liquid.
For samples that contain water, the Carbon Disulfide will be the bottom
layer. Hence extra care should be taken while pipetting Carbon disulfide
layer to avoid upper water layer. Filter the Carbon Disulfide extract
through a 0.45 um filter syringe to remove any suspended particles.
Collect the filtrate into a clean, tightly capped vial.
6. Inject 1 to 5 uL of Carbon Disulfide extract into gas chromatograph.
C-1?
-------
CALCULATIONS
X Tetradecane - (C14) TeCradecane Wt. * 100/(Sample Wt. + Tetradecane Wt.)
X Isopar-L - Area of Solv.peak * X Tetradecane/Area of Tetradecane C14 peak
MINIMUM FREQUENCY OF RUNNING QAPP ANALYSIS FOR SOLVENT ANALYSIS
FOR CARVER-GREENFIELD DEMONSTRATION
Sample Duplicate
Location ("per Test Run)
Feed Stock 1
Solvent (Fresh)
Slurried Feed Stock
Centrate 1
Centrifuge Cake 1
Condensed Water 1
Condensed Solvent 1
Solids Product 1
Vent Gas (GAC) 1
Distilled Solvent 1
Indigenous Oils 1
Trip Blanks
Field Blanks
Note: At least one external standard will be run each day.
QAPP LIMITS AND CORRECTIVE ACTION FOR SOLVENT ANALYSIS
FOR CARVER-GREENFIELD DEMONSTRATION
Matrix
Accuracy
X Recovery
Precision
(RPD)
Corrective Action
Slurry/Solids
Aqueous
75-125
60-150
30
50
Reanalyze the run. If reanalysis
yields acceptable results, only
those will be reported.
Otherwise report both sets of
data with a qualifying note
stating the nature of the
problem.
r 1 1
-------
APPENDIX D
QUALITY CONTROL/QUALITY ASSURANCE DATA
DI-A QA/QC Precision Results for Solvent Analysis
Dl-B QA/QC Accuracy Results for Solvent Analysis
DI-C QA/QC Precision Results for SOW Analysis
Dl-D QA/QC Accuracy Results for SOW Analysis
D2 General Testing Corporation
QA/QC Reports
-------
TABLE Dl-A: QA/QC PRECISION RESULTS FOR SOLVENT ANALYSIS
Sampling
Location
Sample
Number
Solvent in
Sample
<*)
Solvent in
Sample
Duplicate
(%)
RPD
Acceptable
RPD
Solvent
BR-2
101.93
108.14
5.91
50.00
Feedstock
BR-1
0.10U
0.10U
NC
30.00
Condensed Water
BR-1
0.10
0.10U
NC
50.00
Treated Solids
Cl-Cl
0.97
1.03
6.00
30.00
Treated Solids
CI-C3
0.92
0.93
1.08
30.00
Feedstock
Cl-At
0.10U
0.10U
NC
30.00
Treated Solids
C2-C3
1.12
1.08
3.64
30.00
Condensed Water
C1-C3
0.71
0.65
8.82
50.00
Condensed Solvent
CI-C3
87.87
88.86
1.12
50.00
Vent Gas (GAC)
C1-C3
5.25
7.27
32.27
30.00
Slurry
CI-A3
74.91
73.02
2.56
30.00
Slurry
CI-C8
91.61
87.40
4.70
30.00
Centrate
Cl-Al
89.30
90.00
0.78
30.00
Centrate
C1-C9
98.36
98.93
0.58
' 30.00
Centrifuge Cake
CI-A2
36.57
36.55
0.05
30.00
Centrifuge Cake
C1-C9
40.34
42.10
4.27
30.00
Slurry
C2-C9
91.95
92.66
0.77
30.00
Condensed Solvent
C2-C3
101.62
98.93
2.68
50.00
Condensed Water
C2-C3
0.10U
0.10U
NC
50.00
Vent Gas (GAC)
C2-C3
14,55
10.39
33.36
30.00
Centrifuge Cake
C2-C9
31.36
31.18
0.58
30.00
Centrate
C1-C3
104.33
102.85
1.43
30.00
Vent Gas (GAC)
CI-C3
4.68
7.25
43.08
30.00
Vent Gas (GAC)
C2-C3
12.50
8.54
37.64
30.00
Feedstock
C2-A6
0.10
0.10U
NC
30.00
D-I
-------
TABLE Dl-B: QA/QC ACCURACY RESULTS FOR SOLVENT ANALYSIS
Measured
Percentage
Solvent in
Acceptable
Date of
Solvent in
Standard
Percentage
Accuracy
Analysis
Standard
<*)
Recovery
(%)
08/06/91
4,83
4.82
99.79
75-125
08/06/91
2.44
2.37
97.13
75-125
08/06/91
1.07
1.06
99.07
75-125
08/06/91
0.60
0.62
103.33
75-125
08/06/91
0.32
0,33
103.13
75-125
08/07/91
4.83
4.88
101.04
75-125
08/08/91
1.07
1.07
100.00
75-125
08/09/91
2.44
2.40
98.36
75-125
08/12/91
1.07
1.08
100.93
75-125
08/14/91
2.44
2.41
98.77
75-125
08/15/91
0.60
0.63
105.00
75-125
08/16/91
1.07
1.07
100.00
75-125
08/19/91
0.60
0.62
103.33
75-125
08/20/91
1.07
1.07
100.00
75-125
08/22/91
0.60
0.62
103.33
75-125
08/23/91
0.60
0.62
103.33
75-125
08/26/91
2.44
2.41
98.77
75-125
08/27/91
0.60
0.62
103.33
75-125
08/28/91
0.32
0.34
106.25
75-125
. 08/29/91
2.44
2.40
98.36
75-125
09/03/91
0.60
0.64
106.67
75-125
09/04/91
2.44
2.41
98.77
75-125
09/05/91
0.60
0.63
105.00
75-125
09/06/91
0.32
0.34
106.25
75-125
09/09/91
0.60
0.63
105.00
75-125
09/10/91
0.60
0.64
106.67
75-125
09/11/91
2.44
2.41
98.77
75-125
09/12/91
0.32
0.34
106.25
75-125
09/13/91
0.32
0.35*
109.38
75-125
09/17/91
0.60
0.63
105.00
75-125
09/19/91
0.60
0.63
105.00
75-125
D-2
-------
TABLE D1 C. QAIQC PRECISION RESULTS FOR SOW ANALYSIS
Sample Location
Sample
Number
Solids
Water
Indigenous Oil
$am»le
<*>
Sample
Dupl.
<%)
RPD
Accept.
RPD
Sample
(*)
Sample
Dupl.
<%>
RPD
Accept.
RPD
Sample
<%)
Sample
Dupl.
<*)
RPD
Accept.
RPD
Treated Solidi
BR-2
81.39
88.84
0.51
1500
0.1 OU
O.lOU
NC
20 00
0 97
0.81
17.98
20.00
Treated Solidi
C1-C3
96 60
97 09
0.51
15.00
0.10U
0 IOU
NC
20 00
1.32
1 39
5,17
20.00
Treated Solidi
C1-C2
95-91
•97.38
1.52
15 00
0.I0U
O.lOU
NC
20 00
1.49
1 30
13.62
20.00
Treated Solidi
C2-C3
95 33
97.63
2.38
15.00
O.lOU
O.lOU
NC
20.00
0.68
0.81
17.45
20.00
Feedstock.
C2-A3
5268
51.21
2.83
15 00
34.07
31.27
8 57
20.00
7 04
7.47
5.93
20.00
Slurry
CI-AI
10,92
10.92
0.00
15.00
O.lOU
O.lOU
NC
20.00
9.77
8.73
11.24
20.00
Centrate
CI-AI
0.10U
0.1 OU
NC
15.00
O.lOU
O.lOU
NC
20.00
5.72
5 60
2.12
20.00
Centrifuge Cake
C1-B5
57.74
57.64
0 17
15.00
O.lOU
O.lOU
NC
20.00
2 76
2.78
0.72
20.00
Centrifuge Cake
C1-C9
57.89
57.92
005
15 00
0 IOU
0 IOU
NC
20 00
1 46
1.37
6.36
20 00
Cent rate
C2-AI
O.lOU
0.1 OU
NC
15 00
O.lOU
0 IOU
NC
20 00
7.59
7.96
4.76
20 00
Centrate
C2-C9
0.18
0.22
22.67
15.00
O.lOU
0 IOU
NC
20.00
0.25
0.29
14 29
20.00
Sluny
C2-A3
10.96
9.65
12.71
15.00
O.lOU
O.lOU
NC
20.00
6 04
6 52
764
20.00
Centrifuge Cake
C2-A3
68.92
67.48
2.11
15.00
O.lOU
O.lOU
NC
20.00
3.79
3,96
4.39
20.00
Centrifuge Cake
C2-C9
66.67
65.33
2.03
15.00
O.lOU
O.lOU
NC
20.00
1 OS
0.94
13 86
20.00
Centrate
C2-C9
0.12
0 13
8 33
15.00
O.lOU
O.lOU
NC
20 00
0.35
0 41
15.92
20.00
Scrubber Liquid
BR-I
0.10U
0.1 OU
NC
15.00
0 IOU
0 IOU
NC
20 00
0 IOU
0 IOU
NC
20.00
Feedstock
CI A4
52 70
52.29
0.78
IS 00
21 29
20.67
2.96
20,00
17.03
16 87
0.94
20 00
Centrifuge Cake
CI B4
57.23
57 53
0.52
15.00
O.lOU
O.lOU
NC
20.00
1 18
1 14
3 45
20 00
l)-3
-------
TABLE DI D QA/QC ACCURACY RESULTS FOR SOW ANALYSIS
Sundard Composition
Measured Composition
Percentage Recovery
Accept. Accuracy Limit*
Dale of
Analysis
Solid*
(*)
l»d Oil
<*)
Water
(*)
Solids
(%)
Ind. Oil
(%)
Water
(%)
Solids
(%)
Ind. Oil
(%)
Water
(*)
Solids
(%)
Ind. Oil
(%)
Water
(%)
08/06/91 .
87.25
2.81
9.94
87.25
2.36
9 25
100 00
84 15
93 10
95-103
74 118
88-117
08/07/91
85.08
3.73
11.19
85 04
3.39
10.26
99 96
91.00
9167
95-103
74-118
88-117
08/13/91
86.12
3.47
10.41
84 52
2.98
9.72
98 15
86.00
93 33
95-103
74-118
88-117
08/14/91
86 32
3.50
10.19
83.26
2.82
9 17
96.46
80 58
90.00
95-103
74-118
88-117
08/16/91
86.32
3 45
10,24
85.40
3.04
9.89
98.93
88.12
96 67
95 103
74-118
88-117
08/19/91
72.46
7.84
19.70
72 54
7 68
17.73
100.11
97.99
90.00
95 103
74-118
88-117
08/22/91
73 44
7.75
18.81
73.66
7.34
18 43
100.3!
94.66
98.00
95-103
74 118
88-117
08/23/91
80.58
6.92
12.50
79.13
6.38
11.67
98 19
92.17
93.33
95-103
74-118
88 117
08/27/91
83.61
4.48
11.90
81.98
4.40
ll.ll
98 05
98.23
93.33
95 103
74-118
88-117
09/03/91
76.24
3.96
19.80
74.97
3.80
19.80
98.34
96.00
100 00
95-103
74-118
88-117
09/04/91
75 08
4.19
20.73
73.09
3.23
18 66
97.35
77.23
90.00
95-103
74-118
88-117
09/05/91
77.88
3 63
18 50
76.25
3 44
17.02
97 91
94.90
92 00
95-103
74-118
88-117
09/06/91
75 31
4.48
20.20
74,38
3.64
18.59
98.77
81 08
92.00
95 103
74-118
88-117
09/10/91
76.49
3.92
19.59
75.67
3.84
18 81
98.92
98.00
96.00
95-103
74-118
88-117
09/11/91
79 13
3 82
17.OS
79.78
3 55
16 37
100 82
92 86
96.00
95-103
74-118
88-117
09/12/91
75.33
4.35
20.33
75.93
4.02
19 51
100 81
92.52
96 00
95 103
74 118
88-117
09/16/91
74.49
4.36
21 15
72.84
4 10
19 88
97 79
94.17
94.00
95 103
74-118
88-117
09/17/91
76.22
3 96
19 82
74.91
3.61
19 02
98 28
91.00
96 00
95-103
74-118
88 117
09/19/91
77.80
3.73
18 47
76 65
3.47
17.73
98 53
93.07
96.00
95 103
74-118
88-117
l)-4
-------
TABLE D-2: REPORT CROSS-REFERENCE OF SAMPLE JOB
NUMBERS AND SAMPLE DESCRIPTION
General Testing
Test Run
Job Number
Number
Sample Description
R91/03183
1
Feedstock
R91/03185
1
Centra te
R91/03186
1
Condensed Water
R91/03188
1
Condensed Solvent
• R91/03189
I
Treated Solids
R91/03268
2
Feedstock
R91/03270
2
Centrate
R91/03271
2
Condensed Water
R91/03273
2
Condensed Solvent
R91/03276
2
Treated Solids
D-5
-------
GIC LABORATORY QUALITY CONTROL REPORT
I II ORIGIHAL (DUPLICATE | X REL. I ACCEPT, 11 AVERAGE | SPIKE | PERCENT | ACCEPT. || NETHOO | SPUE | PERCENT | ACCEPT.|| REFERENCE | KNOWN | PERCENT | ACCEPT. |J
PARAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X)| RESULT |ADDED |RECOVERY| LIMIT X || BLANK | ADDED (RECOVERY)LIMITS X| | « | PMVAL |RECOVERY| LIMITS X |]
II — II II II ||
lUlllltlllllllllllW * PRECISION II * MATRIX SPIKING || BLANK SPIKES || REFERENCE STANDARD ||
II * II II II I ||
Aiunimm |-006 ||B780 (11,400 |26.0X |30 | |S/80 (37.9 |V 150-150 110.10 U |0.500 |100X (80-120 | | R E F STD |5.00 |101X |90-110 ||
I 11 —I I I II I I I 11 I I __l 11 I I I 11
Antimony |-Q06 ||5.0U |5.0 U |HC |SO ||5.0U |37.9 (40X++ |50-150 ||0.050 U (0.500 |99X |80-1Z0 | |REF STD |5.00 |100X (90-110 ||
: i 11 j i i ii i —i _i 11 -i i i 11 i i i 11
Arsenic |-006 ||5QU |50 U |NC |30 1150 U (379 |82X 150-150 ||0.50U [5.00 |90X |80-120 | |REF STD |5.00 |96X (90-110 ||
I II I I I II I I I II I I I II I I | ||
Bar i un |-0Q6 ||3130 |3080 |1.6X 130 ||3130 (37.9 |V (50-150 110.0050 U|0.500 |10JX |BO-120 | |REf SID |5.00 |101X |90-110 ||
I II I I I II I I I II I I I II I I I ||
Berylliun |-006 ||0.731 |0.742 |1,5X |30 ||0.731 |3.79 |95X (50-150 110.0050 U|0.050 |95X |80-120 | |REF STD |5.00 |100X (90-110 ||
I 11 I I I II I I I 11 -I _l I 11 I I I 11
Boron |-006 1120 U |20 U |NC |30 ||20u (3790 |64X (50-150 (|0.20U (50.0 |93X (80-120 | |R£f STD |5.00 (100X (90-110 ||
I 11 — I I I 11 I _l I 11 I I I 11 I I | 11
Cadniun |-006 ||0.545 |0.576 |5.5X (30 ||0.545 |3.7V |82X (50-150 ||0.0050 U|0.050 |94X |80-120 ||KEF STD |5.00 |100X |90-110 ||
I II I I I II I I I II I I I II I I I ||
Calciim |-006 (|2150 (2220 (I.2X |30 ||2150 (758 |106X |50-150 ||0.50U |2.00 1102% |8O-120 | |REF SID |50.0 |100X (90-110 ||
i ii i i i ii i: i i ii .i i i ii i i i ii
Chromiun |-006 (|24.0 |Z6.8 |11.0X |30 ||24.0 |18.9 |124X |50-150 ||0.010 U (0.250 |101X |80-120 ||REF STD |5.00 |101% (90-110 ||
I II I I I II I I I U I I I II I I I ||
obalt |-006 ||8.01 |6.73 |17.4X (30 ||8.01 118.9 |V2X (50-150 110.050 U |0.250 |95X |80-120 (|REF SID |5.00 (98% |90-110 ||
I II I I I II I I I II I I I II I I I J|
Copper (-006 ||!6.5 |16-2 (1.8X (30 ((16.5 |7.58 |108X (50-150 J|0.010 U |0.100 |101% (80-120 ||REF SID |5.00 |100X (90-110 ||
I 11 I I I II l_ I I 11 I I 1 11 I I I 11
Iron |-006 ||13.500 |13,300 |1.5X |30 1(13,500 |1.89 |V (50-150 (|0.050 U |0.250 |92X |fl0-120 ||REF STD |5.00 |100X |90 110 ||
I II 1 I I II I I I II I I 1 II J I I II
Lead |-006 ||45,7 |37.9 |18.7X (30 ||45.7 (18.9 |84X (50-150 110.050 U |0.250 |106X 100-120 ||REF SIO |5.00 (101X |90-110 ||
.1 ll__ I I I II I I I II I I 1 II I I I II
Analytical results previous to accounting tor dilutions. ** Reference Check samples ore not available for all analyses. Outside of Quality Control Limits,
O
o
CD
-------
-------
GTC LABORATORY QUALITY CONTROL REPORT
•TOMER: HydroQual, Inc.
JOB i : R91/03183
UNITS: ug/g Wet Wt.
REPORT TYPE: Site
1
>ARAME1ER | SAMPLE
|| ORIGINAL|OUPLICATE| % REL.
|| RESULT | RESULT | ERROR
(ACCEPT.
(LIMIT X
|(AVERAGE
|| RESULT
|SPIKE ( PERCENT|
|ADDED |RECOVERY|
ACCEPT.
LIMIT X
|| METHOO
|| BLANK
| SPIKE
| A0DED
| PERCENT I ACCEPT.|( REFERENCE | KNOWN
|RECOVERY|LIM1TS X|| U | PMVAL
| PERCENT] ACCEPT. |
|RECOVERY| LIMITS X |
iiiimiiiiimimw
• PRECISION
II
* MATRIX SPIKING
BIANI
SPIKES
II REFERENCE STANDARD
lagnesitm |
i
-006
||1360
li
|1620
1
|17.4X
1
|30
I
||1360
II
1758
1
1140%
1
|50-150
1
||0.50 U
II
(2.00
1
|102X
1
|80-120
1
||REF SID
II
(50.0
1
|100X
I
(90-110 (
1 1
Manganese |
1
-006
||450
II
|342
1
|27.3%
1
|3Q
1
||450
II
J3.79
1
l«
1
|50-150
1
||0.0050 U
II
|0.050
[94X
1
|80-120
1
(|REF SID
II
(5.00
1
(100X
1
|90-110 (
1 I
et. Hydro | - 006
1
|| 144,000
II
[141,000
1
|2.10%
1
(18.11
1
1(143,000 |31,443 |V
II 1 1
(55.9-130||10 U
1 II
(1998
|98.3X
1
(61.1-123||
1 II
1
1
1
1 1
1 1
Analyt ical
results
previous
to accounting for dilutions.
** Reference Check samples are not availab
le for all analyses. »+
Outside of
QuqIity Control
L imics.
Currently no limits established.
Suspect Matrix Inter
O
O
O
I)-7
-------
General
T^Qtinn \ A Fu" Service Environmental Laboratory
Corporation
HSL VOLATILE ORGANICS - SOIL SAMPLE
SOIL VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03183 -006
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENTRATION
CONCENT.
%
LIMITS
COMPOUND
(ug/kg)
(ug/kg)
(ug/kg)
REC #
REC.
1,1-Dichloroethene
12,500
0.0
11,700
94%
D-234
Trichloroethene
12,500
0.0
11,600
93%
7 L-157
Benzene
12,500
0 . 0
11,900
95%
37-151
Toluene
12,500
0.0
12,700
102%
47-150
Chlorobenzene
12,500
0.0
12,600
101%
37-160
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/kg)
(ug/kg)
REC #
RPD *
RPD
REC.
1,1-Dichloroethene
12,500
11,400
91%
2 . 6%
30
D-234
Trichloroethene
12,500
11,900
95%
2.5%
30
71-157
Benzene
12,500
12,300
98%
3 . 3%
30
37-151
Toluene
12,500
12,500
100%
1.6%
30
47-150
Chlorobenzene
12,500
12,900
103%
2 . 3%
30
37-160
# Columns to be used to flag recovery and RPD values with ++.
++ = Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: ,0_ out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
COMMENTS:
page 1 of 1
D-8
a n n i o
-------
General
Testing vx?
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL BASE/NEUTRAL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03183 —006
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/kg)
(ug/kg)
(ug/kg)
REC . #
REC.
1,4 Dichlorobenzene
101,000
0.0
77,800
77%
20-124
N-Nitroso-Di-n-propylamine
96,300
0.0
68,400
71%
D-230
1,2,4-Trichlorobenzene
101,000
0.0
89,100
88%
44-142
Acenaphthene
87,000
0.0
54,300
62%
47-145
2,4-Dinitrotoluene
100,000
0.0
61,300
61%
39-139
Pyrene
95,000
0.0
59,000
62%
52-115
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/kg)
(ug/kg)
REC #
RPD #
RPD
REC.
1,4 Dichlorobenzene
101,000
76,800
76%
1.3%
30
2 0-12 4
N-Nitrsodi-n-propylamine
96,300
66,500
69%
2.9%
30
D-220
1,2,4-Trichlorobenzene
101,000
85,200
84%
4 . 6%
30
44-142
Acenaphthene
87,000
52,800
61%
1.6%
30
47-145
2,4-Dinitrotoluene
100,000
64,000
64%
4.8%
30
39-139
Pyrene
95,000
54,200
57%
8.4%
30
52-115
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 6 outside limits
Spike Recovery: 0 out of 12 outside limits
COMMENTS:
page 1 of 1
0-9
a n ^ i
-------
General
Testing
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL ACID EXTRACTABLE SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03183 -006
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/kg)
(ug/kg)
(ug/kg)
REC #
REC.
Phenol
203,000
0.0
158,000
78%
5-112
2-Chlorophenol
201,000
0.0
157,0C0
78%
23-134
4-chloro-3-methylphenol
201,000
0.0
190,000
94%
22-147
4-Nitrophenol
200,000
0.0
155,000
78%
D-132
Pentachlorophenol
200,000
0.0
203,000
102%
14-176
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/kg)
(ug/kg)
REC 4
RPD #
RPD
REC.
Phenol
203,000
155,000
76%
2 . 6%
30
5-112
2-Chlorophenol
201,000
155,000
Ilk
1.3%
30
23-134
4-Chloro-3-methylphenol
201,000
180,000
90%
4 . 4%
30
22-147
4-Nitrophenol
200,000
156,000
78%
0%
30
D-13 2
Pentachlorophenol
200,000
201,000
100%
1. 0%
30
14-176
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 5 outside limits
Spike Recovery: _0 out of 10 outside limits
COMMENTS:
page 1 of 1
D-LO
-------
GTC LABORATORY QUALITY CONTROL REPORT
ISTOMER: HydroQual, Inc. JOB « : R91/03185 UNITS: ug/g Uet Ut. REPORT TYPE:
1
PARAMETER | SAMPLE
1 ORIGINAL|DUPLICATE| X REL
| RESULT | RESULT | ERROR
. |ACCEPT.
|LIMIT X
|AVERAGE
| RESULT
|SPIKE | PERCENT|
|ADDED |RECOVERY|
ACCEPT. |
LIMIT X |
METHOD
BLANK
| SPIKE | PERCENT | ACCEPT.
| ADDED |RECOVERY|LINITS X
| REFERENCE | KNOWN
| # | PMVAL
| PERCENT| ACCEPT. |
|RECOVERY| LIMITS X |
'///////////////////
1
1
* PRECISION
* MATRIX SPIKING
1
BLANK
SPIKES
1
| REFERENCE STANDARD
Magnesium |-009
1
1 SO U
1
|50 U
1
| NC
1
130
1
|50 U
|990
1
|94X
I
50-150 |
1
0.50 U
2.00
90X
|80-120
1
|RE F STD
1
| SO. 0
|98X
I
|90-110 I
1 1
Manganese |-009
1
13.83
1
13.86
1
|0.8X
1
130
1
|3.83
14.95
1
194X
I
50-150 |
I
0.0050 U
0.050
95X
|80-120
1
|REF STD
1
15.00
1
1103%
I
|90-110 |
1 1
Molytodenum|-009
1
|5.0 U
1
|5.0 U
1
| NC
1
130
1
15.0 U
1124
1
1102%
1
50-150 |
I
0.050 U
1.250
104X
|80-120
I
|RE F STD
1
15.00
1
1100X
1
|90-110 |
I I
Nickel |-009
1
|2.60
(2.0 U
| NC
130
1
|2.60
119.8
I
1112%
1
50-150 |
0.020 U
0.200
126X
|80-120
I
|RE F SPK
1
| S. 00
1
196%
I
|90-110 |
I I
Potassiun |-009
|S0 U
1
150 U
1
|NC
1
130
1
|S0 U
1952
I
|94%
1
50-150 |
I
50 U
3520
99X
|80-120
I
|REF STD
1
| SO. 0
1
1101%
1
|90-110 |
I I
Seleniun |-009
|50 U
1
| so u
1
|NC
1
130
1
|S0 U
1495
I
|87X
1
50-150 |
I
0.500 U
5.00
98X
|80-120
I
|REF STD
1
|5.00
1
1101%
1
|90-110 |
1 1
Sodiun | -009
|so u
1
| so u
1
| NC
1
130
1
150 U
1990
I
1103%
1
50-150 |
1
0.50 U
2.00
126X
|80-120
1
|REF STD
1
150.0
1100%
I
|90-110 |
I I
Stront iun |-009
1
|5.0 U
1
|S.O u
1
| NC
1
130
1
|S.0 U
149.5
f
|95X
1
50-150 |
I
0.050 U
0.500
100X
|80-120
1
|REF STD
1
| S. 00
1100%
I
|90-110 |
1 1
lhalI inn |-009
1
15.0 U
1
|S.O u
1
| NC
1
130
1
|5.0 U
1124
1
|87X
1
50-150 |
1
0.050 U
1.250
96X
|80-120
I
|RE F STD
1
15.00
1
1100%
I
|90-110 |
I I
Viinadiixn |-009
|5.0 U
1
|5.0 U
1
|NC
1
130
1
| S. 0 U
1124
I
1106X
I
50-150 |
I
0.050 U
1.250
102X
|80-120
1
|RE F STO
1
| S. 00
1
1100%
I
190-110 |
1 1
Zinc |-009
1
|2.54
11.88
I
|29X
1
130
1
|2.54
14.95
I
1112%
1
50-150 |
1
1.00 U
298
91X
|80-120
I
|REF STD
1
11.00
1
1101%
1
|90-110 |
1 1
1 II 1 1 1 II 1 1 1 II 1 1 1 II III |
1 II 1 1 III II 1 II II 1 II II 1 1
Analytical results
previous
to accounting for
di lut ions.
** Reference
Check samp
es are not availab
e for all analyses. ~~
Outside of
Quality Control
L imits.
~ Currently no limits established. Suspect Matrix Inter
D
5
-------
GTC LABORATORY QUALITY CONTROL REPORT
TOMER: HydroGual, Inc.
JOB # : R91/03185
UNITS: ug/g Uct Ut.
REPORT TYPE:
| || ORIGINAL(DUPLICATE| X BEL. (ACCEPT.
ARAMETER | SAMPLE (| RESULT | RESULT | ERIK* (LIMIT X
(AVERAGE (SPIKE | PERCENT| ACCEPT.
I RESULT IADDED (RECOVER*| LIMIT X
| METHOO | SPIKE ( PERCENT| ACCEPT.|| REFERENCE | KNOWN | PERCENT) ACCEPT.
I BLANK I ADDED |RECOVERY|LIMIIS X|| # ( PMVAL (RECOVERY( LIMITS X
//////////////////I
* PRECISION
* MATRIX SPIKING
BLANK SPIKES
REFERENCE STANDARD
II-
iluninut
(-009
1
((lOOJm
II
1101 Jm
1
J1.0X
1
|30
1
||100Jm
II
|47.6
1
1128%
1
|50-150
1
||10.0U 19510
II 1
[ 123X
1
|80-120
I
|(REF STD
|5.00
I
|103X
1
|90-110
1
int i atony
|-009
1
||5.QU
II
(5.0 U
1
|NC
1
|30
1
||5.0 U
II
J49.5
1
1
X
|50-150
1
||0.050 U (0.500
II 1
(106%
1
[80-120
1
|(REF STD
II
15.00
I
1100X
1
|90-110
1
.rsenic
(-009
1
1150 U
II
(50 0
1
|NC
1
|30
1
1|50 U
II
(495
1
jaax
l
|50-150
I
|(0.500 U |S.00
II 1
|99X
1
[80-120
1
|J RE F STO
II
15.00
I
|100X
1
|90-110
1
iartun
|*009
L
1113-9
II
(13.9
I
|O.OX
1
|30
1
||13.9
II
(49.5
1
|98X
1
|50-150
1
(|0.0050 U|0.500
II 1
(104X
I
[80-120
1
([REF SID
II
15.00
1
|100X
1
(90-110
1
lerylliu* (-009
1
||0.50 U
II
(0.50 U
I
|NC
1
|30
1
||0.S0 U
|4.95
1
|94X
1
|50-150
1
||0.0050 U|0.050
II 1
1102X
[80-120
[|REF STD
II
|5.00
1
(100%
I
|90-110
1
lor on
|-009
1
1120 U
II
120 u
I
|NC
1
|30
1
1120 u
II
14950
1
1 .
- 1 2
-------
General
Testing ^ A Fu" Service Environmental Laboratory
Corporation
HSL VOLATILE ORGANICS - AQUEOUS SAMPLE
WATER VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03186 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENTRATION
CONCENT.
%
LIMITS
COMPOUND
(ug/1)
(ug/1)
(ug/1)
REC #
REC.
1,1-Dichloroethene
2500
0.0
2730
109%
D-234
Trichloroethene
2500
0.0
2850
114%
71-157
Benzene
2500
0.0
2900
116%
37-151
Toluene
2500
0.0
3130
125%
47-150
Chlorobenzene
2500
0.0
3010
120%
37-160
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/1)
(ug/1)
REC #
RPD #
RPD
REC.
1,1-Dichloroethene
2500
2910
116%
6.4%
30
D-234
Trichloroethene
2500
2960
118%
3.8%
30
71-157
Benzene
2500
2940
118%
1.4%
30
37-151
Toluene
2500
3067
123%
2.0%
30
47-150
Chlorobenzene
2500
3031
121%
0.7%
30
37-160
# columns to be used to flag recovery and RPD values with '++.
++ = Values outside of QC limits
MS QC Limits » EPA Acceptance criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
COMMENTS:
page 1 of 1
D-13
00056
-------
CTC LABORATORY QUALITY CONTROL REPORT
| || ORIGINAL[DUPLICATE| X REL. |ACCEPT.||ORICINAL|SPIKE | PERCENT| ACCEPT. || HETMOO | SPIKE | PERCENT| ACCEPT.|| REFERENCE | KNOWN | PERCENT| ACCEPT. ||
PARAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X|| RESULT |ADD£0 |RECOVERY| LIMIT X || BLANK | ADDED |RECOVERY jLlMITS X|| « | PMVAL |RECOVERY| LIMITS % ||
- ii - - ii ii - ----- II - - v ||
lUllltltllintllllt II * PRECISION II • MATRIX SPIKING || BLANK SPIKES || REFERENCE STANDARD |[
-II- "II — — II II - ||
Vanadiun |-003 110.050 U |0.050 U |NC |30 110.050 U |1.25 |100X |80-120 ||O.OSO U 11.250 |102X |80-120 11REf SID |5.00 |10QX |90-110 ||
I 11 I : 1 -I 11 I I I. 11 I I I I I I I | ||
Zinc J-003 ||0.m (0.174 |11X |20 JJ0.194 J0.D5G0 |62X« 180-120 110.010 U (0.050 (10QX |80-12Q ||REFSTD |1.00 |10!X J90-110 ||
I 11 I 1. 1 -I I I I I 11 I l_ I 11 I I | 11
I II I I I II I I I II I I I II ill ||
I II I I I II I I I II I I I II I I | ||
I II I I I II I I I II I I I II III ||
I II I I I II I I I II I I I II ,| | | ||
I II I I I II I I I II I I I II III ||
I 11 I i I 11 I I I 11 I I I 11 _l | | 11
I II I I I II I I I II I I I II III II
I II I I I II I I I II I I I _|| I | __| ||
I II I I I II I I I II I I I II III ]|
I 11 I I I 11 I I I 11 I I I 11 __| |__ | j |
I II I I I II I I I II I I I II III II
. -I II I I I II I I I II I I I II I | | H
I II I I I II I I I II I I I II III ||
I II I I I II I I I II I I I II I | | ||
I II I I I II I I I II I I I II III II
I II I I I II I I I II I I I I! I | | ||
I II I I I II I I I II I I I II III II
I II I I I II I I I II I I I II _| | | ||
I II I • I I II I I I II I I I II III II
I II I I I II I I I II 1 I I II III ||
I II I I 1 -II I I I II I I 1 _ll_ I | I; ||
I II I I I II I I I II I I I II III II
I II I I I II I I I II I I I II I I | ||
I II I I I II I I I II I I I II I I I If
I II I I I II I I I || I I I II III It
. ..I. II I I —I II I I I II I __l I II I I | II
D- 1 A
-------
GTC LABORATORY QUALITY CONTROL REPORT
.TOMER: HydroQual, Inc.
JOB * : R91/03186
UNITS: mg/
ARAMETER
1
| SAMPLE
| ORIGINAL|DUPLICATE
| RESULT | RESULT
X REL.
ERROR
|ACCEPT.|
(LIMIT X|
| AVERAGE
| RESULT
|SPIKE | PERCENT|
|ADDED |RECOVERY|
ACCEPT.
LIMIT X
| METMOO
| BLANK
SPIKE
ADDED
PERCENT
RECOVERY
ACCEPT.
LIMITS X
| REFERENCE
( #
| KNOUN
| PMVAL
| PERCENT| ACCEPT.
(RECOVERY| LIMITS X
//////////////////
* PRECISION
• MATRIX
SPIKING
I
BLANK
SPIKES
REFERENCE STANDARD
:a<*nlum
|-003
1
|0.0050 U
|0.0050 U
NC
130 |
1 1
|0.0050 U
|0.0500
94X
80-120
|0.0050 U
I
0.050
94X
80-120
(REF
STD
(5.00
(100X
|90-110
1
alcicn
| -003
1
|4.18
|4.46
6.5X
120 |
1 1
(A. IS
110.0
65X++
80-120
10.50 U
I
2.00
102X
80-120
| RE F
STD
150.0
(100X
|90-110
1
hromiun
|-003
1
|0.0109
(0.010 u
NC
130 |
1 1
|0.0109
|0.250
88X
80-120
(0.010 U
1
0.250
B&X
80-120
| REF
STD
15.00
|101X
(90-110
1
:obalt
|-003
1
(0.050 U
(0.050 U
NC
130 |
1 1
|0.050 U
|0.250
96X
80-120
|0.050 U
1
0.250
95X
80-120
(REF
STD
15.00
|98X
|90-110
1
:opper
|-003
1
|0.010 U
(o.oio u
NC
(30 |
1 1
(0.010 u
(0.100
104X
80-120
(0.010 U
1
0.100
101X
80-120
| REF
STD
15.00
1100X
J 90-110
1
ron
|-003
1
11.82
(2.00
9.4X
130 |
1 1
11.82
|0.250
V
80-120
|0.050 U
1
0.250
93X
80-120
(REF
STD
(5.00
1100X
|90-110
1
ead
|-003
1
|0.050 U
|0.050 U
NC
130 |
1 1
|0.050 U
|0.250
102X
80-120
|0.050 U
1
0.250
106X
80-120
| REF
STD
(5.00
(101X
|90-110
I
lagnesiun
|-003
1
|0.915
11.24
30X
130 |
1 1
|0.915
110.0
60X++
80-120
(0.50 U
1
2.00
102X
80-120
| REF
STD
150.0
|100X
|90-110
I
langanese
|-003
1
(0.0894
|0.0929
3.8X
120 |
1 1
|0.0894
|0.0500
97X
80-120
|0.0050 U
1
0.050
94X
80-120
| REF
STO
15.00
1100X
|90-110
I
1o I ytxjcnum | - 003
1
|0.050 U
|0.050 U
NC
130 |
1 1
|0.050 U
11.25
94X
80-120
|0.050 U
1
1.250
95X
80-120
(REF
STD
15.00
|98X
(90-110
1
1 i eke I
|-003
1
(0.0432
|0.020 U
NC
130 |
1 1
|0.0432
|0.200
82X
80-120
|0.020 U
1
0.200
100X
80-120
| REF
STD
15.00
1100X
|90-110
1
'otassiun
|-003
1
|0.50 U
|0.50 U
NC
130 |
|0.50 U
|10.0
103X
80-120
10.50 U
1
2.00
116X
80-120
(REF
STD
|50.0
1100X
(90-110
I
;cIonium
|-003
1
|0.50 U
|0.50 U
NC
130 |
1 1
(0.50 U
15.00
87X
80-120
|0.50 U
5.00
89X
80-120
(REF
STD
15.00
|98X
|90-110
1
iodium
|-003
1
12.70
|4.53
5U"
120 |
1 1
\2.70
(10.0
128X«*
80-120
|0.50 U
1
2.00
112*
80-120
| RE F
SID
150.0
1101X
|90-110
I
itront iun
|-003
1
|0.0556
|0.0600
7.6X
130 |
1 1
|0.0556
|0.500
98X
80-120
|0.050 U
1
0.500
98X
80-120
| RE F
SID
15.00
1100X
|90-110
1
lhal I lun
|-003
1
|0.050 U
(0.050 U
NC
(30 |
1 1
|0.050 U
11.25
98X
80-120
|0.050 U
1
1.250
104X
80-120
| RE F
SID
15.00
1100X
|80-120
REPORT TYPE: Job Specific
Analytical results previous to accounting for dilutions. ** Reference Check samples are not available for all analyses. ~~ Outside of Quality Control Limits.
n-i 5
-------
GTC LABORATORY QUALITY CONTROL REPORT
.TONER: HydroQual, Inc.
JOB # : R91/03186
UNITS: mg/t
REPORT TYPE: Job Specific
| || ORIGINAL(DUPLICATE| X REt. |ACCEPT.
¦ARAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X
(AVERAGE |SPIKE | PERCENT| ACCEPT. || METHCO | SPIKE | PERCENT| ACCEPT.|| REFERENCE | KNOWN | PERCENT| ACCEPT. ||
| RESULT IADDED |RECOVERY| LIMIT X || BLANK | ADDED (RECOVERY|LIMITS X|| * | PMVAL (RECOVERY| LIMITS X ||
- ii
iiiiiiiihuiiiiiiiW
• PRECISION
"II
* MATRIX SPIKING
•II
II
BLANK SPIKES
"II
|| REFERENCE
STANDARD
"II
I!
>H 13575-1
I
II
J(?.1Z
II
(7.12
|0.0X
1
!*~
I
I|7.12
II
|NA
1
I
I
1
1
||NA
M
1
1
1
1
1
1
(|NA
II
1
1
1
1
1
1
II
II
II
Xcidity (-003
1
||36.0
II
(36.0
|0.0X
1
115
1
||36.0
II
|50.0
1
|96X
I
|78-122
1
||2.0 U
M
(100.0
1
|111X
1
|80-126
1
UN*
II
1
1
1
1
1
1
II
II
Ikalinity |-003
1
f(2.0 U
II
(2.0 U
|NC
1
|10
I
||2.0 U
II
|80.0
1
|81X
I
(82-126
I
112.0 U
II
(80.0
1
|98X
1
|88-123
1
| |R£F STD
II
(203
1
(102X
1
|90-115
1
II
II
100-5 Day |-003
I
||B4.0
II
(84.0
|O.OX
1
|17
1
||84.0
II
|NA
1
I
1
I
I
II"*
II
1
1
1
1
1
1
((REF STO
II
1200
|92X
1
|73-118
1
II
II
.00 (-003
1
||1230
II
|913
|30X**
1
(10
(
1(1230
II
|5Q0
1
(50X**
1
|79-116
1
||100 u
II
(500
1
1100X
1
|87-115
1
(|REF STD
(500
1
|105X
1
|90-119
1
II
\nmonia (-003
1
((0.050 U
II
|0.050 U
(HC
1
(10
I
1(0.050 U (0.500
II 1
(104X
1
|65-128
1
1(0.050 U (0.250
II 1
|!00X
1
|79-130
I
((REF STD
|1.80
1
(102X
1
(90-110
1
II
TKN (-003
1
||0.37V
II
(0.338
(11X
1
(20
(
||0.379
II
|2.00
1
(92X
1
|50-150
1
||0.20 U
II
(1.00
1
} 102%
1
|70-128
1
||REF STD
II
|4.00
1
(102X
1
(81-117
1
II
II
)lids, Sus(-003
1
((76.5
II
|NA
1
1
1
I
||76.5
II
|NA
1
1
1
1
1
||NA
II
1
1
1
1
1
1
||REF STD
II
|39.4
1
(104X
I
|75-114
1
II
II
Sulfate |-003
1
||10.0 U
(10.0 U
|NC
1
|10
I
II10.0 u
II
|21.0
I
(109X
1
|69-130
I
||10.0 u
II
[20.0
1
|9BX
1
|79-116
1
| |REF STD
II
[138
1
|96X
I
|77-114
1
II
.•t. Hydro. (-003
1
||2090
II
(2050
|1.9X
I
I**
I
111250
II
(1998
I"
|v
1
!*~
I
((0.10 u
II
(1998
1
|B5.6
1
(58.7-116||
1
I
1
1
1
II
Uuninum (-003
1
H1.66
II
(3.35
|68%**
I
(20
(
(|1.66
II
|0.500
I
(424X++
1
|80-120
1
||0.10 u
II
|0.500 U|100X
1 1
(80-120
I
(|REF STO
II
(5.00
I
|101X
I
(90-110
1
II
II
\ntimony |-003
|
||0.050 U
II
(0.050 U
|NC
I
130
I
||0.050 U |0.500
II 1
(96%
1
180-120
1
||0.050 U |0.500
II 1
(99X
1
|80-120
1
| [REF STD
N
(5.00
1
|100X
I
|90-110
1
II
II
\rsenic |-003
1
||0.050 U
II
|0.050 U
(NC
I
130
I
||0.050 U |0.500
II 1
(96X
1
|80-120
1
||0.050 U (0.500
II 1
|99X
1
(80-120
1
||REF STO
II
|5.00
1100X
i
|90-110
1
II
II
Jariun |-003
1
((0.0354
II
|0.0392
|10X
I
120
I
||0.0354
|0.500
I
(102%
1
180-120
1
||0.0050 U|0.500
II 1
1103X
1
|80-120
I
||REF STO
(5.00
1
1101*
1
|90-110
1
II
Berylliun (-003
1
1(0.0050 U
|0.0050 U
|NC
I
130
I
1(0.0050 U|0.0500 (96%
II 1 1
|80-120
I
||0.0050 U|0.050
II 1
|95%
1.
(00-120
1
| |REF STO
II
|5.00
1
|100X
1
(90-110
1
II
II
Boron |-003
I
| [0.20 U
10.20 U
| MC
I
(30
I
|(0.20 U
(50.0
I
(92%
1
(80-120
1
(|0.2Q U
II
|5Q.0
.1.
(93%
1
(80-120
1
| |REF STD
II
| S. 00
1
(100%
1
(90-110
I
II
II
Analytical results previous to accounting for dilutions.
Reference Check samples ore not available for all analyses. ~~ Outside of Quality Control Limits.
D- 1 6
-------
A Full Service Environmental Laboratory
SEMI-VOLATILE - WATER SAMPLE
WATER BASE/NEUTRAL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03186 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC.
1,4 Dichlorobenzene
101
0.0
V
20-124
N-Nitroso-Di-n-propylamine
96. 3
0.0
V
D-230
1,2,4-Trichlorobenzene
101
0.0
V
44-142
Acenaphthene
87. 0
0.0
V
47-145
2,4-Dinitrotoluene
100
0.0
V
39-139
Pyrene
95.0
0.0
V
52-115
Genera/^
Testing
Corporation
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC
LIMITS
COMPOUND
(ug/i)
(ug/1)
REC #
RPD #
RPD
REC.
1,4 Dichlorobenzene
30
20-124
N-Nitroso-Di-n-propylamine
30
D-230
1,2,4-Trichlorobenzene
30
44-142
Acenaphthene
30
47-145
2,4-Dinitrotoluene
30
39-139
Pyrene
30
52-115
# - Columns to be used to flag recovery and
RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of . 6 outside limits
Spike Recovery: 0 out of 12 outside limits
COMMENTS:
page 2 of 2
D-17
-------
General
Testing
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - WATER SAMPLE
WATER ACID EXTRACTABLE SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03186 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC.
Phenol
203
0.0
V
5-112
2-Chlorophenol
201
0.0
V
23-134
4-Chloro-3-methylphenol
201
0.0
V
22-147
4-Nitrophenol
200
0.0
V
D-132
Pentachlorophenol
200
0.0
V
14-176
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC
LIMITS
COMPOUND
(ug/L)
(ug/1)
REC #
RPD #
RPD
REC.
Phenol
30
5-112
2-Chlorophenol
30
23-134
4-Chloro-3-methylphenol
30
22-147
4-Nitrophenol
30
D-132
Pentachlorophenol
30
14-176
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
COMMENTS:
page 1 of 2
n-1 s
000 5 9
-------
CTC LABORATORY QUALITY CONTROL REPORT
STOKER: HydroQual, Inc.
JOB # : R9J/031M
UNITS: ug/9 Wet Wt.
REPORT TYPE: Job Specific
I II OR1GINAL|0UPLICATE| X REL. (ACCEPT.
PARAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X
| AVERAGE [SPIKE | PERCENT | ACCEPT. || METHOD | SPUE | PERCENT | ACCEPT.|| REFERENCE | KNOWN | PERCENT) ACCEPT.
| RESULT |ADDED |RECOVERY| LIMIT X || BLANK | ADDED |RECOVERY(LIMITS X|| » | PMVAL (RECOVERY| LIMITS X
///////////////////11
PRECISION
MATRIX SPIKING
BLANK SPIKES
REFERENCE STANDARD
-II-
Pet Hydroi -001 "966,000 '863,000 '11-3*
11 897,00q!52,405 Iq.13S
.11 I I
.11.
MA
Una
Magnesiun
(-001
1
((50 U
II
(50 u
1
| HC
1
(30
1
||50 U
II
|9?1
1
|92%
1
(50-150
1
J(0.50 U
|2.00
I
|90X
1
(80-120
I
I(RET STD
II
|50.0
1
(98X
1
190-110
1
Manganese
(-001
1
||0.50 u
II
|0.50 U
1
| NC
1
|30
1
(|0.50 U
II
(4.85
1
|94X
1
|50-150
1
H0.0050 uJ0.050
II 1
|95X
1
(80-120
1
|)REF STD
II
(5.00
1
1101%
1
(90-110
1
Molybdenum]-001
1
||5.0 U
II
15-0 U
1
| NC
1
130
1
||5.0 U
II
1121
1
1102X
1
|50-150
1
||0.050 U
M
11.250
1
1104X
1
|80-120
1
| |R£F STD
II
|5.00
1
j 100%
1
|90-110
1
Nickel
(-001
I
||2.0 U
II
12.0 U
1
| NC
1
(30
1
||2.0 U
II
|19.4
I
(96X
1
|50-150
1
||0.020 U
II
|0.200
1
1126X
1
|80-120
I
||REF STD
II
J5.00
1
|95X
1
|90-110
1
Potassium
|-001
1
1150 U
II
|50 U
1
| NC
1
(30
1
||50 U
II
|971
1
|96X
1
|50-150
1
||50 U
II
|3520
1
|99X
1
(80-120
1
| |REF STD
II
(50.0
1
|99X
1
|90-110
1
Seleniun
|-001
I
||50 U
II
|50 U
1
[NC
1 '
130
1
1150 U
II
|485
1
(95X
1
(50-150
1
||0.500 U
II
(5.00
1
|98X
J
|00-120
1
) |REF SID
II
|5.00
1
(101X
1
(90-110
1
Sodium
I-001
1
|(50 U
II
150 U
1
| NC
1
130
1
||50 u
II
|971
1
(104X
I
|50-150
1
|(0.50 U
II
12-00
1
|126X
1
(80-120
1
)|REK STD
|50.0
1
)100X
1
|90-110
1
Strontium
1-001
I
||5.0 U
II
15.0 U
1
| NC
1
|30
1
||5.0 U
II
[48.5
1
199%
I
|50-150
1
||0.050 U
|l
(0.500
1
(100X
1
|80-120
1
|(REF STD
II
(5.00
1
|1Q0X
I
|90-110
1
Thai I iun
|-001
I
||5.0 U
II
15.0 U
1
| NC
1
|30
1
||5.0 U
II
1121
1
|95X
I
(50-150
1
||0.050 U
II
|1.250
1
|96X
1
|80-120
1
||REF SID
II
J 5.00
1
1100%
1
|90-110
1
Vanadium
I-001
1
||5.0 U
II
|5.0 U
1
| NC
1
|3Q
1
115-0 U
II
1121
1
1104X
1
(50-150
I
||0.050 U
II
|1.250
I
1102X
I
(80-120
1
|(REF STD
II
(5.00
1
1100%
1
|90-110
1
I inc
|-001
||1.0 U
(1.0 u
(NC
(30
||1.0 U
|4.85
(103%
|50-150
||1.00 U
1298
|91X
|80-120
((REF SID
) 1.00
(98%
(90-110
Analytical results previous to accounting for dilutions.
> Currently no limits established.
Reference Check samples are not available for all analyses. ~ ~ Outside of Quality Control Limits.
Suspect Matrix Inter
II
.11
II
.11
.11
II
J I
O
o>
-»
D- I 9
-------
I II ORIGINAL(DUPLICATE| X REL. |ACCEPT.||AVERAGE (SPIKE | PERCENT( ACCEPT. || METHOD | SPIKE | PERCENT| ACCEPT.|| REFERENCE [ KNOUN | PERCENT| ACCEPT. ||
'ARAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X|( RESULT |ADDED |RECOVERY| LIMIT X || BLANK | ADDED |RECOVERY|LIMITS X|| # | PMVAL (RECOVERY| LIMITS X ||
GTC LABORATORY QUALITY CONTROL REPORT
'//////////////////1 | * PRECISION || * MATRIX SPIKING || BLANK SPIKES || REFERENCE STANDARD ||
II -II- II II II
Uunlnum |-001 ||11.1 113.0 |16X |30 ||11.1 J48.5 |101X (50-1S0 ((10.0 U |951Q (123X 180-120 ||REF STD |5.00 |100X (90-110 (|
_l 11 I I I- 11 I I I 11 I I I 11 I I _| 11
\ntimony |-001 ||5.0U |5.0 U |NC (30 ||5.0U |48.5 |1Q3% (50-150 ||0.050 U |0.500 |1Q6X (80-120 ||REF STD (5,00 |100X (90-110 ||
I 11 -_l I I 11 I I I 11 I I I 11 I I I ((
Arsenic |-001 ||50U |50 U |NC (30 ||50U |485 |95X (50-150 ((0.500 U (S.00 ( 99X |B0-120 | |REF STD |5.00 (100X (90-110 ||
I ll_ l_ I I II- I I I II I I I II I I I |(
iariuti |-001 ||0.50 U |0.50 U |NC (30 ||0.50U |48.5 |99X (50-150 110.0050 U|0.500 (104X (80-120 | |REF SID (5.00 |100X (90-110 ||
I II I I I II I I I II I I I II I !_ I II
lerylliun |-001 |[0.50 U (0.50 U |NC (30 ((0.50 U |4.85 |98X (50-150 |(0.0050 U|0.050 |102X (80-120 |(REFSID (5.00 |100X (90-110 ||
I 11 I I I 11 I I I 11 I I I 11 I __l I 11
ioron (-001 ||2Q U (20 U (NC |30 ||20U (4850 (94% (50-150 |(0.200 U (50.0 (94X (80-120 (|REf SID (5.00 (100X (90-110 ||
I II I l_ I _ll I I I II I I L II I I i (I
^admiun (-001 ((0.50 U |0.50 U (NC |30 ((0.50 U (4.85 (82X (50-150 ||0.0050 U|0.050 |89X |80-120 ||REfS!D (5.00 (96X (90-110 ||
I ji I I I 11 I i i 11 i I i 11 I i i 11
:alciun |-001 ((50 U (SO U (NC |30 ((50 0 (971 |102% (50-150 ((0.50 U (2.00 |100X |80-120 | (REF STD (50.0 |10QX (90-110 |(
I II I I I II I I I II I I- I II _l I I (I
hromium |-001 ||1.0U (1.0 U (NC (30 ||1.0U (24.3 [68% (50-150 ((0.010 U (0.250 |92X (80-120 ||REF STD (S.00 |98X (90-110 (|
I II I I I II I I I II I I I II I I |_ (I
>balt (-001 ||5.0 U (5.0 U |NC (30 ||5.0U (24.3 (101% (50-150 ||D.050 U (0.250 (102X (80-120 |(REF STD (5.00 (100% |90-110 ||
I II I I I II I I I II I I I II I I I II
:opper I-001 1(1.0 U (1.0 U |NC (30 |(t.0 U (9.71 |93X (50-150 ((0.010 U (0.100 |100X |80-120 |(REF STD |5.00 (100X (90-110 ||
I II —I I I II I I I H I I 1 II I I |_ II
iron |-001 ||5.0 U (5.0 U (NC (30 ||5.0 U |24.5 (104% (50-150 ||0.050 U (0.250 |100X (SO-120 ||REF STD (5.00 |100X (90-110 ||
I II I l__ I II I I I -II I I I II -I I I II
ead |-001 ||5.0 U |5.0 U (NC |30 ((5.0 U |24.3 |102% (50 150 ((0.050 U (0.250 |97X (80-120 ||REFSI0 (5.00 (101% (90-110 ||
I II I I I II I I I II I I I II I I I II
.Analytical results previous lo accounting for dilutions. ** Reference Check samples are not available for oil analyses. Outside of Quality Control Limits,
J
I
-------
General
Testing
Corporation
HSL VOLATILE ORGANICS - SOIL SAMPLE
SOIL VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name; General Testing Corp.
Matrix Spike - Sample No. : R91/03189 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENTRATION
CONCENT.
%
LIMITS
COMPOUND
(ug/kg)
(ug/kg)
(ug/kg)
REC #
REC.
1,1-Dichloroethene
1,250,000
0.0
1,300,000
104%
D-234
Trichloroethene
1,250,000
0.0
1,040,000
83%
71-157
Benzene
1,250,000
0.0
1,120,000
90%
37-151
Toluene
1,250,000
0.0
1,120,000
90%
47-150
Chlorobenzene
1,250,000
0.0
1,190,000
95%
37-160
SPIKE
MSD
MSD
ADDED
CONCENT.
.%
%
QC LIMITS
COMPOUND
(ug/kg)
(ug/kg)
REC #
RPD #
RPD
REC.
1,1-Dichloroethene
1,250,000
1,430,000
114%
9.5%
30
D-234
Trichloroethene
1,250,000
1,160,000
93%
11%
30
71-157
Benzene
1,250,000
1,320,000
106%
16%
30
37-151
Toluene
1,250,000
1,260,000
101%
12%
30
47-150
Chlorobenzene
1,250,000
1,240,000
99%
4 • 1%
30
37-160
# Columns to be used to flag recovery and RPD values with ++.
++ = Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
.COMMENTS: •
jage ^ of *
D-21
-------
I
GTC LABORATORY QUALITY CONTROL REPORT
is TOMER: HydroOuat,
Inc.
JOS # :
R91/031B9
UNITS: ug/o Wet Wt.
REPORT TYPE: Job Specific
I
PARAMETER | SAMPLE
II ORIGINAL)DUPLICATE! XREl. (ACCEPT. 11 AVERAGE |SPIKE | PERCENT | ACCEPT.
|| RESULT | RESULT j ERROR (LIMIT Xj j RESULT (RODEO |REC0VERY| LIMIT X
METHOD | SPIKE ( PERCENT) ACCEPT.
BLANK | ADOED (RECQVERY|L1NIT$ X
REFERENCE
#
| KNOWN | PERCENT! ACCEPT.
| PMVAL |RECOVERY( LIMITS X
///////////////////||
• PRECISION
II
• MATRIX SPIKING
¦LAN
K SPUES
REFERENCE STANDARD
Nagnesiua (-003
1
(12400
11
|2390
1
|0.4X
I
|30
I
||2400
II
(877
1
|147X~
1
(80-120
I
0.50 U |2.00
1
|90X
1
(80-120
1
REF SID
|50.0
1
(98X
1
(90-110
1
Maneanese (-003
i
||693
II
(693
1
|0.0X
I
[30
1
\\m
ii
}4.39
1
1*
1
|80-120
1
0.0050 U|0.050
1
|95X
1
|80-120
1
REF STO
(5.00
»
|97X
1
(90-110
1
Molyfadarftja)-005
1
||37.1
II
(45.1
1
|20X
|
|30
1
1137.1
II
1110
1
|89X
1
|80-120
I
0.050 U (1.2S0
1
|104X
1
|80-120
1
REF STO
|5.00
1
jioox
I
(90-110
1
Nickel |-003
i
||278
II
|282
i
|1.4X
I
|30
1
11278
II
J17.5
1
IV
1
|80-120
1
0.020 U (0.200
1
|126X
1
|80-120
I
REF STO
(5.00
1
|94X
1
(90-110
1
Potass tua |-003
1
H1290
II
11230
1
|4.«X
|
(30
i
||1290
II
|#77
1
|133X
1
|80-120
I
50 U (3520
i
|99X
1
|80-120
1
REF STO
|50.0
i
(100X
1
(90-110
1
Selaniua |-003
1
||50 U
II
(50 U
1
|NC
I
|»
l
||50 U
II
(439
1
|81X
1
(80-120
1
0.500 U (5.00
1
|98X
1
(80-120
I
REF STO
|5.00
1
(101*
1
(90-110
1
Sodium (-003
1
((2130
II
|2040
1
|4.3X
|
1M
1
||2130
II
|«77
I
|86X
1
|80-120
1
0.50 U |2.00
1
(126X
I
|B0-120
1
REF STO
(50.0
1
|100X
1
(90-110
1
Strontiua |-003
1
||124
II
|125
1
|0.8X
i
ISO
1
||5.0U
II
|43.9
1
|130X~
1
|80-120
1
0.050 U |0.500
1
|100X
t
(80-120
1
REF STO
|5.00
1
J100X
1
|90-110
I
Ihallius |*003
I
H5.0U
II
J5.0 U
1
(NC
|
|30
1
|[5.0 U
II
|110
1
|94X
1
(80-120
1
0.050 U |1.250
1
|96X
1
180-120
1
REF STO
|5.00
1
i 100*
1
(90-110
1
Vanadiua |-003
i
||25.7
II
|26.fl
1
|4.2X
\
(30
1
M25.7
II
|110
I
|103X
1
(80-120
1
0.050 U (1.250
1
1102X
1
(80-120
I „„
REF STO
(5.00
1
|100X
I
(90-110
1
Zinc |-003
1
ll«*
II
(143
1
|2.1X
1
(30
1
11146
II
J4.39
1
1*
1
(80-120
1
1.00 U (298
1
|91X
I
(80-120
1
REF STO
11.00
1
|98X
1
(90-110
I
Pet. HydroI-003
, MS.MSD
1(10,900
II
|10,200
I
|6.64
1
!*~
1
(J7690
II
|63,900 P8.9J
J 1
|.+
1
10.0 U (63,900 179.11
i 1
161.1-121
1
REF STD
182.30
1
I97.8J
1
K
l
Analytical results previous to accountino for dilution*. ** Reference Chack saaples are not available lor all analyses. ~~ ftitside of Quality Control Liaits.
» Currently no listits established. Suspect Matrix Inter
D-22
-------
GTC LABORATORY QUALITY CONTROL REPORT
fuMER: HydroQual, Inc. JOB # : R91/03189 UNITS: ug/9 Wet Ut. REPORT TYPE: Job Specific
I II ORIGINALlOUPLICATE| X REL. (ACCEPT.11AVERAGE |SPIKE | PERCENT| ACCEPT. || METMGO | SPIKE | PERCENT| ACCEPT.|| REFERENCE | KNOWN | PERCENT) ACCEPT. ||
¦ARAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X|| RESULT |ADDED |RECOVERY| LIMIT X || BLANK | ADDED jRECOVERY|LIMIIS X|| 0 | PMVAL (RECOVERY) LIMITS X ||
- II
'//////////////////II
* PRECISION
•II
II
* MATRIX SPIKING
II-
| f BLANK
SPIKES
II -
(I REFERENCE
STANDARD
I
I
initablity
-003
||95.9
11
(95.9
1
|0.0X
1
I*4
1
"Ml
||95.9
II
|NA
i
1
1
*11
||NA |
II 1
I
1
II
|J RE F STD
II
(27.0
1
1116%
1
I I
!*~ I
1 1
Uuninua
-003
1116500
II
(16200
1
|1.8X
I
130
1
(|16500
II
|43.9
1
|V
1
|80-120
||10.0 U I
II I
1
1
| |REF STD
II
|5.00
1
1106%
1
(90-110 I
I i
Vnt(oooy
-003
||5.0 U
II
(5.0 U
1
|NC
I
(30
1
|(5.0 U
II
|43.9
1
|14X*»
1
|80-120
||0.050 U (0.500
II 1
) 106%
(80-120
1
11RE F STD
II
|5.00
1
1100X
1
|90-110 I
1 1
irsenic
-003
||50U
H
|50 u
1
| MC
I
|30
1
((50 U
II
|439
1
[78X^
1
(80-120
||0.500 U |5.00
II 1
|99X
(80-120
1
||REF STD
II
(5.00
1
(100%
1
(90-110 |
1 1
lariun
-003
||3210
II
(3260
1
|1.5X
1
130
1
||3210
II
|43.9
1
|v
1
(80-120
|(0.0050 U|0.500
II 1
1104X
|80-120
1
| |REF ST0
II
|5.00
1100%
1
|90-110 |
1 1
leryl1 turn
-001
M1.39
II
|1.34
t
|3.7X
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1
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II
|4.39
1
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||0.0050 U|0.050
tl 1
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I
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|5.00
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1 1
lOf U<1
-003
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(20 U
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|NC
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1
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1
|86%
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||0.200 U |50.0
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1 1
:*dmiun
-003
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M
[0,50 U
1
|NC
1
130
1
||0.50 U
II
(4.39
1
(91X
1
|80-120
||0.0050 U|0.050 U
II 1
|87%
|80-120
1
((REF SID
II
|5.00
1
(96%
1
|90-110 |
1 I
:atciur
-003
115300
II
(5120
(3.4X
1
|30
1
|| 5300
II
|877
1
1*
1
|50-150
||0.50 U |2.00
II 1
|100X
|80-120
1
||R£F STD
II
(50.0
1
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1
|90-110 |
1 1
:hromlun
-003
||398
II
|405
I
|1.7X
1
|30
I
11398
II
121.9
1
IV
1
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110.010 U |0.250
II 1
|92X
|80-120
I
| (REF STO
I)
|5.00
1
198%
1
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1 1
>balt
-003
IIH.2
II
(14.4
1
11.4%
I
|30
1
(|14.2
II
|21.9
1
(97X
1
|80-120
||0.050 U (0.250
II 1
1102%
|80-120
1
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II
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1
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I I
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-003
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|27.a
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1(0.010 U (0.100
II 1
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(80-120
1
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(5.00
1
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1
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1 1
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-003
||20,500
II
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1
|0.0X
I
|30
1
(|20,500
II
|4.39
1
|v
I
|80-120
()0.050 U |0.250
II 1
1100%
(80-120
1
||REF SID
II
J5.00
1
(100%
I
(90-110 (1
1 II
ead
-003
||46.5
II
(45.5
1
|2.2X
I
130
1
||46.5
|21.9
1
I SOX
I
(80-120
1
||0.050 U (0.250
II 1
|97X
I
(80-120
1
11REF STD
II
(5.00
... 1
1101%
I
(90-110 ||
1 II
a i./suUu picvioua lo accounting for dilutions. ** Reference Check samples arc not available for all analyses. ~~ Outside of Quotity Control Limits,
D-23
-------
General
Testing W
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL BASE/NEUTRAL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03189 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
1
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC.
1,4 Dichlorobenzene
6670
0.0
3650
55%
20-124
N-Nitroso-Di-n-propylamine
6360
0.0
0
0%++
D-23 0
1,2,4-Trichlorobenzene
6670
0.0
5280
79%
44-142
Acenaphthene
5740
0.0
2930
51%
47-145
2,4-Dinitrotoluene
6600
0.0
2980
45%
39-139
Pyrene
6270
0.0
2460
39%++
52-115
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC
_IMITS
COMPOUND
(ug/L)
(ug/1)
REC #
RPD #
RPD
REC.
1,4 Dichlorobenzene
6670
2150
32%
52%++
30
20-124
N-N itrsodi-n-propylamine
6360
0
0%
0%++
30
D-230
1,2,4-Trichlorobenzene
6670
2800
42%++
61%++
30
44-142
Acenaphthene
5740
1540
27%++
62%++
30
47-145
2,4-Dinitrotoluene
6600
1370
21%++
74%++
30
39-139
Pyrene
6270
1360
22%++
58%++
30
52-115
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 6 out of 6 outside limits
Spike Recovery: 6 out of 12_ outside limits
COMMENTS:
page ~l~ of _L
-------
General
Testing \3^
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL ACID EXTRACTABLE SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03189 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC.
Phenol
13,400
0.0
8100
60%
5-112
2-Chlorophenol
13,300
0.0
7640
57%
23-134
4-Chloro-3-methylphenol
13,300
0.0
22,700
171%++
22-147
4-Nitrophenol
13,200
0.0
8090
61%
D-132
Pentachlorophenol
13,200
0.0
11,600
88%
14-176
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/L)
(ug/1)
REC #
RPD #
RPD
REC.
Phenol
13,400
4710
35%
53%++
30
5-112
2-Chlorophenol
13,300
4470
34%
52%++
30
23-134
4-Chloro-3-methylphenol
13,300
11,900
89%
62%++
30
22-147
4-Nitrophenol
13,200
3960
30%
68%++
30
D-132
Pentachlorophenol
13,200
5430
41%
73%++
30
14-176
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 5 out of 5 outside limits
Spike Recovery: 1 out of 10 outside limits
COMMENTS:
page y of 2.
D-25
-------
GTC LABORATORY atMlITr CONTROL REPORT
; TOMER: Hydrodual, Inc. JOB i : R91/03268 UNITS: ug/fl Wet Wt. REPORT TYPE: Job Specific
I || ORIGINAL(DUPLICATE| X DEL. |ACCEPT.||AVERAGE |SPItCE | PERCERI| ACCEPT. || METHOD f SPIKE | P£8C£KT| ACCEPT.
'ARAHETER I SAMPLE || RESULT | RESULT | ERROR (LIMIT X|( RESULT |ADDED |RECOVERV| LIMIT X || BLANC | ADDED |RECOVERY|LIMITS X
///////////////////11
* PRECISION
II
• MATRIX SPIKIRG
9nit«bltty|-006
1
||NA
II
1
1
1
1
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I
II
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|«006
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11
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|-006
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1
| I.9X
1
130
I
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II
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1
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1
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II
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1
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1
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|(0.685
n
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|
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1-006
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|-006
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[-006
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| -006
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|-006
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t|202
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(203
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|0.5X
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IL
118.6
1
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REFEREKCk | KNOWN | PERCENT| ACCEPT.
* | PWAl (RECOVER*( UNITS X
11
II -
ll«*
Jl_
BLANK SPIKES
REFERENCE STANDARD
JI-
IJC
JL
IK
JL
.1—
180-120 IIO.OOSO U|0.500 (104X
I_ II I I
JL
lie
JL
U|0.050 (89X
|80-120 ||0.SO U
IL _
J.
(2.00
160-120 H0.010 U |0.250
I— II- -I
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JL
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|CO-120 110.010 u |0.100 [lDOX
I II I I
(80-120 IIO.OSO U 10.250 |100X
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I
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I
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||REF SID
|5.00
|101X
(90-110
J.
*»<>l y( it ..l f.-.ults previous to accounting for dilutions, ** Reference Check SMples ore rvot available for ell analyses. ~ ~ Outside of Quality Control Limits,
00014
l)-2b
-------
GTC LABORATORY QUALITY CONTROL REPORT
STOHER: HydroQual, Inc. JOB * : R91/03268 UNITS: ug/g Uct Ut. REPORT TYPE: Job Specific
1
PARAMETER |
SAMPLE
| ORIGINAL(DUPLICATE| X REL.
| RESULT | RESULT | ERROR
1ACCEPT.
|LIMIT X
|AVERAGE |SPIKE | PERCENT|
| RESULT |ADDED |RECOVERY|
ACCEPT.
LIMIT X
| METHOO
| BLANK
| SPIKE I PERCENT I ACCEPT.
| ADDED |RECOVERY|LIMITS X
| REFERENCE
I *
| KNOWN
| PMVAL
| PERCENT I ACCEPT. |
|RECOVERY| LIMITS X |
///////////////////
1
* PRECISION
• MATRIX
SPIKING
BLANK
SPIKES
| REFERENCE STANDARD
Magnet tun
-006
1
11270
1
11280
1
|0.BX
\
|30
|1270
1746
1
112X
|80-120
I
10.50 U
2.00
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1
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I
150.0
|98X
1
|90-110 I
I I
Manganese
-006
1281
1
|289
1
|2.8X
1
130
1281
|3.73
1
V
|80-120
1
|0.0050 U
0.050
|95X
|80-120
I
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I
|5.00
|98X
1
|90-110 I
1 1
Molytxienun
-006
|24.7
|28.1
113X
1
130
|24.7
|93.3
1
100X
|80-120
1
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1.250
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|80-120
1
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I
15.00
|100X
I
|90-110 |
1 1
Nickel
-006
|22.4
1
|21.6
I
|3.6X
1
130
|22.A
114.9
1
92X
|80-120
I
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215
|S6X
|80-120
1
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I
|5.00
|94X
I
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1 1
PotassItm
-006
1776
1
1806
1
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1
130
|776
|746
1
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180-120
1
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3520
|99X
|80-120
1
|REF STD
I
|50.0
|98X
I
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I I
SelenlL«n
006
|S0 u
|S0 u
1
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1
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150 U
1373
1
SIX
|80-120
I
|0.500 U
5.00
|98X
|80-120
I
|REF STD
I
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1101X
1
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1 1
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-006
| S81
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1597
1
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1
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I
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1
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I
150.0
|100X
1
|90-110 |
I I
Stront ium
-006
|26S
1
|277
1
|4.8X
1
130
|26S
|37.3
1
V
|80-120
I
|0.050 U
0.500
|100X
|80-120
1
I RE F STD
I
|5.00
|100X
1
|90-110 |
1 1
Ihal I iun
-006
|5.0 U
1
|5.0 U
1
|NC
1
130
15.0 U
193.3
1
92X
|80-120
I
|0.050 U
1.250
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|80-120
1
|RE F STD
1
15.00
1100*
1
|90-110 |
1 1
Vanadiun
-006
|22.7
1
|24.8
1
|8.8X
1
130
|22.7
193.3
1
104X
|80-120
I
|0.050 U
1.250
|102X
|80-120
1
|REF STD
1
|5.00
|100X
I
190-110 |
I I
2 inc
-006
|1010
1
(973
1
|3.7X
1
130
11010
|3.73
1
V
|80-120
I
|1.00 U
298
|91X
(80-120
1
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1
11.00
|96X
I
|90-110 |
1 1
Pet. Hydro
-006
|88,600
1
|82,900
1
|<$.65X
1
|18.11
|98,100
|31,443
1
V
|55.9-130
I
110 u
1998
1102X
|61.1-123
I
1
1
I
I
1 1
1 1
Analytica
results
previous
to accounting for di
lutions.
•* Reference Check samples are not availab
e for a
U analyses. ~~
Outside of Quality Control Limits.
~ Currently no limits established. Suspect Matrix Inter
O
O
o
cn
I) - 21
-------
General
~[&Gtinn \ A Fu" ^ervice Environmental Laboratory
Corporation
HSL VOLATILE ORGANICS - SOIL SAMPLE
SOIL VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03268 -006
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENTRATION
CONCENT.
%
LIMITS
COMPOUND
(ug/kg)
(ug/kg)
(ug/kg)
REC #
REC.
1,1-Dichloroethene
12,500
0.0
11,700
94%
D-234
Trichloroethene
12,500
0.0
11,800
94%
71-157
Benzene
12,500
0.0
12,900
103%
37-151
Toluene
12,500
0.0
12,900
103%
47-150
chlorobenzene
12,500
0.0
12,800
102%
37-160
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/kg)
(ug/kg)
REC #
RPD #
RPD
REC.
1,1-Dichloroethene
12,500
9190
74%
24%
30
D-234
Trichloroethene
12,500
10,900
87%
7.9%
30
71-157
Benzene
12,500
.12,000
96%
7.2%
30
37-151
Toluene
12,500
11,800
94%
8.9%
30
47-150
Chlorobenzene
12,500
11,900
95%
7.3%
30
37-160
# Columns to be used to flag recovery and RPD values with ++.
++ = Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0_ out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
"MMENTS:
page of
v 00016
n-?R
-------
General
Testing
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL BASE/NEUTRAL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03268 -006
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/l)
(ug/L)
REC #
REC.
1,4 Dichlorobenzene
101,000
0.0
91,300
90%
20-124
N-Nitroso-Di-n-propylamine
96,300
0.0
83,000
86%
D-230
1,2,4-Trichlorobenzene
101,000
0.0
95,700
95%
44-142
Acenaphthene
87,000
0.0
69,000
79%
47-145
2,4-Dinitrotoluene
100,000
0.0
80,000
80%
39-139
Pyrene
95,000
0.0
90,700
95%
52-115
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/L)
(ug/l)
REC #
RPD #
RPD
REC.
1,4 Dichlorobenzene
101,000
87,800
87%
3.3%
30
20-124
N-Nitrsodi-n-propylamine
96,300
75,000
78%
9.8%
30
D-230
1,2,4-Trichlorobenzene
101,000
91,400
91%
4 .3%
30
44-142
Acenaphthene
87,000
65,900
76%
3.9%
30
47-145
2,4-Dinitrotoluene
100,000
67,000
67%
29%
30
39-139
Pyrene
95,000
85,000
89%
6.5%
30
52-115
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of
Spike Recovery; 0_
6 outside limits
out of 12 outside limits
MMENTS *.
page _2_ of _2m
D-29
00020
-------
General
Testing \$y
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL ACID EXTRACTABLE SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03268 -006
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC.
Phenol
203,000
0.0
182,000
90%
5-112
2-Chlorophenol
201,000
0.0
190,000
95%
23-134
4-Chloro-3-methylphenol
201,000
0.0
218,000
108%
22-147
4-Nitrophenol
200,000
0.0
142,000
71%
D-132
Pentachlorophenol
200,000
0.0
144,000
72%
14-176
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC
LIMITS
COMPOUND
(ug/L)
(ug/l)
REC #
l
l
1 V
1 10
1 o
1
1 =•*=
RPD
REC.
Phenol
203,000
168,000
83%
8.0%
30
5-112
2-Chlorophenol
201,000
176,000
88%
7.6%
30
23-134
4-Chloro-3~methylphenol
201,000
190,000
95%
13%
30
22-147
4-Nitrophenol
200,000
126,000
63%
12%
30
D-132
Pentachlorophenol
200,000
124,000
62%
15%
30
14-176
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
^MMENTS:
page _i_ of _2_
00010
-------
CTC LABORATORY QUALITY CONTROL REPORT
ISTCHER: HydroQual, Inc. JOB 0 : fi91/03270 UNITS: ug/g Met Mt. REPORJ TYPE: Job Specific
1 1
PARAMETER | SAMPLE |
ORIGINAL(DUPLICATE| X REt.
RESULT | RESULT | ERROR
(ACCEPT.)
(LIMIT X|
|AVERAGE
| RESULT
|SP1K£
|A00E0
| PERCENT) ACCEPT.
(RECOVERY| LIMIT X
|| METHOO
|| BLANK
( SPIKE I PERCENT I ACCEPT. || REFERENCE
( ADDED (RECOVERY(LIMITS X|j #
| (NOUN
| PHVAL
1 PERCENT I ACCEPT. ||
(RECOVERY| LIMITS X ||
///////////////////|
* PRECISION
• MATRIX SPIKING
II
BLANK
SPIKES
|| REFERENCE STAN0AR0
II
II
1
Hagnestun |-009 |
1 1
50 U
(50 U
1
[MC
1
(30 |
1 i
)50 U
(855
1
(88X
1
|50-150
1
||50 U
II
(3700
1
(108X
1
|80-120
1
||REF STD
II
(50.0
1
(100X
I
(90-110
1
II
II
Manganese [- 009 |
1 1
0.63
|0.62
1
|2.5X
1
130 |
1 1
|0.63
(4.27
1
|90X
1
|S0-150
1
||0.50 U
M
1315
1
|98X
1
|80-120
1
11RE F STD
|5.00
1
|100X
1
|W-110
1
II
||
Molybdenum]-009 |
1 1
5.0 U
|5.0 U
1
|NC
1
130 |
1 1
|5.0 U
|107
1
|8SX
1
|50-150
1
||5.0 U
M
(18
1
(102X
1
|80-120
1
||REF STD
II
|5.00
1
1102X
1
|90-110
I
II
||
Nickel |-009 |
1 1
2.0 U
12.0 U
1
|MC
1
|30 |
I 1
|2.0 U
117.1
1
1102X
I
|50-150
I
||2.0 U
II
(215
I
|97X
1
(80-120
1
| |REf STD
II
|5.00
1
1100X
1
|90-1I0
1
II
||
Potessiun |-009 |
1 1
50 U
|50 U
1
|HC
1
130 |
150 U
1855
1
|96X
I
|50-1SO
1
1150 u
11
[3520
I
|112X
1
|80-120
1
||REF STD
(50.0
1
(100X
1
|90-110
1
II
||
Selenium J -009 |
I I
50 U
|50 U
1
|NC
I
(30 |
1 I
| SO u
(427
1
| MX
I
|50-150
1
||50 u
II
|11
1
|0X
1
|80-120
1
||REF STD
II
(5,00
1
|1Q2X
1
|90-110
1
5 odiun [-009 |
1 1
54.7
1 so u
l
|NC
1
|30 |
i 1
|S4.7
|855
1
(100X
I
|50-150
i
||50 U
II
|485
1
1 nix
1
|80-120
1
| |REf STD
(50.0
1
1102X
1
(90-110
1
II
Strontium |-0Q9 |
1 1
5.0 U
|5.0 U
1
|NC
1
(30 |
1 1
|5.0 U
(42.7
)94X
1
|50-150
1
||5.0 U
M
(MA
1
) HA
1
|80-120
1
| |REF STD
|5.00
1
|100X
1
|90-110
1
||
Thallium |-009 |
1 1
5.0 U
|5.0 U
1
|NC
1
|30 |
1 1
|5.0 U
1107
1
|86X
1
|50-150
1
||5.0 0
II
|29
1
|70X
1
(80-120
1
| |REF STO
II
|5.00
1
|101X
I
|90-110
1
II
||
Vanadium |-009 |
1 1
5.0 U
|5.0 U
1
| MC
1
|30 |
1 1
15.0 U
(107
1
|94X
1
150-150
1
||5.0 U
H
151
1
|110X
1
|80-120
1
||REF STD
II
|5.00
1
|100X
I
|90-110
1
II
II
Zinc 1-009 |
[ .. 1
t .74
|2.69
1
|42.9X
I
130 |
I 1
|1.74
|4.27
1
|108X
1
)50-150
1
||1.0 U
II
1298
1
|100X
1
|80-120
1
||REF STD
II
|1.00
1
1102X
1
|90-110
1
II
||
1 II
1 II
1
1
1
1 1
1 1
1
1
1
1
1
1
11
II
1
1
1
1
I
1
II
II
1
1
I
1
1
1
II
II
Currently no limits established.
** Reference Check samples are not available for ell analyses.
~~ Outside of Quality Control Limits.
Suspect Matrix Inter
O
o
o
D-31
Crt
-------
GTC LABORATORY QUALlir COMTROL REPORT
iTOMER: HydroOual, Inc. JOB 0 : R91/03270 UNITS: ug/g Uet Ut. REPORT TYPE; Job Specific
I II ORIGINAL|DUPLICATE | % REL. |ACCEPT.||AVERAGE |SPIKE | PERCENT | ACCEPT. || METHOD | SPIKE | PERCENT) ACCEPT.|| REFERENCE I KNOWN | PERCENT | ACCEPT. ||
PARAMETER | SAMPLE || RESULT { RESULT | ERROR (LIMIT X| | RESULT |ADDED (RECOVERY| LIMIT X || BLANK ) ADDED |RECOVERY|LIMITS %|| i | PHVAL |RECOVERY| LIMITS X
II-
II-
II
I!-
V///////////////// II
II-
PREC1S10N
II
MATRIX SPIKING
BLANK SPIKES
REFERENCE STANDARD
Mumt nun
|-009'
1
||17.9
II
115.4
1
|15.0*
1
130
1
||17.9
II
|42.7
I
1106X
1
|50-150
1
1110.0 u
II
(9510
1
1119X
I
|80-120
1
11RE F ST0
II
(5.00
1
|100X
I
|90-110
1
Antimony
| -009
1
||5.0 U
II
[5.0 U
1
|NC
1
130
1
||5.0 U
II
|48.5
I
|97X
1
|50-150
1
(|0.050 U |0.500
| ioax
1
|80-120
1
||REF STD
(5.00
1
|98X
I
|90-110
1
irsenic
|-009
i
| |S0 u
II
|S0 U
1
|NC
1
130
1
||50 U
II
|427
I
|90X
1
|50-150
1
1150 U
II
1203
1
|71X
1
|80-120
1
|(REF STD
II
(5.00
1
J102X
1
|90-110
1
lariua
|-009
1
1130.3
II
|27.5
1
|9.7X
1
(30
1
||30.3
II
|42.7
I
1 1
S
8
|50-150
I
||0.50 U
(210
1
|93X
1
|80-120
I
((REF ST0
II
(5.00
1
1101X
1
|90-110
I
leryli iim
|-009
1
110.50 U
II
|0.50 U
1
| NC
1
130
1
||0.50 U
M
|4.27
I
(50-150
1
||0.50 U
II
|52
1
|94X
1
|80-120
1 •
|)REF STD
II
(5.00
1
|100X
1
|90-110
I
loroo
|-009
1
1120 U
II
|20 U
1
| NC
1
130
1
1120 U
II
14270
I
|91X
I
|50-150
1
||NA
II
1
1
1
1
1
1
||REF SID
II
|5.00
1
1101X
1
|90-110
1
:achiiun
| -009
1
| [0.50 U
II
|0.50 U
1
| NC
1
|30
1
110.50 U
II
[4.27
I
|S6X
I
|S0-150
1
||0.50 U
II
170
1
|97X
1
|80-120
1
11RE F STD
II
|5.00
1
1100X
1
|90-110
I
alciun
|-009
i
11 so u
150 U
1
|NC
1
130
1
||50U
II
1855
I
I
i
|50-150
1
1150 U
H
17520
1
[109X
I
|80-120
1
|(REF STD
|50.0
1
|100X
1
|90-110
1
:hroroiun
1-009
i
||1.0 u
|1.0 u
I
| NC
1
|30
I
111.0 u
II
121.4
1
|86X
1
|50-150
I
1(1.0 U
II
152
1
|99X
I
|80-120
1
(|REF ST0
|5.00
1
|100X
1
|90-110
1
•bait
| -009
1
||5.0 U
II
15.0 U
I
|NC
1
130
I
||5.0 U
II
|21.4
1
|82X
1
(50-150
1
1)5.0 U
II
130
1
1104X
1
|80-120
1
||REF STD
II
15.00
1
|99X
1
|90-110
1
:opper
|-009
1
lli.ou
II
|1.0 u
1
|NC
1
130
I
||1.0 U
II
|S.55
1
|96X
1
|50-150
1
||1.0 u
II
16910
1
|94X
1
(80-120
1
| | RE F STD
II
15.00
1
|100X
1
190-110
1
ron
|-009
1
||29.6
II
|27.4
1
|7.7X
1
130
1
I|29.6
II
(21.4
1
|88X
1
|50-150
1
||5.0U
II
|15,500 I105X
1 1
|80-120
1 -
||REF ST0
II
(5.00
1
1100X
1
|90-110
1
cad
j-009
1
||5.0 U
II
1S.0 u
1
|NC
1
130
1
||5.0U
II
(21.4
1
|88X
1
(50-150
1
H5.0U
II
|B2
1
1102X
1
180-120
1
| |REF STD
il
|5.00
_ I
|100X
I
|90-110
1
Analytical results previous to accounting for dilutions.
O
O
o
Reference Check samples are not available for all analyses. ~~ Outside of Duality Control Limits,
n-32
-------
General
Tocf/nrt \ X/tx A Full Service Environmental Laboratory
Corporation
HSL VOLATILE ORGANICS - AQUEOUS SAMPLE
WATER VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03271 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENTRATION
CONCENT.
%
LIMITS
COMPOUND
(ug/l)
(ug/l)
(ug/l)
REC #
REC.
1,1-Dichloroethene
2500
0.0
1990
80%
D-2 3 4
Trichloroethene
2500
0.0
2170
87%
71-157
Benzene
2500
0.0
2320
93%
37-151
Toluene
2500
0.0
2320
93%
47-150
Chlorobenzene
2500
0 . 0
2410
96%
37-160
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/l)
(ug/l)
REC #
RPD #
RPD
REC.
1,1-Dichloroethene
2500
2020
81%
1.5%
30
D-2 3 4
Trichloroethene
2500
2360
94%
8.4%
30
71-157
Benzene
2500
2480
99%
6.7%
30
37-151
Toluene
2500
2420
97%
4.2%
30
47-150
Chlorobenzene
2500
2540
102%
5.2%
30
37-160
# Columns to be used to flag recovery and RPD values with ++-.
++ = Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
COMMENTS:
page 1 of 1
00064
-------
| || ORIGINAL|DUPLICATE | X DEL. (ACCEPT.|(ORIGINAL(SPIKE | PERCENT | ACCEPT. || METHOD | SPIKE | PERCENT| ACCEPT. || REFERENCE | KNOWN | PERCENT| ACCEPT. ||
ARAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X| | RESULT |ADDED |REC0VERY| LIMIT X || BLANK | ADDED (RECOVERYjLIMlTS X|| # | PMVAL (RECOVERY| LIMITS X ||
CTC LABORATORY QUALITY CONTROL REPORT
///////////////////11 * PRECISION || • MATRIX SPIKING || BLANK SPIKES || REFERENCE STANDARD ||
— II— II II — "II ||
Vanadiun |-003 ||S.OU |5.0 U |NC |30 1)5.0 U 1125 |B8X (80-120 ||5.0U |51 1110X (80-120 ||REF STD (5.00 |100X |90-110 ||
I 11 I -I l_ 11 I I I 11 I I I 11 1 1 I 11
line |-003 ||1.0 U (1.0 U |NC |3Q ||1.0 U |5.00 |88X |80-120 ||1.0 U |298 |100X (80-120 ||REF SID (1.00 (102X |90-110 ||
I II I I I II I I I II I I I II I I I li
I II I I I II I I I II I I I II III II
I 11 I I I 11 I I I 11 I I I 11 I I I 11
I II I I I II I I I II I I I II III II
I 11 I I I 11 I I I 11 I I I 11 __l I I 11
I II I I I II I I I II I I I II III II
I 11 I I I 11 I I I 11 I I I 11 I I | 11
I II I I I II I I I II I I I II III II
I _ll I I I II I I I II —I I I II I | | ||
I II I I I II I I I II I I I II III II
I II I I I II I —I I II I I I II I I | ||
I II I I I II I I I II I I I II III II
l_, II I I I II I I I II I I I II I I | ||
I II I I I II I I I II I I I II III II
I II I I I II I I I II I I I II I I | ||
I II I I I II I I I II I I I II III II
I II I I I II I I I II I I I II I | | ||
I II I I I II I I I II I I I II III II
I II I I I II I —I I II I I I II I I | II
I II 1 I. I II I I I II I I I II III II
I II I I I II I I I II I I I II III II
I 11 I I I 11 I I I 11 I I I 11 I I | II
I II I I I II I I I II I I I II III II
I 11 I I I 11 I I I 11 I I I 11 1 I I 11
I II I L I II I I I II I I I II 1 I I II
I II I I I II I I I II I I I II III II
I _ll I I I II I I I II I I I II 1 I i 11
00063
D- "i4
-------
CtC LABORATORY QUALITY CONTROL REPORT
rOMER: HydroQual, Inc. JOB • : R91/Q327I UNITS-, mg/l REPORT TYPE: Job Specific
I || ORIGINAL I DUPLICATE I X REL. (ACCEPT.|(AVERAGE |SPIKE | PERCENT| ACCEPT. || METHOD | SPIKE | PERCENT| ACCEPT.|| REFERENCE | KNOWN | PERCENT) ACCEPT. ||
WAMETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X|| RESULT |AD0ED |RECOVERY| LIMIT X || BLANK | ADDED |RECOVERY|LIMITS X| | * | PMVAL |RECOVERY| LIMITS X ||
li II II -II II
//////////////////II * PRECISION II * MATRIX SPIKING || BLANK SPIKES j| REFERENCE STANDARD ||
- II II II II II
adniun |-003 |(0.50U |0.50 U |NC |30 (|0.50u (5.00 |S0X |80-120 ||0.50U |70 |97X |8a-12Q ||REf STD 15.00 |100X (90-110 ||
I 11 J I I 11 I .1 I 11 I I _l 11 I I J 11
alciun |-003 ||50U |S0 U |NC |3Q | |J0 U (1000 |92X 180-120 |(50U 17520 |109X 180-120 ||REF STD |50.0 |100X (90-110 ||
I 11 I I I 11 I I I —I I I __l I 11 I I I 11
hromiun (-003 (11.0 U |1.0 U |NC |30 (H-OU (25.0 (80X 180-120 ((1.0 U (52 |99X 180-120 ||REFST0 (5.00 1100% |90-!10 (|
I 11 I. I I 11 I I I 11 I I _l 11 I I I 11
Obalt |-003 ((5.0 U |5.0 U |NC |30 | |S.O U |25.0 |»X" (80-120 ||S.0U (30 |1 |B0-120 ||REF STD |5.00 |102X |90-110 ||
I 11 I I I 11 I I I 11 I I I 11 I I | 11
odiua |-003 |{60.0 |66.9 (11* (30 |(60.0 |1000 |94X |8Q-120 ||50 U |485 |113X (80-120 ||REF STD |50.0 (102X (90-110 ||
i (i i : i i ii i i i it i i i ii i i i ii
trontium (-003 ||5.0U |5.0 U |NC (30 ||5.0U |50.0 |9QX 180-120 ||5.0U |NA |NA |80-120 ||REFST0 |5.0Q |100X |90-110 ||
I II I -I I II I I I II I I I II I | | ||
halUum J-003 ((S.OU |S.O U |MC |30 ||5.QU (125 (80-120 ||5.0U (29 J 70X»» 180-120 ||REFSID 15.00 1101X |90-110 ||
I II I I I II I I I II I I I-. II I I I ||
Analytical results previous to accounting for dilutions. ** Reference Check samples are not available for all analyses. ~~ Outside of Quality Control Limits.
00062
D-JS
-------
CIC LABORATORY QUALITY CONTROL REPORT
4ER: HydroOual, Inc. JOB • ; R91/03271 UNITS: mg/t REPORT TYPE; Job Specific
OR IGINAL|DUPLICA IE ( % BEL. |ACCEPT.|(AVERAGE |SPIKE J PERCENT( ACCEPT. || METHOO | SPIKE | PERCENT( ACCEPT.|| REFERENCE | KNOWN | PERCENT| ACCEPT.
AflETER | SAMPLE || RESULT | RESULT | ERROR (LIMIT X|| RESULT |AOOED |RECOVERY| LIHIT X || BLANK | ADDED (RECOVERY(LIMITS X|| « | PMVAL (RECOVERY| LIMITS X
II-
nmuiimiin |
* PRECISION
MATRIX SPIKING
BLANK SPUES
REFERENCE STANDARD
it —
(|NA
:n
6-25 J6.27
dlty |-003 )|29
129
Unity (-003 |
I I
2.0 U |2.0 U
»-5 Day |-003 |
16.0
[16.0
l-OOJ |
944
1769
nan I a |-003 j
I I
0.050 U |O.OSO u
I
NC
|-003 |
0.20 U |0.20 U
ids, Susj 003 |
73.0
176.0
lfate |-003 |
10.0 U |10.0 U
. hydro.| |
I I
uminm |-003 |
NA
10.5
|11.2
\timony |-003 |
0.050 U (0.050 U
senic (-003 |
0.050 U (0,050 U
ariua (-003 |
0.50 U (0.50 U
eryliiwi | -003 |
I I
0.50 U |0.50 U
I
oron (-003 |
20 U
(20 U
0.3X
0.0X
NC
o.ox
20X
NC
4.OX
NC
6.5X
NC
NC
NC
NC
MC
10 IIO.OSO U (O.SOO
II L
15
10
10
20
30
30
30
I(6.25 (NA
.11 l_
1129
¦ ll_
(100.0
-I
||2.0 U |40.0
.11 I
ir ||i6.o (na
II I
||944 |500
||0.20 U (2.00
II I
1? (|73.0 jNA
10 1(10.0 U (22.0
(|MA
.11
X
((10.5 J50.0
30 ||0.050 U |0.500
n i
30 ||0.050 U (0.500
II l_
(jo.SOU |50.0
30 )|0.50 U (5.00
II I
|(20 U (5000
79%
102X
15X»*
111X
89X
104X
atx
iiox
iiox
99*
72X
-I-
78-122 1)2.0 U (200.0
82-126 ||2.0 U |80.0
||NA
JL_
-I.
79-116 ||25.0U (500
65-128 ||0.050 U |0.250
II I
1UX
50-150 110.20 l) 11.00
(|NA
69-130 ||10.0 U (20.0
IP-1 U |1.998
.11 I
80-120 1(10.0 U (9510
80-120 ||0.050 U |0.500
80-120 |(0.050 U (0.500
II I
80-120 ((0.50 U (210
80-120 (|0.50 U (52
_l_
I
88X (80-120 ||NA
I ll_
Analytical results previous to accounting for dilutions. •* Reference Check samples are not available for a
102X
98X
98X
100X
104X
89. IS
119X
108X
108X
93X
94X
((NA
80-126 ((NA
Il-
ea-123 (|REF STD 1203
(| BE F STD 1200
II I
87-115 (|REF STD |500
II I
79-130 (|REF STD |1.80
II I
70-128 ((REF SID (4.00
II I
| (REF STD 159.50
J I I
79-116 ||REF STD |138
II I
61.1-12||NA |
II I.
80-120 |(REF STD (5.00
II I
80-120 (|R£f SID (5.00
80-120 ((REF SID (5.00
II J
80-120 ((REF SID |5.00
80-120 ||R£f SID . (5.00
: II -I
100X
92X
100X
100X
100X
91X
101X
100X
98X
98X
101X
100%
| (REF STO (5-00 (101X (90-110
I analyses. ~~ Outside of Quality Control Limits.
00^61
D-36
-------
A FullService Environmental Laboratory
SEMI-VOLATILE - WATER SAMPLE
WATER BASE/NEUTRAL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03271 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC.
1,4 Diehlorobenzene
101
0.0
63 .8
6 3%
20-124
N-Nitroso-Di-n-propylamine
96.3
0.0
0
0%*+
D-230
1, 2 ,4-Trichlorobenzene
101
0.0
59.9
59%
44-142
Acenaphthene
87.0
0.0
45.5
52%
47-145
2,4-Dinitrotoluene
100
0.0
61.7
62%
39-139
Pyrene
95.0
0.0
54 .8
58%
52-115
General
Testing
Corporation
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/1)
(ug/1)
REC #
RPD #
RPD
REC.
=========•====«==«==«====»==—=—
USaSBSB
«===«==^==»===
=======
=======
=======
======
1,4 Diehlorobenzene
101
63.7
63%
0%
30
20-124
N-Nitroso-Di-n-propylamine
96.3
0
0%++
NC
30
D-230
1,2,4-Trichlorobenzene
101
65.4
65%
10%
30
44-142
Acenaphthene
87 . 0
45.3
52%
0%
30
47-145
2,4-Dinitrotoluene
100
64. 1
64%
3.2%
30
39-139
Pyrene
95.0
59.5
63%
8.3%
30
52-115
# - Columns to be used to flag recovery and RPD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 1 out of 6 outside limits
Spike Recovery: 2 out of 12 outside limits
"5MMENTS:
page 2 of 2
» 00069
D-37
-------
General
Testing vr
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - WATER SAMPLE
WATER ACID EXTRACTABLE SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03271 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/l)
(ug/L)
REC #
REC.
Phenol
203
0.0
126
62%
5-112
2-chlorophenol
201
0.0
127
63%
23-134
4-Chloro-3-methylphenol
201
0.0
192
96%
22-147
4-Nitrophenol
200
0.0
145
72%
D-132
Pentachlorophenol
200
0.0
192
96%
14-176
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(•ug/L)
(ug/1)
REC #
RPD #
RPD
REC.
Phenol
203
127
63%
1.6%
30
5-112
2-Chlorophenol
201
125
62%
1.6%
30
23-134
4-Chloro-3-methylphenol
201
163
81%
17%
30
22-147
4-Nitrophenol
200
133
67%
72%
30
D-132
Pentachlorophenol
200
195
98%
2.1%
30
14-176
# - Columns to be used to flag recovery and RPD values with ++.
++ - values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 0 out of 5 outside limits
Spike Recovery: 0 out of 10 outside limits
COMMENTS:
page 1 of 2
4 OOfSS
D-38
-------
CTC LABORATORY QUALITY CONTROL REPORT
iTOHER: HydroQual, Inc.
JOB U : R91/03273
UNITS: ug/g Wet U(.
REPORT TYPE: Job Specific
I || ORIGINAL(DUPLICATEI X BEL. |ACCEPT.11AVERAGE |SPIKE | PERCENT| ACCEPT. |
•ARAMETER | SAMPLE || RESULT |.RESULT | ERROR |LIHIT X|| RESULT |ADDED |RECOVERY| LIMIT X |
METHOD I SPIKE | PERCENT| ACCEPT.|| REFERENCE | KNOWN | PERCENT| ACCEPT.
BLANK | ADDED |RECOVERY|LIMITS X|| » | PMVAL |RECOVCRY| LIMITS X
II
II REFERENCE STANDARD
'//////////////////11
PRECISION
* MATRIX SPIKING
BLANK SPIKES
lagnesiim |-003
1
"II
1150 U
II
|50 U
1
|NC
I
J30
I
"•II
||50 U
II
(971
1
|85X
1
|50-150
1
1150 u
II
13700
1
1108X
I
|80-120
1
| |REF STD
II
150.0
1
1100X
I
|90-110
1
langanese |-003
1
||0.50 u
1!
|0.50 U
1
|NC
I
130
1
||0.50 U
II
|4.85
1
|8SX
1
|50-150
1
110.50 U
II
1315
1
|98X
1
|80-120
1
||REf STD
II
15.00
1
|100X
I
|90-110
I
Holyt>denun| -003
I
||5.0 U
II
15.0 U
1
|NC
I
|30
1
||5.0 U
II
1121
1
|86X
1
(50-150
I
||5.0 U
II
|18
1
|102X
1
(80-120
1
||RE F ST0
II
15.00
1
1102%
1
|90-110
I
Jickel (-003
1
||2.0 U
II
|2.0 U
1
|NC
I
|30
1
||2.0 U
II
119.A
1
|93X
1
|50-150
1
||2.0 U
II
|215
1
|97X
1
180-120
I
|J REF STD
II
15.00
1
|100X
1
|90-110
1
'otassiim |-003
1150 U
II
150 U
1
|NC
I
|30
1
||50U
II
|971
1
|93X
1
(50-150
1
1150 U
II
(3520
1
1112%
1
(80-120
1
11RE F STD
II
150.0
1
|100X
I
(90-110
I
¦eleniun |-003
1
||50 U
II
150 U
1
|NC
I
130
1
(150 U
II
|485
1
|89X
1
|50-150
1
||50 U
II
|H
1
|0X
1
(80-120
1
(|REF STD
II
15.00
1
[102*
1
|90-110
|
iodium | 003
1
1150 U
II
150 U
1
|NC
I
|30
1
1150 U
II
|971
I
|96X
1
|50-150
1
| {50 U
11
1 1
X"
CD
(113X
1
|80-120
I
11RE F STD
II
150.0
1
1102X
I
|90-110
|
, tront iun |-003
1
||5.0 U
II
|5.0 U
1
|NC
I
|30
1
||5.0 U
(48.5
I
|91X
1
|50-150
1
(|5.0 U
II
|NA
1
| NA
1
|80-i20
1
| (REF STD
II
(5.00
1
|100X
I
|90-110
|
hat I iun | -003
1
||5.0 U
II
|5.0 U
1
| NC
I
|30
1
||5.0 U
II
1121
1
|80X
1
|50-150
1
115.0 U
II
|29
1
|70X
1
|80-120
1
| |REF STD
II
15.00
1
1101X
1
|90-110
I
'anadiun |-003
||5.0 U
II
|5.0 U
1
| NC
I
130
1
||5.0 U
II
j 121
|93X
1
|50-150
1
115.0 U
151
1
|110X
1
|80-120
1
||REF STD-
II
15.00
1
1100X
1
|90-110
(
inc (-003
111.63
II
11.0 u
I
| NC
I
130
1
||1.63
II
|4.85
1
|54X
1
(50-150
t
||1.0 U
II
(298
1
(100X
1
(80-120
1
11REF STD
II _ .
|1.00
1
|102X
1
(90-110
1
1 II 1 1 1 II 1 1 1 II 1 1 1 II III
1 II 1 1 1 II 1 1 1 II 1 1 1 11 III
Analytical results previous to accounting for dilutions.
Currently no limits established.
Reference Check sanples are not available for all analyses.
~~ Outside of quality Control Limits.
Suspect Matrix Inter
00087
D-39
-------
GTC LABORATORY QUALITY CONTROL REPORT
ONER: HydroQual, Inc. JOB # : R91/03273 UNITS; ug/g Met Wt. REPORT TYPE: Job Specific
I
RAHETER I SAMPLE
| ORIGINAL(DUPLICATE| X REL. (ACCEPT.||AVERAGE (SPIKE | PERCENT| ACCEPT. || HETHOO | SPIKE ( PERCENT| ACCEPT.|| REFERENCE | KNOWN | PERCENT| ACCEPT.
| RESULT | RESULT | ERROR (LIMIT X[( RESULT |ADDED |RECOVERY| LIMIT % || BLANK | ADDED (RECOVERY(LIMITS X|| 0 ( PMVAL (RECOVERY) LIMITS X
'/////////////////
II
II
II
* PRECISION
-II
II
• MATRIX SPIKING
-II
II
BLANK SPIKES
II
|( REFERENCE
STANOARD
.uninun
(-003
1
11
1110.0 u
II
|10.0 U
1
|NC
1
(30
1
1(10.0 u
II
(48.5
1
(101X
1
(50-150
1
||10.0 u
II
(9510
1
(119X
1
J80-120
1
||REF STD
II
|5.00
1
(100X
1
|90-110
1
it itnooy
|-003
1
1(5.0 1)
II
(5.0 U
1
|NC
1
130
1 •
((5.0 U
II
|44.6
1
(102%
1
|50-150
1
((0.050 U |0.500
II I
(108X
1
|80-120
1
||REF STD
II
15.00
1
|98X
1
|90-110
1
senic
|-003
1
| |so u
II
(50 U
1
|NC
1
|30
1
||50 U
II
|485
1
|90X
1
|50-150
| (50 U
II
(203
1
|71X
I
|80-120
I
11RE F STD
II
(5.00
1
(102*
1
|90-110
1
ariun
|-003
i
110.50 U
II
(0.50 U
1
(NC
1
|30
1
||0.50 U
II
(48.5
1
(100X
1
|50-150
1
| (0.50 U
II
(210
1
(93X
I
(80-120
1
j|RE F STD
II
(5.00
1
(101X
I
|90-110
1
erytliun
|-003
1
((0.S0 u
II
|0.50 U
1
[NC
1
(30
1
(|0.50 U
II
|4.85
1
176%
1
|50-150
1
((0.50 U
II
(52
1
|94X
1
|80-120
1
||REF SID
|5.00
1
(100X
I
|90-110
1
oron
(-003
1
1120 U
II
(20 U
1
(NC
1
130
1
|(20 U
II
|4850
1
(89X
1
|50-150
1
||NA
II
1
1
1
1
1
1
(|REF STD
II
15 00
1
(101X
1
|90-110
1
acini un
|-003
1
||0.50 U
II
|0.50 U
1
| NC
1
(30
1
||0.50 U
II
|4.85
1
(80S
1
|50-150
1
|(0.50 U
II
(70
1
|97X
1
|80-120
1
|(REf STD
II
(5.00
1
(100X
1
(90-110
1
atciun
|-003
I
11 SO u
II
(50 U
1
| NC
1
(30
1
1150 U
II
|971
1
|92X
1
|50-150
||50U
II
17520
1
|109X
1
|80-120
I
((REF SID
II
(50.0
1
(100*
1
|90-110
1
hroffliun
|-003
1
111.0 u
II
(1.0 u
1
(NC
1
(30
1
1(1-0 U
II
|24.3
1
|82X
1
(50-150
1
||1.0U
II
152
1
(99X
1
(80-120
1
| (REF STD
II
* (5.00
1
|100X
1
|90-110
1
bait
|-003
1
(|5.0 U
II
(5.0 U
1
(NC
1
(30
1
I|5.0 U
II
(24.3
J
|78X
1
(50-150
1
115.0 U
II
|30
1
(104X
1
(80-120
1
1|REF STD
II
(5.00
1
|99X
1
|90-110
1
opper
|-003
1
II1.0 u
II
|1.0 u
1
|NC
1
|30
1
||1.0 U
II
(9.71
1
|88X
1
|50-150
1
||1.0 u
II
|6910
1
|94X
1
(80-120
1
| (REF STD
II
(5.00
1
|10UX
1
|90-110
1
ron
|-003
1
||5.0 U
II
|5.0 U
1
(NC
1
130
1
|(5.0 U
II
|24.3
1
|96%
1
(50-150
1
||5.0 U
II
|15,500 |105X
1 1
|80-120
1
||REF STD
II
J 5.00
1
|100X
1
|90-110
I
fad
| -003
1
I|5.0 U
II
|5.0 U
1
|NC
1
130
1
||5.0 U
II
|24.3
1
|82X
1
|50-150
1
1(5-0 U
II
J 82
1
(102X
1
|80-120
1
((REF STD
II
(5.00
1
1100*
1
(90-110
1
Aii.ilyiic.it results previous to accounting for dilutions.
0008fi
** Reference Check samples are not available for all analyses.
IWtl)
~~ Outside of Quality Control Limits,
-------
General
Testing W
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL BASE/NEUTRAL MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name; General Testing Corp.
Matrix Spike - Sample No. : R91/03276 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT,
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC,
1,4 Dichlorobenzene
6730
0.0
4600
68%
20-124
N-Nitroso-Di-n-propylamine
6410
0.0
0
0*++
D-23G
1,2,4-Trichlorobenzene
6730
0.0
4 53 0
67%
44-142
Acenaphthene
5790
0.0
3200
55%
47-145
2,4-Dinitrotoluene
6660
0.0
3260
49%
39-139
Pyrene
6330
0.0
3500
55%
52-115
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC LIMITS
COMPOUND
(ug/L)
(ug/l)
REC #
RPD #
RPD
REC.
1,4 Dichlorobenzene
6730
4830
72%
4.3%
30
20-124
N-Nitrsodi-n-propylamina
6410
0++
0%++
NC++
30
D-23Q
1,2,4-Trichlorobenzene
6730
4800
71%
58%
30
44-142
Acenaphthene
5790
3230
56%
2.0%
.30
47-145
2,4-Dinitrotoluene
6660
3200
48%
2.0%
30
39-139
Pyrene
6330
3800
60%
8.7%
30
52-115
# - Columns to be used
to flag recovery and
*PD values with ++.
++ - Values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD: 1 out of 6 outside limits
Spike Recovery; 2 out of 12 outside limits
5MMENTS; •
pa9S-2-°f-2- 00102
-------
General
Testing \3^
Corporation
A Full Service Environmental Laboratory
SEMI-VOLATILE - SOIL SAMPLE
SOIL ACID EXTRACTABLE SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name: General Testing Corp.
Matrix Spike - Sample No. : R91/03276 -003
SPIKE
SAMPLE
MS
MS
QC
ADDED
CONCENT.
CONCENT.
%
LIMITS
COMPOUND
(ug/L)
(ug/1)
(ug/L)
REC #
REC,
Phenol
13,500
0.0
9260
69%
5-112
2-Chlorophenol
13,400
0.0
9360
70%
23-134
4-Chloro-3-methylphenol
13,400
0.0
12,300
92%
22-147
4-Nitrophenol
13,300
0.0
6530
49%
D-132
Pentachlorophenol
13,300
0.0
10,400
78%
14-176
SPIKE
MSD
MSD
ADDED
CONCENT.
%
%
QC
LIMITS
COMPOUND
(ug/L)
(ug/1)
REC #
RPD #
RPD
REC.
Phenol
13,500
9690
72%
4.2%
30
5-112
2-Chlorophenol
13,400
9690
72%
2.8%
30
23-134
4-Chloro-3-methylphenol
13,400
13,100
98%
6.3%
30
22-147
4-Nitrophenol
13,300
6490
49%
0%
30
D-132
Pentachlorophenol
13,300
8960
67%
15%
30
14-176
# - Columns to be used to flag recovery and RPD values with ++.
++ - values outside of QC limits
MS QC Limits = EPA Acceptance Criteria
RPD Limits = Internal Acceptance Criteria
RPD; 0 - out of 5 outside limits
Spike Recovery; 0 out of 10 outside limits
COMMENTS;
page __1_ of _2_
00101
-------
ETC LABORATORY QUALITY CONTROL REPORT
| || ORIGINAL (DUPLICATE | X REl. (ACCEPT. 11 AVERAGE (SPItCE | PERCENT | ACCEPT. || METHOD | SPIKE | PERCENT | ACCEPT.|| REFERENCE | KNOWN | PERCENT) ACCEPT. ||
'ARAMETER ( SAMPLE || RESULT | RESULT ( ERROR (LIMIT X| | RESULT (ADDED |RECOVERY| LIMIT X || BLANK | ADOED (RECOVERY|LIMITS %|| « | PNVAL |RECOVERY) LIMITS X ||
II * * II II II II
'lltlllHNiUIIUI| ( * PRECISION || * MATRIX SPIKING || BLANK SPIKES || REFERENCE STANDARD ||
II II II II ||
ttgnesiun (-005 ||1920 |2240 |15X (30 |(1920 (952 |142X*» (80-120 ||50U (3700 |108X |80-t20 ||REFST0 |50.0 |100X (90-110 ||
l_ 11 I I I 11 I I U 11 I I I 11 1 I I | i
longwise (-003 |(501 (522 (4.1X (30 ||501 (4.76 |V (80-120 |[0.50 U |315 |98X (80-120 ||REF STD [S.OO (100X (90-110 ||
I 11 I I I 11 I I I 11 I I I 11 I I | 11
iolytodenun|003 II*6-5 |51.5 |10X (SO ||46.5 1119 |90X 180-120 ||5.0 U 118 |102X 180-120 (|REF STD |5.00 |102X (90-110 ||
J. 11 I I I -I I I I I 11 I I I 11 I I I 11
ticket |-003 (1154 ( 212 |31X~ (30 ||154 (19.0 |V (80-120 | (2.0 U |215 | 97X 180-120 | |REF STD |S.OO |100X 190-110 ||
I 11 I- I I .11 I I I 11 I. _l _l 11 I I | 11
•ot ass inn (-003 ; ||922 (1230 |29X (30 JJ922 J952 |140X (80-120 ((SOU (3520 (112X (80-120 ((REf STD |50.0 (100X (90-110 ||
__ I II I I I II I I I II I I I II I I I ||
•clantui |-003 ||SOU (50 U |NC |30 | (50 U |476 |74X |80-120 1150 U (11 |0X~ (80-120 (| REF STD |5.00 |102X |90-11Q ||
I. 11 I -I I- 11 —I I :l II I I I 11 I I | 11
¦odiui |-003 ||2350 12460 (4.6X (30 ((2350 (952 (105X (80-120 ||50U |485 (113* 180-120 | |REF STO (50.0 1102X (90-110 ||
_l 11 I I I 11 I I I 11 I I I 11 J I | 11
.trontiun (-003 ||332 |352 |5.8X |30 |(332 |47,6 |V (80-120 ||5.0U |NA |NA |80-120 ||REF STO |5.00 |100X (90-110 ||
-I 11 I I- I 11 I I I 11 I I I 11 I I ( 11
r hat I tin |-003 ||5.0U |5.0 U |NC (30 ||5.0U |119 172* (80-120 ||5.0U 129 |70X" 180-120 ||REF SID (5.00 (101% 190-110 ||
I II I I I II I I I II I I I II I I ( I|
/anadiun (-003 J119.6 (22.6 (14X (30 (119.6 (119 | 98X (80-120 ||5.0U |51 J110X (80-120 | (REF STO |5.00 |100X (90-110 ||
I 11 I I I 11 I I I 11 I I -I 11 I I | 11
{inc |-003 ||1180 (1320 |11X |30 ||1180 |4.76 |V |80-120 ||1.0U |298 |100X |80-120 ||REF STD (1.00 |102X |90-110 ||
J N )_ I, I II I I I II I I I II I I |_ ||
>et. Hydro)-003 | (29,600 |27,700 |6.63X \*+ 117880 |41O00| 12.21 (•~ (| 10.0 U |4260 |07.7X |58.7-11 €J pEF STD (83.26 p8.9X ||
I 11 I I I- 11 I I I 11 I I I 11 I I I 11
Analytical results previous to accounting for dilutions. •• Reference Check samples are not available for all analyses. ~~ Outside of Quality Control Limits.
~ Currently no limits established. Suspect Matrix Inter
* 00100
D-43
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6TC LABORATORY OUALIir CONTROL REPORT
| || 081GlHAL|DUPL1CATE| X REL. (ACCEPT.||AVERACE (SPIKE | PERCENT | ACCEPT. || HETHOO | SPIKE | PERCENT | ACCEPT.([ REFERENCE | KNOWN | PERCENT) ACCEPT. ||
¦RAKETER | SAMPLE || RESULT | RESULT | ERROR (UNIT X|| RESULT (AODEO |RECOVERT| LIHIT X || BLANK | ADDED [RECOVERY|LIHITS X|| # | PMVAl |RECOVERT| UNITS X ||
* II II II II - ||
//////////////////11 * PRECISION || * MATRIX SPIKING || BUNK SPIKES || REFERENCE STANDARD ||
II II "II "11 I ||
nitabtltyJ-003 ||»100 (>100 |0.0X |*« ||>100 |NA | | ||NA | | | ||NA | | | ||
J 11 I I I 11 I I I 11 I I I 11 I I I 11
tuninua |-0Q3 ll**0 17250 |2.8X (30 ((7080 (47.6 |V 180-120 ||10.QU (9510 |119X (80 120 | |REF STD |5.00 |100X (90-110 ||
I II I I I II I I I II I I I II I I |__ ||
,fitlmor>y |-003 ||5.0 U (5.0 U |NC |30 |(5.0 U (47.6 |?5**» |60-120 ||5.0U |27 |0X+* |80-120 ||RLFSTO (5.00 (JOOX |90-110 ||
I 11 I I I 11 I- I I 11 I I I 11 I I |. 11
vrsenic |-003 ||50 U (SOU |NC |30 1150 U (476 |80X | SO-120 ((SOU |203 |71X (80-120 ||REF STD |5.00 |102X J90-110 ||
I 11 l_ I I 11 I I I 11 I I I 11 I I | 11
lariua |-003 |(1820 11310 |33X»* |30 ||1820 (47.6 |V |80-120 ||0.50U |210 |93X (80-120 ||REF SID (5.00 |101X (90-110 ||
l__ll I t I H I I I II I I I II I I | I)
J OOi 1(1.02 (1.02 |0.0X 130 111.02 |NA | | ||0.50l> (19.4 |94X (80-120 | |REF STD |5.00 |102X (90 110 ||
_ _ll I I I II I I J II I I I II I I I ||
, ,><*1 | 005 | 120 U (20 U |NC (30 ||20U (4760 |B7X |80-120 ||NA ( | ( ||REF STD (5.00 (101X 190-110 (|
i II I I I II I I I II I I I II I 1 .1 ||
.ictniurn |-003 ||5-50 |6.01 |8.9X |30 ||5.50 |4.76 |90X |BO-120 ||0.50U 170 |97X |BO-120 11 RE F STD |5.00 |100X (90-110 ||
I II I I I II I I I II I I I II I | | ||
;atcium |-003 ((12,200 (12,700 |4.0X (30 ||12,200 |952 |V 150-150 ||50U 17520 |10VX (80-120 | |REF SID |50.0 |100X 190-110 ||
I II I I I II I I I II I I I II I | | ||
Ch.omium (-003 ||336 |428 |24X |30 |(336 |23.8 |V |S0-120 ||1.0U |52 |99X (80-120 ||REFSTO |5.00 |100% |90-110 ||
I II L I I II I I I II I I I II _! | i ||
.call |-00 J ||13.0 |K.9 |HX |10 | 113.0 |23.8 (VOX 180-120 | (5.0 U |30 |104X 180-120 ||REFSID |5.00 |99X (90-110 | |
J II I I L II I I I II I I I II I | l_ ||
Copper |-003 ||99 ( 98.2 |0.8X |30 ||99 |9.52 |V |80-120 ||1.0U |6910 |94X (80-120 )|REF SID |5,00 |100X |90-110 ||
.I II I I I II I I I II I I I II I | | ||
iron |-003 ||34,800 |34,4QQ |1.3X |30 ||34,800 |1.76 |V (80-120 ||0.050 U 10.250 |106X (80-120 ||REF SIO |5.00 |98X |90-110 ||
I II I I I II I I I II I I I II I | | ||
lead (-003 11239 ( 244 |2.1X (30 ((239 (23.8 |¥ (80-120 (J5.0U (82 |102X (80-120 ||REF STD (5.00 (100X (90-110 j|
_l II I I I II I I I (I I I I II : I ( | (I
Analytical results previous to accounting for dilutions. ** Reference Check camples, are not available (or all analyses. *~ Outside of duality Control limits.
00099 n-44
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APPENDIX E
EQUIPMENT CALIBRATION DOCUMENTATION
• Flow Meter Calibration
• Thermocouple and Pressure Gauge Calibration
-------
FLOW METCR CALIBRATION: SEPTEMBER 3, 1991
Pump
Tea
Meter
Calibrated Ttnk
Percent
Average
Setting
Number
Reeding
Reeding
Ewor
Emir
DTC"
39.9
1
351
319
+ 10
+6.4
+6.1
2
351
332
+5.7
3
361
349
+3.4
49.8
1
565
525
+ 7.6
+ 8.4
+ 5 9
2
564
506
+ 11.5
3
565
532
+6.2
60
I
760
623
+22.0
*18.6
+ 21.5
2
756
658
+ 14.9
3
760
640
+ 18.8
'''Percent error determined by DTC on June 12, 1991
E-l
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REPAIR ORDER NUMBER A 8658"
(wnnrrn\ N0RTH JERSEY instrument service co., inc.
W0I15CU) 243 TEANECK ROAD, RIDGEF1ELD PARK, N. J. 07660 CUSTOMER'S ORDER NUMBER .
AREA CODE 201/641-2700 SHOP REPAIR Q FIELD SERVICE^T" PW | |
CPU mamf CHAM ADDRESS
DATE OF /* ATT: .
DESCRIPTION OF ITEMS COVERED
C;fl l/ilfA-T/M ,J A et-^/tA 3ZT - V Jlif ~ "
^WTT^fpZ Y-V -id* ***$<- cltecfft /V'' M
C AU^ATO^ IS ActisftA-B?' Y~E. I ft
M ^J^ v '"A/ S ' (-'b p c /It £) ^ <^S'^
C*A ligg/iT/py >s ft YZ-'l rA
*f-(2tWo/riftloV tjtc, aa/^4- 0-99V c Aoc^rtoM t*fAc
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1, REPORT NO. 2.
EPA/540/R-92/002
3. RECIPIENT'S ACCESSION NO.
A. TITLE AND SUUTITLE
Technical Evaluation Report: THE. CARVER-GREENFIELD ¦'
PROCESS DEHYDRO-TECH CORPORATION
5. REPORT DATE
Auaust 1992
6. PERFORMING ORGANIZATION CODE
7. AUTMORISI
PRC, Inc.
8. PERFORMING ORGANIZATION REPORT NO|
1
I
D. PERFORMING ORGANIZATION NAME AND ADDRESS
644 Linn Street
Cincinnati, Ohio 45203
10. PROGRAM ELEMENT NO.
1 1. CONTRACT/GRANT MO.
68-CO-0047
12. SPONSORING AGENCY NAME AND ADDRESS
Risk Reduction Engineering Laboratory-~Cin., OH
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
13. TYPE OF REPORT AND PERIOD COVERED
Summary
14 SPONSORING AGENCY CODE
EPA/600/14
15. SUPPLEMENTARY MOTES
Laurel Staley, 513-569-7863
ig."abstract i'his report~e~va~iiTate d the ability of Dehydro-Tech Corporation's fDTC) Carver-
Greenfield Process to separate oil contaminated waste drilling muds to their constituent
solids, oil and water fractions. The Carver-Greenfield Process (C-G) was developed by
DTC in the late 1950's and is licensed in over 80 plants worldwide. The technology is
designed to separate solid-liquid mixtures into three product streams: a clean, dry
solid; a water product substantially free of solids and organics; and a concentrated
mixture of extracted organics. A mobile pilot plant was used for the demonstration.
The C-G Process demonstration was conducted at EPA's Edison, New Jersey facility in
August, 1991. Waste drilling muds from the PAB Oil and Chemical Services, Inc.(PAD Oil)
site in Vermilion Parish, Louisiana were processed in the demonstration. PAB Oil, which
ceased operation in 1983, operated three oil drilling mud separation pits from which the
waste material used in the demonstration was collected. The demonstration consisted of
two test runs. Both test runs produced a clean dry solids product similar to bentonite
in appearance. Indigenous oil removal was 91.8 percent and 88.3 percent in Test Runs 1
and 2. respectively. Indigenous total petroleum hydrocarbon and water removal was
greater than 99.9 percent in both test runs.
RCRA Toxicity Characteristic (TC) limits for
organics. DTC has projected treatment costs
C-G Process to be $523 per wet ton of waste,
specific and_$302 per ton is site specific
.Hoi;—Ln cjjiamtj-cui—cl£—t.h6—ijid i-g ©nou s—94-1—ox-tF-a t h e-wti'S ¦fre'
The dry solids product also complied with
metals, volatile organics, and semivolati le
for the PAB Oil site drilling muds by the
Of this total, $221 per ton is technology
Of .the site specific costs, $240 per ton is
OhSCMll'YOHS
key words AND DOCUMENT ANALYSIS
iMDKNTlPllinii/OlMiN tiNOGD TtHMLi
cosaTi I icUi/(Jump
Separation Technology
Extraction
Innovative Waste Treatment
If DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (77h.i 11,•port)
Unclassified
20. SECURITY CI.ASS (This j'uxci
Unclassi fied
21 NO. or- PAGES
111
77 PRICE
EPA V or m 2220-1 (Rov. A-'/h
PHtV liUI TION i S ODSOLE T£
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