vvEPA
United States
Environmental Protection
Agency
Office of Research and
Development
Washington DC 20460
EPA/600/9-90/049
March 1991
Alternative Biological
Treatment Processes for
Remediation of Creosote- and
PCP-Contaminated Materials
Bench-Scale Treatability Studies
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EPA/600/9-90/049
March 1991
Alternative Biological Treatment Processes for
Remediation of Creosote- and PCP-Contaminated
Materials
Bench-Scale Treatability Studies
James G. Mueller, Suzanne E. Lantz
Southern Bio Products, Inc.,
Beat O. Blattmann
Technical Resources, Inc.,
Douglas P. Middaugh and Peter J. Chapman
Microbial Ecology and Biotechnology Branch
U.S. Environmental Protection Agency
Environmental Research Laboratory
Gulf Breeze, Florida
Peter J. Chapman
Project Officer
Contract Number
68-033479
U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th Floor
Chicago, IL 60604-3590
U.S. Environmental Protection Agency
Office of Research and Development
Environmental Research Laboratory
Gulf Breeze, Florida
Printed on Recycled Paper
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Notice
The information in this document has been subjected to Agency review and approved
for publication. Mention of trade names of commercial products does not constitute
endorsement or recommendation for use.
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Preface
The abandoned American Creosote Works at Pensacola, Florida, used creosote as a
wood preservative from 1902 until 1950, then a mixture of creosote, pentachlorophenol
(PCP) and copper-chromium arsenate (CCA) from 1950 until its closure in 1981. Improper
disposal of wastes resulted in extensive contamination of surface soil and the shallow
groundwater aquifer at this site. In September 1989, bioremediation was selected to
ameliorate surface soils contaminated with creosote and PCP.
To determine the most effective approach to bioremediation of contaminated sediments
and surface soil (i.e., slurry phase vs. solid phase), the Microbial Ecology and Biotechnology
Branch of the U.S. EPA Environmental Research Laboratory at Gulf Breeze Florida
(GBERL) was commissioned in February 1990 to perform bench-scale biotreatability
studies. This work was performed as part of a Cooperative Research and Development
Agreement between the Gulf Breeze Environmental Research Laboratory and Southern Bio
Products, Inc., (Atlanta, GA) as defined under the Federal Technology Transfer Act, 1986
(contract no. FTTA-003). Results and conclusions of these studies have contributed to the
selection of an efficient, cost-effective remedial technology.
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Abstract
Bench-scale biotreatability studies were performed to determine the most effective of
two bioremediation application strategies to ameliorate creosote- and pentachlorophenol
(PCP)-contaminated soils presentat the American Creosote Works Superfund site, Pensacola,
Florida: solid-phase bioremediation or slurry-phase bioremediation. When indigenous
microorganisms were employed as biocatalysts, solid-phase bioremediation was slow and
ineffective (8-12 weeks required to biodegrade >50% of resident organics). Biodegradation
was limited to lower-molecular-weight constituents rather than the more hazardous, higher-
molecular-weight (HMW) compounds); PCP and HMW polycyclic aromatic hydrocarbons
(PAHs) containing 4 or more fused rings resisted biological attack. Moreover, supplemen-
tation with aqueous solution of inorganic nutrients had little effect on the overall effectiveness
of the treatment strategy. Alternatively, slurry-phase bioremediation was much more
effective: >50% of targeted organics were biodegraded in 14 days. Again, however, more
persistent contaminants, such as PCP and HMW PAHs, were not degraded when subjected
to the action of indigenous microorganisms.
IV
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Contents
Notice ii
Preface iii
Abstract iv
Tables vi
Figures vii
Acknowledgments viii
1. Introduction 1
1.1 Purpose..: 1
1.2 Test Objectives 1
1.3 Site Description 1
1.4 Site History 1
2. Remedial Technology Description 3
2.1 Biological Treatment 3
2.1.a Solid-Phase Bioremediation 3
2.1.b Slurry-Phase Bioremediation 3
3. Experimental Procedures 5
3.1 Solid-Phase Bioremediation 5
3.1.a Sample Acquisition and Storage 5
3.1.b Experimental Design 5
3.2 Slurry-Phase Bioremediation 7
3.2.a Sample Acquisition and Storage 7
3.2.b Soil Washing 7
3.2.c Experimental Design 7
3.3 Shake Flask Studies 8
3.3.a Groundwater Shake Flask Studies 8
3.3.b Solidified Material 9
3.4. Extraction Procedures 9
3.4.a Aqueous Samples 9
3.4.b Soil and Sediment Samples 10
3.4.c Slurry Samples 10
3.4.d Extraction of PCP from Soils 10
3.4.e Activated Carbon Traps 13
3.5 Analytical Methods 13
3.5.a PAH Analysis 13
3.5.b N-, S-, 0-Heterocycles 13
3.5.C Phenol Analysis 13
3.5.d PCP Analysis 13
3.5.e CLP Analyses 14
3.5.f Microbial Population Counts 14
3.5.g Percent Moisture Content 15
3.6 Microtox Assays 15
3.7 Teratogenicity Assays 15
3.8 Quality Assurance/Quality Control 15
4. Results and Discussion 17
4.1 Compound Identification Numbers 17
4.2 Extraction Efficiency 17
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4.3 Groundwater Shake Flask Studies 17
4.4 Solid-Phase Bioremediation 18
4.5 Slurry-Phase Bioremediation 19
4.6 Sediment Shake Flask Studies 22
5. Conclusions 42
S.I Solid-Phase Bioremediation: Surface Soil 42
5.2 Solid-Phase Bioremediation: Sediment 42
5.3 Slurry-Phase Bioremediation: Surface Soil 42
5.4 Slurry-Phase Bioremediation: Sediment 42
5.5 Site Specific Factors 42
5.6 Preliminary Studies 42
Appendices
A Soil Washing Report 43
B CLP Analytical Data (ESD, Athens GA) 53
Tables
Table 3.1 Composition of Modified Bushnell-Haas Medium 5
Table 3.2 Amounts of Modified Bushnell-Haas Inorganic Nutrient Solution
or Distilled Water Added to Each Land Farming Chamber at Weekly Intervals 6
Table 3.3 Standard Mixture of 22 PAH Components of Creosote Used for Instrument
Calibration and Determination of Detection Limit 16
Table 3.4 Standard Mixture of 10 Phenolic Constituents of Creosote Used for Instrument
Calibration and Determination of Detection Limit 16
Table 3.5 Standard Mixture of 13 N-, S-, and 0-Heterocyclic Constituents of Creosote
Used for Instrument Calibration and Determination of Detection Limit 16
Table 4.1 Chemicals Corresponding to Compound Identification Numbers 18
Table 4.2 Recovery of PCP and Creosote Constituents from Spiked Soil and Water Samples
from the ACW Site, Pensacola, Florida 20
Table 4.3 Concentration in \ig/ml of PCP and Selected Creosote Constituents in Groundwater
Subjected to the Action of Indigenous Microorganisms (Groundwater Shake Flask Study) 21
Table 4.4 Response of Embryonic Menidia beryllina to Untreated and Biotreated Filtered
Groundwater from the ACW Site, Pensacola, Florida 22
Table 4.5 Concentration of PCP and 42 Creosote Constituents during
Solid-Phase Bioremediation of Creosote-Contaminated Surface Soils
from the ACW Site, Pensacola, Florida: Unamended Soil 23
Table 4.6 Loss (volatilization) from the Land Farming Chamber Containing Unamended Surface Soil 24
Table 4.7 Percent Biodegradation of PCP and 42 Creosote Constituents during Solid-Phase Bioremediation
of Creosote-Contaminated Surface Soils from the AGW Site, Pensacola, Florida: Unamended Soil 25
Table 4.8 Concentration of PCP and 42 Creosote Constituents during Solid-Phase
Bioremediation of Creosote-Contaminated Surface Soils from the ACW Site,
Pensacola, Florida: Plus Nutritional Amendments 26
Table 4.9 Loss (volatilization) from the Land Fanning Chamber Containing Nutrient-Amended Surface Soil 27
Table 4.10 Percent Biodegradation of PCP and 42 Creosote Constituents during Solid-Phase Bioremediation
of Creosote-Contaminated Surface Soils from the ACW Site, Pensacola, Florida:
Soil Amended with Inorganic Nutrients 28
Table 4.11 Changes in Soil Microbial Numbers during Solid phase Bioremediation of
Creosote-Contaminated Surface Soils Obtained from the ACW Site, Pensacola, Florida 29
Table 4.12 Concentration of PCP and 42 Creosote Constituents during Solid-Phase
Bioremediation of Creosote-Contaminated Sediments from the ACW Site, Pensacola, Florida:
Unamended Sediment 29
Table 4.13 Loss (Volatilization) from the Land Farming Chamber Containing Unamended Sediment 30
Table 4.14 Percent Biodegradation of PCP and 42 Creosote Constituents during Solid-Phase Bioremediation of
Creosote-Contaminated Sediment from the ACW Site, Pensacola, Florida: Unamended Sediment 31
VI
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Table 4.15 Concentration of PCP and 42 Creosote Constituents during Solid-Phase
Bioremediation of Creosote-Contaminated Sediments from the ACW Site, Pensacola, Florida:
Nutrient-Amended Sediment 32
Table 4.16 Loss (Volatilization) from the Land Farming Chamber Containing Nutrient-Amended Sediment 33
Table 4.17 Percent Biodegradalion of PCP and 42 Creosote Constituents during Solid-Phase Bioremediation
of Creosote-Contaminated Sediment from the ACW Site, Pensacola, Florida:
Nutrient-Amended Sediment 34
Table 4.18 Changes in Soil Microbial Numbers during Solid phase Bioremediation of
Creosote-Contaminated Sediments Obtained from the ACW Site, Pensacola, Florida 35
Table 4.19 Concentration of PCP and 42 Monitored Creosote Constituents during Slurry-Phase
Bioremediation of Creosote-Contaminated Surface Soils from the ACW Site, Pensacola, Florida 35
Table 4.20 Abiotic Losses during Slurry-Phase Bioremediation of
Creosote-Contaminated Surface Soils from the ACW Site, Pensacola, Florida 36
Table 4.21 Percent Biodegradation of PCP and 42 Monitored Creosote Constituents during Slurry-Phase
Bioremediation of Creosote-Contaminated Surface Soils from the ACW Site, Pensacola, Florida 37
Table 4.22 Concentration of PCP and 42 Monitored Creosote Constituents during Slurry-Phase
Bioremediation of Creosote-Contaminated Sediment from the ACW Site, Pensacola, Florida 38
Table 4.23 Abiotic Losses during Slurry-Phase Bioremediation of Creosote-Contaminated
Sediments from the ACW Site, Pensacola, Florida 39
Table 4.24 Percent Biodegradation of PCP and 42 Monitored Creosote Constituents during Slurry-Phase
Bioremediation of Creosote-Contaminated Sediments from the ACW Site, Pensacola, Florida 40
Table 4.25 Biodegradation in jig/ml of 21 PAHs during Slurry-Phase Bioremediation of Solidified Material
from the ACW Site, Pensacola, Florida 41
Figures
Figure 1.1 Site layout; American Creosote Works Superfund site, Pensacola, Florida 2
Figure 3.1 Diagram of land farming chambers used for solid-phase biotreatability studies 6
Figure 3.2 Diagram of Biostat M bioreactor used for slurry-phase biotreatability studies 8
Figure 3.3 Flow chart for extraction and chemical analysis of aqueous samples 11
Figure 3.4 Flow chart for extraction and chemical analysis of soils and sediments 12
Figure 3.5 Flow chart for extraction and analysis of PCP in soils 14
VII
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Acknowledgments
Technical assistance was provided by Miriam Woods, Maureen Downey, Dava Dalton
and Mike Shelton (Technical Resources, Inc.). Susan Franson graciously offered a QA/QC
review of these studies. Assistance from Natalie Ellington and Beverly Houston (U.S.
EPA, Region IV) is gratefully acknowledged. Financial support for these studies was
provided by the U.S. EPA Superfund Program (Region IV).
This work was performed as part of a Cooperative Research and Development
Agreement between the Gulf Breeze Environmental Research Laboratory and Southern
Bio Products, Inc., (Atlanta, GA) as defined under the Federal Technology Transfer Act,
1986 (Contract No. FTTA-003).
VIII
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1. Introduction
1.1 Purpose
The Microbial Ecology and Biotechnology Branch of the
U.S. Environmental Protection Agency's Environmental Re-
search Laboratory at Gulf Breeze, Florida (GBERL) per-
formed bench-scale biotreatability studies to help delineate
the most applicable approach for remediation of creosote-
contaminated surface soils at the American Creosote Works
Superfund site, Pensacola, Florida. .Two approaches were
evaluated: 1) solid-phase bioremediation (land fanning), and
2) slurry-phase bioremediation. This document presents per-
formance data generated at the bench-scale level.
1.2 Test Objectives
The primary objective of these studies was to generate
bench-scale performance data on two approaches to the
bioremediation of PCP- and creosote-contaminated sediment
(material beneath the solidified sludge) and surface soil (Op-
erable Unit 1). The two approaches evaluated were: 1) solid-
phase bioremediation (land farming), and 2) slurry-phase
bioremediation. In addition, preliminary studies were per-
formed to evaluate the potential applicability of biological
treatment processes to ameliorate PCP- and creosote-contami-
nated solidified material and groundwater also present at this
site (Operable Unit 2). These data will be used to help
delineate the most applicable approach for surface soil
bioremediation.
1.3 Site Description
The American Creosote Works site (ACW) at Pensacola,
Florida is an 18 acre (7.3 ha) abandoned wood-preserving
facility located approximately 600 yards (550 m) north of
Pensacola Bay near the entrance of Bayou Chico (Figure 1.1).
This plant used creosote as a wood preservative from 1902
until 1950, then a mixture of creosote, pentachlorophenol
(PCP) and copper-chromium-arsenic (CCA) from 1950 until
its closure in December 1981. Improper disposal of creosote-
and PCP-contaminated waste resulted in extensive contami-
nation of surface soil and the shallow groundwater aquifer at
this site.
1.4 Site History
In March 1980, considerable quantities of "oily/asphaltic/
creosotic material" were found by the City of Pensacola in the
groundwater near the intersection of L and Cypress streets. In
July 1981, the U.S. Geological Survey installed nine ground-
water monitoring wells in the vicinity of the ACW site. Data
from these studies led to a decision to close this site in
December 1981.
In February 1983, the Site Screening Section of EPA
Region IV (Atlanta, GA) conducted a Superfund investigation
which included sampling and analysis of on-site soils, waste-
water sludges, sediment in drainage ditches, and on-site and
off-site groundwater monitoring wells. Because of the threat
posed to human and environmental health by frequent over-
flows from waste ponds located at this site, the U.S. EPA
Region IV Emergency Response and Control Section per-
formed an immediate cleanup during September and October,
1983.
A Remedial Investigation/Feasibility Study (RI/FS) under
CERCLA was completed by EPA Region IV in 1985. Based
on these studies, EPA signed a Record of Decision (ROD) in
September 1985, which specified that all on-site and off-site
contaminated soils, sludges, and sediments be placed in an on-
site RCRA-type landfill. However, the state of Honda was
not in agreement with the ROD developed at that time.
Consequently, a Post-RI was conducted by EPA Region IV
Environmental Services Division (ESD) to identify, develop,
and evaluate alternatives for remediation at this site. These
studies were completed in August 1989 at which time a
proposed plan outlining these alternatives was presented to
the public.
In September 1989, a second ROD was adopted which
organized the remedial work into two discrete operable units:
1) surface soil remediation, and 2) remediation of contami-
nated groundwater, solidified material, and underlying sedi-
ment Biological treatment (bioremediation) was selected as
the most appropriate technology for operable unit 1 (the
second Operable Unit is undergoing additional study to better
define the applicability of various remediation alternatives).
To determine the most effective approach to
bioremediation of contaminated sediments and surface soils
(i.e., slurry phase vs. solid phase), the Microbial Ecology and
Biotechnology Branch of the U.S. EPA's Environmental Re-
search Laboratory at Gulf Breeze Florida (GBERL) was com-
missioned in February 1990 to perform bench-scale
biotreatability studies. This document reports the results and
conclusions of these studies.
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II II
Main Pond
Overflow Pond
R. R. Impoundment
pen**01
lla0ay
0 200 400 600 800 1000
Scale of Feet
Figure 1.1 Site layout, American Creosote Works, Superfund site, Pensacola, Florida.
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2. Remedial Technology Description
2.1 Biological Treatment
Bioremediation describes the process whereby organic
wastes are biologically degraded under controlled conditions
to an innocuous state, or to levels below concentration limits
established by law. Biological catalysts used to facilitate this
process can include indigenous microbes and/or specially
selected microbial inocula. Characteristics of the ACW site
(e.g., nature of contaminants, soil type, climate) make it
amenable to bioremediation. Hence, bioremediation has been
chosen as the treatment technology for Operable Unit 1 (sur-
face soil remediation). However, the exact means through
which bioremediation will be employed to restore these ma-
terials remains to be defined (this study).
2.La Solid-Phase Bioremediation
Solid-phase bioremediation (land farming) is a process
that treats contaminated soils in an above-ground system
using conventional soil management practices (i.e., tilling,
irrigation, fertilization) to enhance the microbial degradation
of contaminants. These systems can be designed to reduce
abiotic losses of targeted contaminants through processes
such as leaching and volatilization. Bench-scale treatability
studies described herein have assessed the significance of
these processes, and have considered the extent to which they
affect the overall performance of solid-phase bioremediation
of creosote-and PCP-contaminated sediment and surface soil
from the ACW site.
Solid-phase bioremediation has been reportedly used to
treat PCP and creosote wastes, oil field and refinery sludges,
petroleum products and pesticide wastewaters. While the pro-
cess is claimed to be effective in treating creosote-contami-
nated soils, existing data show that the more recalcitrant
contaminants (i.e., higher-molecular-weight PAHs and highly
chlorinated aromatics) tend to persist. Unfortunately, these
same compounds are responsible for a number of the potential
adverse effects on environmental and human health.
2.1.b Slurry-Phase Bioremediation
Slurry-phase bioremediation involves the treatment of
contaminated solid materials (soil, sediment, sludge) in a
bioreactor. Bioreactors can be specially designed in a variety
of configurations to accommodate the physical and chemical
characteristics of the targeted pollutant(s). Bioreactors can
contain indigenous microbes, or they may be inoculated with
specially selected microorganisms capable of rapidly and
extensively degrading targeted pollutants. In general, the rate
and extent of biodegradation is more manageable with
bioreactors than with solid-phase biotreatment processes be-
cause bioreactors facilitate mixing and intimate contact of
microorganisms with targeted pollutants, and they maintain
environmental conditions (pH, dissolved oxygen, nutrients,
substrate bioavailability, etc.) optimum for the biodegradation
processes.
While slurry-phase bioremediation systems have been
reported to be effective in treating creosote-contaminated
soils, the activity of the microorganisms housed in these
reactors can be severely limited by the presence of toxic or
inhibitory compounds (i.e., heavy metals). As with solid-
phase bioremediation, care must be taken to minimize abiotic
losses (adsorption, volatilization), and biodegradation of the
more recalcitrant pollutants must be demonstrated.
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3. Experimental Procedures
3.1 Solid-Phase Bioremediation
Solid-phase bioremediation studies were performed at the
bench-scale level with creosote- and PCP-contaminated sedi-
ment and surface soil obtained from the ACW site at Pensacola,
Florida. The rate and extent of biodegradation by indigenous
microorganisms were determined, and the influence of
supplementation with inorganic nutrients on the biodegrada-
tion process was evaluated. Data generated in these studies
have been used to predict the potential effectiveness of solid-
phase bioremediation to ameliorate the ACW site.
3.La Sample Acquisition and Storage
On March 28, 1990, composite samples of surface soil
and sediment were collected from the ACW site by the U.S.
EPA Environmental Services Division (ESD), Athens, Geor-
gia. Approximately 56.7 kg of creosote- and PCP-contami-
nated surface soil (SS) were obtained from Grid no. 47, and an
approximate 56.7 kg of highly contaminated sediment mate-
rial (SD) were removed from a depth of 3-5 m beneath the
capped solidified material. A 4.5 kg composite subsample of
each of these materials was placed in a 19 L plastic bucket,
sealed air-tight and stored at 2°C for solid-phase bioremediation
studies. The remainder of each material was divided as fol-
lows: approximately 45 kg were stored on site in separate 208
L steel drums (DOT-17C) for subsequent soil washing, a 500
g composite subsample of each material was placed in a clean,
sterile, 16 oz I-CHEM jar and stored at 2°C for enumeration
of indigenous microorganisms, and a second 500 g composite
subsample of each material was placed in a clean, sterile, 16
oz I-CHEM jar and stored at 2°C for Microtox assay, teratoge-
nicity testing and chemical analysis.
3.1. b Experimental Design
Bench-scale biotreatability studies to evaluate the effi-
ciency of land farming (solid-phase bioremediation) to treat
creosote-contaminated sediment and surface soil were initi-
ated on April 5,1990. "Land farming chambers" (Figure 3.1)
were specially designed as contained systems by placing large
(253 mm ID, 110 mm bowl depth, 50 mm stem), porcelain
Buchner funnels (special order, Coors Ceramics, Denver, CO)
inside inverted 300 mm OD x 300 mm height, amber-colored,
polyetherimide, vacuum chambers (Nalgene Labware, Roch-
ester, New York). Funnels were seated on top of a 250 ml
beakers to collect leachate, if any. Oil-free air (oil-free com-
pressor) entering the chambers was saturated with water to
prevent drying of the materials within the chambers. Separate
lines were used to connect each individual chamber to the air
source, and air flow was established through the chambers at
100 ml/min. Air leaving the chambers was passed through an
activated carbon trap to retain volatile emissions. An up-
stream, in-line carbon trap was used as the control for extrane-
ous organics. Since the vacuum chambers were being used
under positive pressure, a 4.5 kg weight was placed on top of
each chamber to insure an air-tight seal between the chamber
and the base-plate.
Approximately 3 kg (± 30 g) of creosote-contaminated
surface soil (1.0% creosote [wgt], 6.6% moisture) or sediment
(5.5% creosote [wgt], 14% moisture) were placed into each of
two Buchner funnels lined with a Whatman no. 1 filter paper
(4 chambers). Two treatments were established for each type
of material: 1) unamended, and 2) supplementation with aque-
ous solution of inorganic nutrients (a third treatment, nutri-
tional supplementation plus bioaugmentation using propri-
etary microbial inocula, is described in an auxiliary repent). At
the time of loading, 50 ml of sterile, modified Bushnell-Haas
(MBH) inorganic nutrient solution (Table 3.1) were added to
the chambers designated to receive inorganic nutritional
amendments, and materials were mixed well (tilled) by hand
using a small trowel. Those materials not supplemented with
inorganic nutrients received 50 ml of sterile, distilled water
prior to mixing. Solid materials were mixed well (tilled) on a
weekly basis. Subsequent additions of water or inorganic
nutrient solution were based on maintaining a 10-15% mois-
ture content of the sediment or soil. The resultant schedule for
the additions of water or nutrient solution to surface soil and
sediment is summarized in Table 3.2.
TM» 3.1 Competition of Modified Bushndl-Haai Medium
Compound Amount Added (mg/L)
K,HP04
(NH4HN03
MgSO4 7H,O
CaCI,2HtO
FeCI
1000
1000
1000
200
20
5
7.1 (adjusted)
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"I —— Air leaving chamber
\*
Air source
Weight
Top plate
Whatman no.1 filter paper
Air entering chamber
3 kg soil or
sediment
Porcelain Buchner
funnel
Leachate collection
beaker (250 ml)
Polyetherimide vacuum chamber
Figure 3.1 Diagram of land farming chambers used for solid-phase biotreatability studies.
Table 3.2 Amount* of Modified Bu*hnell-Haa* Inorganic Nutrient Solution or Distilled Water Added to Each Land Farming
Chamber at Weekly Interval*
Date
4/5
4/12
4/21
4/27
5/5
5/11
5/18
5X5
5/31
6/8
6/15
6/22
6/29
(time-zero)
(weekl)
(week 2)
(weekS)
(week 4)
(week 5)
(weekB)
(week 7)
(week 8)
(week 9)
(week 10)
(week 11)
(week 12)
Surface Soils
SO ml MBH or 50 ml water
25 ml MBH or 25 ml water
50 ml MBH or 50 ml water
25 ml MBH or 25 ml water
50 ml MBH or 50 ml water
50 ml MBH or 50 ml water
50 ml MBH or SO ml water
50 ml MBH or 50 ml water
25 ml MBH or 25 ml water
25 ml MBH or 25 ml water
25 ml MBH or 25 ml water
25 ml MBH or 25 ml water
terminate
Sediments
50 ml MBH or 50 ml water
no additions
no additions
25 ml MBH or 25 ml water
50 ml MBH or 50 ml water
25 ml MBH or 25 ml water
25 ml MBH or 25 ml water
25 ml MBH or 25 ml water
no additions
25 ml MBH or 25 ml water
25 ml MBH or 25 ml water
25 ml MBH or 25 ml water
terminate
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Composite subsamples (ca. 45 g) of soil or sediment were
removed from each land-farming chamber prior to mixing at
time-zero and after 1,2,4,8 and 12 weeks incubation at room
temperature (23 ± 3°C). The following parameters were deter-
mined on samples: 1) moisture content, 2) microbial popula-
tion counts, and 3) amounts of PCP and creosote constituents.
A 35 g sample was placed in a clean, sterile, 125 ml I-CHEM
jar fitted with a Teflon-lined screw-cap, labeled appropriately
and stored at 2°C for subsequent moisture and chemical
analyses (see ANALYTICAL METHODS). A separate 10 g
sample stored at 4°C was used for enumeration of microbial
populations (see ANALYTICAL METHODS).
Activated carbon was removed from each trap (including
the control trap) and replaced with freshly activated carbon
(500°C for 6 hr) at the same time that the soil and sediment
samples were collected. An additional sampling was made 2
days after initiation. Activated carbon samples were placed in
clean, 125 ml Erlenmeyer flasks fitted with Teflon-lined
screw-caps and extracted immediately as described below
(see ANALYTICAL METHODS). At the conclusion of these
studies (12 weeks incubation), composite subsamples of sur-
face soil and sediment from each chamber were forwarded to
ESD (Athens, GA) for independent chemical analysis (see
APPENDIX).
Design of the land-farming chambers allowed periodic
sampling of soil or sediment, and the quantitation of abiotic
losses of PCP and creosote constituents (volatilization, leach-
ing). Hence, losses directly attributable to biodegradation
could be quantified accurately. However, materials within the
chambers were not exposed to photooxidation or extremes in
temperature or moisture content. Therefore, losses observed
through volatilization and leaching are probably conservative
in comparison to those expected to occur in situ. Furthermore,
since soil and sediment were incubated in the laboratory
within amber-colored chambers, any direct or indirect effects
of photocatalysis on the biodegradation of monitored chemi-
cals were eliminated. Thus, creosote and PCP biodegradation
data are conservative as well.
3.2 Slurry-Phase Bioremediation
Bench-scale studies evaluated the potential applicability
of slurry-phase bioremediation of creosote- and PCP-con-
taminated soil and sediment from the ACW site. The rate and
extent of biodegradation of PCP and selected creosote con-
stituents were monitored, and the removal of pollutants from
contaminated materials was determined. Performance data
generated has been used to predict the efficacy of this approach
employing indigenous microorganisms.
3.2.a Sample Acquisition and Storage
Refer to section 3.1.a.
3.2.b Soil Washing
On April 19, 1990, approximately 34 kg of surface soil
and sediment from the ACW site were shipped via overnight
express to Chapman, Inc., Freehold, New Jersey (on-site soil
washing was performed on April 6 and 7, 1990 but the
resultant slurries were not usable). Upon arrival, materials
were stored at 4°C for subsequent processing. On April 30,
1990, soil and sediment samples were washed separately with
0.05% Triton X-100 to facilitate dispersion and the transfer of
pollutants into the aqueous phase (see APPENDIX A). Nine-
teen L of resultant slurry of each material were shipped to
GBERL on May 10, 1990, and received on May 15, 1990,
where, upon arrival, they were stored at 4°C for subsequent
studies.
3.2.c Experimental Design
Preliminary analyses established the following properties
for sediment and soil slurries, respectively: 1) pH = 10 and 7,
2) percent suspended solids = 2.7 and 2.1%, and 3) organic
loading rate = approximately 10 and 1% of the solids (i.e.,
10% of the suspended sediment solids was creosote/PCP). On
June 5,1990, slurries were homogenized (mixed for 2 hr) and
1.2 L of each slurry was added to one of two bioreactors. The
appropriate amount of dry, inorganic salts was then added to
each reactor to provide a base-line level of nutrients as de-
scribed in Table 3.1. At the same time, 100 ml of each slurry
was transferred to a clean, sterile 125 ml I-CHEM jar for time-
zero chemical analyses.
Slurry-phase bioremediation studies were performed with
two, 1.5 L Biostat M bioreactors (see Figure 3.2), (B. Braun
Biotech, Allentown, PA). The bioreactor design was such that
all surfaces exposed to hydrophobic creosote constituents
were either glass or stainless steel. The pH of each slurry was
adjusted to 7.1, and the reactors were operated in a batch
culture mode for 30 days. Bioreactors were programmed to
automatically maintain pH=7.1 ± 0.1, dissolved oxygen (DO)=
90%, and temperature=28.5°C. The DO concentration was
maintained by adjusting both agitation (< 300 rpm) and air-
flow rates, while the pH was maintained through the automatic
addition of acid (1.0 N H2SO4) or base (1.0 N NaOH). Al-
though the operating parameters were controlled electroni-
cally, bioreactors were inspected on a daily basis.
Bioreactors were sampled following 1,3,5,7,14,21 and
30 days of batch culture operation. Samples were obtained by
manually removing 50 ml of medium from each bioreactor
with a clean, sterile borosilicate glass pipette. Duplicate 25 ml
samples of culture medium from each bioreactor were trans-
ferred to a clean, sterile 125 ml I-CHEM jar for immediate
extraction and analysis as described below (see ANALYTI-
CAL METHODS). At the same times, separate 1.0 ml samples
of culture media were removed from each bioreactor to moni-
tor changes in microbial protein concentrations (see ANA-
LYTICAL METHODS).
Air leaving each bioreactor was passed through an acti-
vated carbon trap which was sampled periodically (day 7, 21
and 30) to monitor for losses via volatilization. At the conclu-
sion of these studies, undissolved sludge and oily-creosotic
material adhering to the internal surfaces of the bioreactors
were removed by washing with methylene chloride which was
made up to a standard volume for quantitation of PCP and
creosote constituents. By accounting for these different means
of abiotic removal of creosote/PCP from aqueous solution
(volatilization and adsorption), loss from soil and sediment
directly attributable to biodegradation could be quantified
accurately.
-------
Mr leaving
— Stirring device
& ** . s M* -^^^^
Figure 3.2
Diagram of Biostat M bioreactor used for slurry-phase biotreatability studies.
3.3 Shake Flask Studies
While the objective of this biotreatability study was to
identify appropriate bioremediation techniques for Operable
Unit 1 (surface soil remediation), preliminary studies were
also performed to determine the potential effectiveness of
biological treatment to degrade creosote and PCP present in
groundwater and solidified material at the ACW site. These data
will be used to help define appropriate treatment technologies
for Operable Unit 2.
3.3. a Groundwater Shake Flask Studies
On March 27, 1990, approximately 400 L of PCP- and
creosote-contaminated groundwater (G W) were recovered from
Well no. 320 at the ACW site. Groundwater was removed
from a depth of 7 m through Teflon-coated Bev-a-line tubing
(15 mm ID) by means of an electric pump, transferred directly
into two freshly rinsed, 208 L steel drums (DOT-17E) and
stored on site for ancillary testing (Supplement to the Final
Report). At intermittent times during sampling, five subsamples
(1.0 L) were collected in clean, sterile Wheaton bottles fitted
with Teflon-lined screw-caps and stored on ice for transport to
the laboratory. Upon arrival at the laboratory, subsamples
were stored at 2°C for subsequent biodegradation studies,
teratogenicity testing and chemical analyses.
Biodegradability of chemicals present in groundwater
recovered from the ACW site was evaluated as follows: a total
of 15 flasks (125 ml Erlenmeyer flasks fitted with Teflon-
lined screw-caps) containing 12.5 ml of filtered groundwater
(passed through a plug of silanized glass wool to remove
undissolved solids) plus 12.5 ml of modified Bushnell-Haas
medium (1:1 ratio/vol:vol) were prepared. Additionally, two
clean, sterile 1.0 L Wheaton bottles fitted with Teflon-lined
screw-caps received 200 ml of the same groundwater medium
(GWM). No difference in terms of organic pollutants present
in filtered and unfiltered groundwater could be detected by
gas chromatographic analyses or toxicity/teratogenicity stud-
ies (data not shown). Hence, the filtered GWM was used to
monitor the fate of organic pollutants upon exposure, under
optimum conditions for biodegradation, to catabolic activities
of indigenous microorganisms.
8
-------
Microbial inoculum was prepared by mixing 25 g of
creosote- and PCP-contaminated surface soil (freshly ob-
tained from grid no. 47) with 100 ml of 2.5 mM phosphate
buffer (pH=7). Soils were mixed well and suspensions were
centrifuged (2500 rpm, 10 min) to remove larger soil particles.
The resultant supernatant was decanted and used as a source
of indigenous, "creosote-adapted" microorganisms for the
GWM.
Each flask containing 25 ml GWM was inoculated with
1.0 ml (27 ng microbial protein) of the washed soil microbial
suspension. The two 1.0 L Wheaton bottles, each containing
200 ml GWM, received 8.0 ml of the same cell suspension.
Duplicate 25 ml samples were immediately extracted (see
below) for time-zero chemical analysis. Flasks were incubated
at 30°C with shaking (200 rpm) in the dark for 14 days.
Killed-cell controls were prepared for each sampling time
point by adding 2.5 ml of a 37% formaldehyde solution to five
of the shake flasks containing 25 ml GWM.
After 1,3,5,8 and 14 days incubation, the entire contents
of two active flasks and one killed-cell control flask were
separately extracted and analyzed for the presence of PCP and
selected creosote constituents (see below). After 14 days
incubation, the contents of flasks containing 200 ml GWM
were filtered (0.2 micron Teflon filter) and assessed for changes
in toxicity (Microtox assay) and teratogenicity as described
below (see ANALYTICAL METHODS). These data were
compared with those obtained from untreated (non-inoculated)
GWM that had been stored at 2°C during the 14 day incuba-
tion period.
3.3.b Solidified Material
Creosote- and PCP-contaminated solidified material was
recovered from beneath the capped area at the ACW site by
BSD (Athens, GA) on March 28,1990. This material was
placed in clean, sterile, 64 oz I-CHEM jars and stored at 2°C
for subsequent analyses. Shake flask studies were performed
to determine the ability of microorganisms indigenous to the
ACW site to biodegrade organic contaminants present in this
material. This potential was assessed under 3 separate condi-
tions: 1) solidified material as it occurs in situ (pH=9.5), 2)
solidified material adjusted to pH=7.2, and 3) solidified ma-
terial adjusted to pH=7.2, plus augmentation with indigenous
surface soil microorganisms.
For condition 1,6.25 g of solidified material were added
to a 125 ml Erlenmeyer flask fitted with a Teflon-lined screw-
cap containing 18.75 ml of modified Bushnell-Haas medium
(Table 3.1) resulting in a slurry containing 25% suspended
solids at pH=9.5. Condition 2 was established in the same
manner, but the pH of the slurry was adjusted to pH=7.2 with
8.5% phosphoric acid. For the third incubation condition, 5.25
g of solidified material was mixed with 1.0 g of surface soil
obtained from the nutrient amended land-farming chamber
(after 12 weeks incubation), and the pH was adjusted to
pH=7.2. This procedure resulted in the addition of 4.0 x 107
bacterial cells as determined by total heterotrophic plate counts.
A sufficient number of flasks was prepared for each
treatment such that duplicate flasks could be removed at each
sampling point. Additionally, a sufficient number of killed
cell control flasks (3.7% formaldehyde) was prepared for each
treatment to allow for extraction of duplicate control flasks of
each treatment at each time point (4 killed cell control flasks
for each treatment). The pH of the flask contents was checked
on a daily basis and adjusted as needed since the pH tended to
rise with agitation.
After 7 and 14 days incubation at 30°C with shaking (200
rpm), duplicate 1.0 ml samples were recovered from each
flask for bacterial plate counts. The remaining slurry was
extracted with methylene chloride according to the procedure
developed for slurry samples (see EXTRACTION PROCE-
DURES). Organic extracts were then analyzed by gas chro-
matography for the presence of PCP and creosote constituents
(see ANALYTICAL METHODS).
3.4 Extraction Procedures
3.4.a Aqueous Samples
The procedure for extraction and analysis of aqueous
samples from groundwater shake flask studies is outlined in
Figure 3.3. The entire volume of GWM from each flask was
transferred to a clean (rinsed with methylene chloride), 60 ml
separatory funnel. Flasks were then rinsed with 10 ml methyl-
ene chloride, and this was added to the aqueous sample. The
GWM was adjusted to pH=12.0 with IN NaOH, then ex-
tracted 3 times with 10 ml volumes of methylene chloride
resulting in the transfer of non-polar (PAHs, O, 5-hetero-
cycles) and weakly basic creosote constituents (A/-hetero-
cycles) to the organic phase. The combined organic phases
were washed once with 10 ml of distilled water (returned to
the aqueous phase), dried by passage over a layer of anhydrous
sodium sulfate (25 g) and collected in clean, 25 ml Kuderna-
Danish concentrating tubes. The volume of methylene chloride
was reduced to 1.0 ml by evaporating under a stream of dry
nitrogen at 30°C. The organic phase was divided into two, 0.5
ml aliquots, placed in glass vials, spiked with an internal
standard (C32-n-alkane; dotriacontane), and crimp-sealed for
subsequent analysis for PAHs, 0-, S- and JV-heterocycles by
GC-FID (see ANALYTICAL METHODS).
The pH of the extracted aqueous phase was re-adjusted to
pH=7.0 through the addition of 8.5% phosphoric acid. Aque-
ous solutions were then extracted 3 times with 10 ml volumes
of methylene chloride to remove weakly acidic phenols, and
certain 0- and S-heterocycles, and transfer them to the organic
phase. The combined methylene chloride organic phases were
dried by passage through a layer of anhydrous sodium sulfate
(25 g), and collected into clean, 25 ml Kuderna-Danish con-
centrating tubes. The organic phase was reduced in volume to
1.0 ml under a stream of dry nitrogen at 30°C and placed in a
glass vial. For analysis of phenol constituents by GC-FID (see
ANALYTICAL METHODS), o-xylene was added as the in-
ternal standard.
The pH of the extracted aqueous phase was brought to
pH=2.0 by the addition of 8.5% phosphoric acid. Protonated
PCP (pKa = 4.7) was then extracted into methylene chloride
(3x, 10 ml volumes). The methylene chloride organic phase
was washed once with 10 ml distilled water, then dried by
passage through a layer of anhydrous sodium sulfate (25 g).
The organic phase was reduced in volume to 1.0 ml under a
stream of dry nitrogen at 30°C, and transferred to a glass vial.
PCP was derivatized (trimethylsilyl derivative) and determined
-------
by GC-ECD analysis (see ANALYTICAL METHODS).
Quantitation of PCP derivative was based on an external
standard curve (0.1-10 ppm), and its identity was confirmed
by GC-MS analysis (data not shown).
3.4.b Soil and Sediment Samples
The fractionation and extraction procedures used for
analysis of surface soil and sediment are outlined in Figure
3.4. For each analysis (run in duplicate), 10 g samples of soil
or sediment were placed into a 25 mm x 80 mm (internal diam
x external length) cellulose extraction thimble (Whatman
International Ltd., Maidstone, England) and Soxhlet extracted
with 100 ml methylene chloride for 4-5 hours. The methylene
chloride extracts were then prepared through a series of
liquid: liquid extractions to selectively remove PAH, phenolic
and heterocyclic components of creosote as described below.
Methylene chloride Soxhlet extracts were first washed 3
times with 15 ml volumes of IN NaOH. This procedure re-
sulted in the transfer of acidic creosote phenolics from the
organic phase into the aqueous phase. The organic phase was
washed once with 10 ml distilled water to remove residual
base, and the wash water was added to the basic aqueous
phase which was reserved. Creosote phenolics were removed
from the IN NaOH aqueous phase by carefully acidifying to
pH=2 with concentrated sulfuric acid, and extracting 3 times
with 10 ml volumes of methylene chloride. The combined
methylene chloride organic phase was washed with 10 ml
distilled water to remove residual acid (wash water and the
aqueous phase were discarded). Residual water was removed
from the organic phase by passage through a layer of anhy-
drous sodium sulfate (25 g). The organic phase was then
reduced in volume to 1.0 ml under a stream of dry nitrogen at
30°C, transferred to a glass vial, spiked with internal standard
(o-xylene), and crimp-sealed for GC-FID analysis of extracted
phenolic components of creosote (see ANALYTICAL
METHODS).
The base-extracted organic phase was subsequently ex-
tracted 3 times with 15 ml volumes of 2.5 N sulfuric acid. This
step was designed to transfer any 7V-heterocycles present in the
samples to the acidified aqueous phase. The remaining organic
phase was washed once with 10 ml distilled water to remove
residual acid (and N-heterocycles), and wash water was added
to the pooled acidic aqueous phase which was reserved.
Residual water was removed from the remaining organic
phase by passage through a layer of anhydrous sodium sulfate
(25 g). The volume of the organic phase was reduced to 1.0 ml
under a stream of dry nitrogen at 30°C, divided into two, 0.5
ml aliquots, and spiked with internal standard (C32) for
analysis of PAHs, and neutral 0- and S-heterocyclic compo-
nents of creosote by GC-FID analysis (see ANALYTICAL
METHODS).
To extract weakly basic AMieterocycles from the remain-
ing aqueous phase, the pH was adjusted to pH= 12 via the slow
addition of 10 N NaOH. The basified aqueous phase was cooled
to room temperature, then extracted 3x with 10 ml volumes of
methylene chloride. The resultant organic phase was washed
once with 10 ml distilled water to remove residual base (wash
water and extracted aqueous phase were discarded), dried
over sodium sulfate, reduced in volume to 1.0 ml under a
stream of dry nitrogen at 30°C, transferred to a glass vial and
mixed with internal standard (C32). The amount of A'-hetero-
cycles was subsequently determined by GC-FID analysis of
organic extracts (see ANALYTICAL METHODS). Quantita-
tion of monitored creosote constituents was calculated from a
standard curve for identified chemicals. The ability of this
extraction procedure to fractionate creosote constituents into
the defined groups (phenolics, PAHs, N-, S- and 0-heterocy-
clics) was verified (see QA/QC).
3.4.c Slurry Samples
Extraction of slurries was accomplished through a combi-
nation of the procedures described for the extraction of aqueous
and solid samples. The process was initiated by adjusting
duplicate, 25 ml samples of soil or sediment slurry to pH=12
with 10 N NaOH. A 10 ml volume of methylene chloride was
added directly to the slurry while still in the original I-CHEM
jar. The contents of the jar were shaken vigorously for 1 min,
then centrifuged for 20 min at 3500 rpm (NOTE: I-CHEM jars
tend to break at >4000 rpm). The resultant methylene chloride
organic layer was subsequently transferred to a clean (solvent
rinsed) 250 ml separatory funnel with a solvent-rinsed Pasteur
pipette taking care not to remove any emulsion. This procedure
was repeated twice for a total of 3 extractions at pH=10. After
the third extraction, the slurries were centrifuged a fourth time
to recover residual methylene chloride from the emulsion.
The pooled methylene chloride extracts were washed once
with 10 ml volume of distilled water to remove residual base,
and the wash water was added back to the aqueous phase
(slurry). Water was removed from the organic extract by
passage through a layer of anhydrous sodium sulfate (25 g),
and the volume of the organic phase was reduced to 1.0 ml
under a stream of dry nitrogen at 30°C. The final volume of
basic extract was divided into two, 0.5 ml aliquots and spiked
with internal standard (C^) fdr quantitative analysis of PAH
and O-, S- and Af-heterocyclic components of creosote (see
ANALYTICAL METHODS).
The aqueous slurry was adjusted to pH=7.0 with concen-
trated phosphoric acid, and extracted 3x with 10 ml volumes
of methylene chloride as described above. The centrifugation
step was reduced to 10 minutes. The fourth centrifugation
following extraction was still necessary since residual methyl-
ene chloride was recoverable from the emulsion. Residual
water was removed from the combined organic phase by
passage through a layer of anhydrous sodium sulfate (25 g),
the volume was reduced to 1.0 ml under a stream of dry
nitrogen at 30°C and transferred to a glass vial. For analysis of
phenolic constituents, o-xylene was added as the internal
standard (see ANALYTICAL METHODS).
Lastly, PCP was extracted from the slurries by carefully
acidifying the aqueous phase to pH=2 with concentrated
phosphoric acid and extracting 3 times with 10 ml volumes of
methylene chloride. Samples were centrifuged between each
extraction. For analysis by GC-ECD, PCP was derivatized to
facilitate its chromatographic determination (see ANALYTI-
CAL METHODS). Recovery of derivatized PCP was calcu-
lated from an external standard.
3.4.d Extraction of PCP from Soils
The amount of PCP in soil and sediment was determined
by placing duplicate 5.0 g samples into clean, 125 ml Erlen-
10
-------
25 ml groundwater placed in a 60-ml separatory funnel. Aqueous
solutions basified to pH=2 with 1N NaOH then extracted 3x with 10-ml
volumes of methylene chloride.
Wash with 10 ml distilled water (dHsO)
Remove water from organic phase
with anhydrous sodium so/fate
Adjust to pH=7.0 with 8.5% phosphoric
acid.; extract 3x with 10-ml volumes of
methylene chloride
I
c
PAH and N-, S-, O-
heterocyde fractions
J
\
Organic
phase
|
Wash with 10 ml dH 2O
\
Aqueous
phase
t
Remove water from organic phase
with anhydrous sodium sulfate
Phenolic fraction
andPCP
J
Acidify aqueous phase to pH=2 with
8.5% phosphoric acid and extract 3x
with 10-ml volumes of methylene
chloride
Aqueous
phase
•*•
discard
\
Wash organic phase with 10 ml distilled water, and dry with 25 g
anhydrous sodium sulfate
POP fraction
Figure 3.3
Flow chan for extraction and chemical analysis of aqueous samples.
11
-------
V
10 grams of soil placed into a cellulose extraction thimble and Soxhlet
extracted with 100 ml methylene chloride for 4-5 hours
Methytene chloride organic phase I
I
Extract 3x with 15 ml IN NaOH
\
Aqueous
phase
\ I
Wash organic phase once with 15 ml distilled
water (add to aqueous phase)
I
Organic
phase
I I
L I
Acidify aqueous phase to pH=2; cool to
room temperature and extract 3x with 10 ml
methylene chloride.
I
1
• "^v
Aqueous A
phase ^^/
\ Wash (10 ml
I
Organic
phase
water) \
I
Dry organic phase by draining over
25 g anhydrous sodium suHate
c
Phenolic fraction
I
Extract 3x with 15 ml 2.5N
sulphuric acid
I
Wash (10 ml water)
Slowly basify to pH= 12 with NaOH;
cool to room temperature and extract
3x with 10 ml methylene chloride
Dry with 25 g anhydrous
sodium sulfate
PAHs
O-, S-heterocycles
Discard
N-heterocycles
J
Dry organic phase with 25 g
anhydrous sodium sulfate
Figure 3.4 Flow chart for extraction and chemical analysis of soils and sediments.
Figure 3.4Flow chart for chemical analysis of soils and sediments
12
-------
meyer flasks fitted with Teflon-lined screw-caps (Figure 3.5).
To each flask was added IS ml methanol, and the methanol
slurry was carefully acidified to pH=2 with concentrated
sulfuric acid. The transfer of PCP to the organic phase was
facilitated by mixing (150 rpm) for at 4-5 hours at room
temperature. The soil/methanol slurry was then charged with
10 ml of 0.1 M HC1/0.1 M KC1, and filtered under vacuum
through a Whatman no. 1 filter paper. The filter was washed
with ca. 5 ml hexane and 5 ml distilled water. Wash solutions
were added to the filtrate. The combined filtrate and washes
were then extracted 3x with 5 ml volumes of hexane. The
pooled hexane phase was reduced in volume to 1.0 ml under a
stream of dry nitrogen at 35°C. As the hexane phase used to
extract PCP from soil or sediment was reduced in volume, a
precipitate was usually formed. Thus, once the volume was
reduced to 1.0 ml, it was necessary to filter hexane extracts
through a 0.2 micron Teflon filter (Gelman Sciences, Ann
Arbor, MI). Prior to injection and analysis of PCP by GC-
ECD, PCP was derivatized to facilitate its chromatographic
determination (see ANALYTICAL METHODS). Recovery
of PCP was calculated from an external standard curve (see
QA/QC), and its identity was confirmed by mass spectral
analysis (data not shown).
3.4.e Activated Carbon Traps
The contents of each trap were emptied into separate 125
ml Erlenmeyer flasks fitted with Teflon-lined screw-caps. To
each flask was added approximately 25 ml of methylene
chloride, and slurries were shaken at 100 rpm for 24 hours at
room temperature. The methylene chloride/carbon slurries
were then separated by filtration through a Whatman no. 1
filter paper. Residual moisture was removed from the meth-
ylene chloride organic phase by passage through a layer of
anhydrous sodium sulfate (25 g), then reduced in volume to
2.0 ml under a stream of dry nitrogen at 30°C. The final
volume was divided into 4x, 0.5 ml aliquots which were
analyzed for PAH, phenolics, heterocyclics, and PCP, respec-
tively. Due to low levels of creosote organics in the activated
carbon traps, differential extractions were not performed.
3.5 Analytical Methods
3.5.a PAHAnalysis
The amounts of PAH components of creosote in soil,
sediment, aqueous samples, slurries, and activated carbon
traps were determined by gas chromatographic analysis of
organic extracts of these materials. Analyses were performed
on a Hewlett-Packard Model 5890 Series II gas chromatograph
equipped with cryogenics, two autosamplers, two injection
ports, and two flame ionization detectors (FID). Hydrogen
was used as the carrier gas (linear velocity 48 cm/sec) while
air (250 kPa) and hydrogen (150 kPa) were supplied for the
FID. Nitrogen (flow rate 30 ml/min) was used as the make up
gas for the detector. Creosote PAHs (present in duplicate 1.0
Hi injections) were separated on an SPB-5 (Supelco, Bellafonte,
PA) capillary column (15 m x 0.32 mm [inside diam] with a
0.25 urn film thickness). The temperature program was as
follows: 30°C for 3 min followed by a linear increase of 5°C/
min to 300°C where it was held for 4 min. Injector and
detector temperatures were maintained at 300 and 310°C,
respectively. The amounts of targeted compounds present
were calculated by comparing peak area obtained by duplicate
1.0 pi injections with standards for each chemical and related
to the amount of internal standard (C32). The limit of detection
for PAHs was set at 400 ppb.
3.5.b N-, S-, O-Heterocycles
The amounts of creosote heterocycles in organic extracts
were determined by gas chromatographic analysis as de-
scribed for PAHs. However, the temperature program was
slightly modified to facilitate the separation of creosote het-
erocycles: initial temperature of 25°C for 1 min followed by a
linear increase of 5°C/min to 300°C. The amounts of targeted
compounds present were calculated by comparing peak area
obtained by duplicate, 1.0 |il injections with those of standards
of each chemical and related to the amount of internal standard
(C32). The limit of detection for creosote heterocycles was set
at 100 ppb.
3.5.C Phenol Analysis
Phenolic compounds, excluding PCP, were identified and
quantified by GC-FID analysis on a Hewlett-Packard model
5890 gas chromatograph equipped with dual injection ports,
dual columns, an autosampler, a FID detector, and an electron
capture detector (ECD). Phenolic compounds were separated
with a Nukol (Supelco) fused silica capillary column (30 m x
0.25 mm [inside diam], 0.25 Jim film thickness) connected to
the FID detector. Hydrogen (linear velocity 48 cm/sec) was
used as the carrier gas while air (250 kPa) and hydrogen (150
kPa) were supplied for flame ionization. Nitrogen (flow rate
of 30 ml/min) was used as the make up gas for the detector.
The oven temperature was programmed as follows: 40°C for 3
min followed by a linear increase of 25°C/min to 150°C
where it was held for 10.2 min, then increased at a rate of 5°C/
min to 200°C where it was held for 15 min. Injector and
detector temperatures were maintained at 180°C and 220°C,
respectively. For quantitation of phenolic compounds present
in the organic extracts, o-xylene was used as the internal stan-
dard. The amounts of targeted compounds present were calcu-
lated by comparing peak area obtained by duplicate injection
(1.0 pi) with standards for each chemical in relation to the
amount of internal standard. The limit of detection for creosote
phenolics was set at 50 ppb.
3.5.d PCP Analysis
Extracted PCP was quantitatively analyzed as its
trimethylsilyl derivative (using BSTFA (N,O-
b/s[trimethylsilyl]trifluoroacetamide)) by gas chromatographic
analysis employing a Hewlett-Packard model 5890 gas chro-
matograph equipped with dual injection ports, dual columns, a
FID detector and an ECD detector. Pentachlorophenol deriva-
tives were injected onto a SPB-5 capillary column connected
to the 63Ni-electron capture detector. Hydrogen (linear veloc-
ity 48 cm/sec) was used as the carrier gas and P-10 (flow
rate=30 ml/min) as the ECD make up gas. Column tempera-
ture was programmed for 50°C for 0.5 min followed by a
linear increase of 10°C/min to 180°C, then 25°C/min to
290°C where it was held for 5 min. Injector and detector
temperature was maintained at 150°C and 300°C, respectively.
For quantitative analysis of PCP, the amount of targeted
compound present in duplicate, 1.0 \i\ injections was calcu-
lated by comparing its peak area with that of derivatized-PCP
standards. The limit of detection for PCP was set at 50 ppb.
13
-------
5 grams of soil placed In a 125-ml Erienmeyor flask; add 15 ml methanol
and acidify to pH=2 with 12 N sulfuric acid
shake (150 rpm) for 4 hours at room temperature
Methanol/soil slurry
Charge slurry with 10 ml 0.1 M HCI/0.1 M KCI and filter through a Whatman
no. 1 filter paper. Wash filter with distilled water andhexane (5.0 ml)
Filtrate
Extract filtrate 3x with 5 ml hexane
Pass hexane extracts through a 0.2 micron Teflon filter
to remove precipitate
PCP fraction
J
Figure 3.5
Flow chart for extraction and analysis of PCP in soils.
3.5.e CLP Analyses
see APPENDIX
3.5.f Microbial Population Counts
Microbial population counts were obtained for both soil
and sediment at time-zero and after 1, 2,4, 8 and 12 weeks
incubation in the land-farming chambers. Total heterotrophic
bacterial counts were obtained by serially diluting duplicate,
1.0 g samples of soil or sediment (stored at 4°C in clean,
sterile I-CHEM jars) to 10* in sterile, 2.5 mM phosphate
buffer (pH=7.1). For surface soil, duplicate, 0.1 ml samples
from lO^-lO"8 dilutions were spread-plated onto complex me-
dium (AB3 agar, Difco Laboratories, Detroit, MI) whereas
sediment samples were plated at dilutions from 10"2 to 10-s
(additional dilutions plated if necessary). Plates were incu-
bated at 30°C for 3 days prior to counting.
In an effort to establish a better correlation between total
heterotrophic plate counts and in situ creosote-biodegradation
potential, phenanthrene was used as a reporter chemical to
determine the number of cultured organisms potentially ca-
pable of degrading this creosote constituent. The number of
phenanthrene-degrading microorganisms was determined by
spraying AB3 plates containing between 30 and 300 indi-
vidual colonies with an ethereal solution of phenanthrene
(0.04% phenanthrene). As the ether evaporated, this proce-
dure resulted in the deposition of a thin film of phenanthrene
on the surface of the agar medium. Plates were incubated for 3
more days at 30°C after which time the number of phenan-
14
-------
threne-degrading microorganisms was determined by record-
ing the number of colonies which cleared the hydrocarbon
substrate.
Microbial populations from the bioreactor and groundwa-
ter shake-flask studies were measured after treatment with
NaOH using the bicinchoninic acid (BCA) protein assay
(Pierce Chemical Co., Rockford, IL).
3.5.g Percent Moisture Content
The moisture content of soil and sediment in the land-
farming chambers was measured intermittently as follows:
duplicate, 1.0 g samples were weighed into tared trays and
dried at room temperature for 3 days. The percent moisture of
each material was subsequently calculated:
% moisture- wet W0ight- dry weightx 100
wet weight
3.6 Microtox Assays
Toxicity of various samples was determined with a
Microtox model 500 toxicity autoanalyzer (Microbics Corp.,
Carlsbad, CA). This system was used according to manufac-
turer specifications to generate data on the toxicity of ground-
water and soil slurries before and after treatment. Where
appropriate these data were used in conjunction with teratoge-
nicity data to thoroughly evaluate the extent of removal of
hazardous components from various media. Since the Microtox
system can only analyze aqueous samples, soil and sediment
from the land-farming chambers were not analyzed.
3.7 Teratogenicity Assays
Teratological responses in inland silversides (Menidia
beryllind) embryos exposed to materials from the ACW site
before and after treatment were evaluated. Preliminary studies
have shown that this test organism offers a sensitive indicator
for the presence of creosote and PCP (data not shown).
Naturally spawned embryos from an adult population of sil-
versides, maintained in the laboratory at 25°C and 5%o salinity
in the absence of teratogenic substances, were used for all
tests.
To initiate experiments, blastula stage embryos were
washed 5 times with sterile fresh water of moderate hardness
(80-100 mg/L CaCO.,), and single embryos were placed in
each of 120 randomized Leighton culture tubes. Six ml of
clean, sterile media, or waste sample to be evaluated (untreated
groundwater, treated groundwater, untreated surface water
[creek water], soil slurry, sediment slurry), were added to each
of 30 tubes to yield: a) 30 control tubes with a single embyro
in each tube, b) 30 tubes containing 100% waste sample with
a single embryo in each tube, c) 30 tubes with a 1:10 dilution
of waste sample, and d) 30 tubes with 1:100 dilution of waste
sample. Tubes were sealed with Teflon-lined screw-caps,
placed in stainless steel racks, and incubated in a horizontal
position at 25°C with a photoperiod of 14 hr light: 10 hr
darkness.
On a daily basis, tubes were removed from the incubator
and individual embryos were viewed microscopically to de-
termine the presence or absence of terata. A ranking system
was used to assign numerical values for the severity of re-
sponses in three important organ systems within the develop-
ing embryos: a) the craniofacial-central nervous system (CR),
b) the cardiovascular-circulatory system (CV), and c) the
skeletal system (SK). Teratological responses were documented
with photomicrography.
Seven to eight days after exposure, control embryos
hatched. The minimum acceptable percentage hatch of control
embryos was 80% (if less than 80% experiments were re-
peated). All hatched larvae were immediately examined mi-
croscopically to determine the extent of impact on CR, CV
and SK systems. Total test duration did not exceed 10 days,
and the dissolved oxygen and pH of the medium of represen-
tative tubes was determined at the end of each test. Prelimi-
nary studies showed that inland silversides are very suscep-
tible to the complex aqueous phase of creosote/PCP residues,
and that this test system offered a very sensitive indicator of
teratogenic/toxic components of creosote.
3.8 Quality Assurance/Quality Control
The Biotreatability Study Work Plan describing these
studies was submitted to the U.S. EPA Environmental Moni-
toring Systems Laboratory (Las Vegas, NV) for review. Par-
ticular attention was paid to experimental design and statisti-
cal soundness. By and large, QA/QC is limited to the procedures
for extracting creosote constituents from contaminated mate-
rials and their subsequent analysis.
For analysis of PAH, O-, S-, and W-heterocycles, and
phenolic components of creosote, various dilutions of stan-
dard mixtures of targeted chemicals in each group were used
for daily instrument calibration. For PCP analysis, PCP stan-
dards were used for instrument calibration. Level 1 concentra-
tions for each standard mixture are reported in Tables 3.3,3.4
and 3.5. Levels 2,3, and 4 were prepared by diluting the Level
1 standards 10-, 100-, and 1000-fold, respectively. When
necessary, other dilutions were made in order to generate a 3-
point calibration curve within the appropriate range. The
lowest level of each standard was used to verify the limit of
detection (LOD) for individual chemicals. If the LOD was
exceeded, then corrective measures were taken (i.e., septum
change, insert change).
Instrument performance was verified using standard ref-
erence materials (SRM), quality control (QC) samples, and
performance evaluation (PE) samples obtained from the U.S.
EPA Quality Assurance Branch, Environmental Monitoring
Services Laboratory (Cincinnati, OH). Standards were run as
unknowns every sixth sample to monitor instrument perfor-
mance, and methylene chloride blanks were injected daily as
contamination checks.
The quantitative analysis of targeted compounds was
based on the presence of the internal standards. For PAH and
N-, S-, and 0-heterocycle analyses, exactly 10 p.1 of a
dotriacontane stock solution (1.0 mg C32in 1.0 ml hexane) were
added to each 1.0 ml organic extract sample (or exactly 5 nl to
0.5 ml sample) at the time of extraction (see EXTRACTION
PROCEDURES). All measurements were based on the pres-
ence of this standard. Likewise, 0-xylene was used as the in-
ternal standard for the analysis of phenolic compounds in
organic extracts.
15
-------
The ability to extract creosote constituents from soil and
water substrates was verified by processing samples to which
known amounts of authentic chemical standards had been
added. Percent recovery for each component was subsequently
determined. Likewise, the ability of the various fractionation
schemes to differentially extract related groups of contami-
nants was verified.
Table 3.4 Standard Mixture of 10 Phenolic Constituents of
Creosote Used for Instrument Calibration and
Determination of Detection Limit
Com-
pound1
1
2
3
4
5
6
7
8
9
Chemical2
2,6-xylenol
o-cresot
2,5-xylenol
2,4-xylenol
p-cresol
m-cresol
2,3-xylenol
3,5-xylenol
3,4-xylenol/
2, 3. 5-trimethylphenol
Level 1
Concentration
frg/ml)
52.1
35.0
54.2
48.0
38.1
52.0
51.4
52.2
77.0
' Compounds listed in order of elution.
* All compounds used were of the highest purity available (>98%).
Table 3.3 Standard Mixture of 22 PAH Components of
Creosote Used for Instrument Calibration and
Determination of Detection Limit
Level 1
Com-
pound1
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
Chemical1
naphthalene
1-methylnaphthalene
2-methylnaphthalene
biphenyl
2,6-dimethylnaphthalene
2, 3-dimethylnaphthalene
acenaphthene
acenaphthylene
fluorene
phenanthrene
anthracene
2-methylanthracene
anthraquinone
fluoranthene
pyrene
benzo[b]fluorene
benz[a]anthracene
chrysene
benzo[b]fluoranthene/
benzo[k]fluoranthene
benzo[a]pyrene
indeno[1,2,3-c,d]pyrene
Concentration
(\ng/ml)
105.4
102.5
103.7
102.3
137.3
100.2
102.1
112.6
102.3
106.1
105.8
100.7
128.8
128.7
102.3
101.5
200
102.0
70.0
114.7
10.0
'Compounds listed in order of elution.
'All compounds used were of the highest purity available
Table 3.5 Standard Mixture of 13 N-, S-, and O-Heterocyclic
Constituents of Creosote Used for Instrument
Calibration and Determination of Detection Limit
Com-
pound1
1
2
3
4
5
6
7
8
9
10
11
12
Chemical2
2-picoline
3-picoline/
4-picoline
lutidine
thianaphthene
quinoline
isoquinoline
quinaldine
lepidine
dibenzofuran
dibenzothiophene
acridine
carbazole
Level 1
Concentration
(\ng/ml)
50.0
112.0
45.0
102.0
100.0
112.0
103.0
100.0
100.0
92.0
98.0
100.0
'Compounds listed in order of elution.
*AII compounds used were of the highest purity available
16
-------
4. Results and Discussion
4.1 Compound Identification Numbers
The efficacy of various biotreatability efforts was evalu-
ated primarily by monitoring the fate of PCP and 42 compo-
nents of creosote. For the sake of simplicity, all data tables
make use of compound identification numbers as opposed to
continually listing each of these compounds. Table 4.1 identi-
fies the chemical which corresponds to each compound ID
number. In the text, brackets, [ ], indicate when a compound
ID number is being used in reference to a specific chemical. In
the cases where two chemicals co-elute, an individual number
refers to the mixture [20,30,33].
4.2 Extraction Efficiency
Recovery of PCP and 42 creosote constituents from the
spiked soil and water samples are summarized in Table 4.2. In
an effort to obtain soils of similar type and texture as those
used in actual studies, samples were obtained from just outside
the fenced area of the ACW site. However, as is apparent from
the background data listed in Table 4.2, these materials con-
tained relatively high concentrations of high-molecular-weight
PAHs. Therefore, when the background concentration of indi-
vidual chemicals was high in relation to the amount added in
the matrix spike, percent recoveries were impossibly high
(>500%j. This was most apparent with compounds [20 and
21] where the background concentration was 4 and 10-times
greater than the spike concentration, respectively. Neverthe-
less, the ability to recover from soil at least 85% of the
contaminants present was consistently established, and recovery
values were within acceptable limits.
Recovery of spiked materials from aqueous substrates
were also within acceptable limits. Excluding lutidine [34],
efficiency of extraction for all chemicals was consistently
>70%.
4.3 Groundwater Shake Flask Studies
Preliminary studies evaluating the potential for bioreme-
diation of creosote- and PCP-contaminated groundwater at
the ACW site demonstrated that many of the contaminants
present in this material may be attacked by the indigenous
microflora (Table 4.3). While the phenolic components [22-
30] were readily biodegraded, a short acclimation period was
apparently required before the soil microorganisms degraded
resident PAHs [1-21]. With the exception of anthracene [11]
and 2-methylanthracene [12], most PAHs with molecular
weights less than that of fluoranthene [14] were extensively
biodegraded after 5 days incubation. No degradation of PCP
was evident.
The catabolic abilities of these organisms appears to have
been realized within 8 days of incubation since most of the
observed changes had occured by this time. However, some
low-level activity or secondary catabolism may have contin-
ued since the concentration of the high-molecular-weight
PAHs decreased with continued incubation. A shift in the
microbial population may also have contributed to this de-
crease. The concentration of all constituents in the killed cell
controls did not decrease with time (data not shown), hence
observed losses could be directly attributed to biological
activity.
From the analytical chemistry data described above, it
was determined that, with the exception of PCP, all monitored
contaminants were extensively degraded by the indigenous
microflora after 14 days incubation. However, data generated
from both the Microtox and teratogenicity assays showed that
the bioremediated groundwater was still capable of eliciting a
response. Microtox assays showed an ECj,, of 0.72 (a solution
containing 0.72% of the parent material killed 50% of the test
organisms) for filtered (silanized glass wool), untreated
groundwater freshly recovered from the ACW site (well 320).
An ECjjOf 3.8 was observed for filtered groundwater exposed
to biological activity for 14 days.
Teratogenicity assays showed that filtered, untreated
groundwater freshly obtained from Well no. 320 at the ACW
site was embryo toxic at 100%, and teratogenic at 10 and 1%
concentrations (Table4.4). At the 1% concentration, all hatched
larvae had terata, including stunted skeletal axes and deformed
hearts. Bioremediation of Well no. 320 groundwater did not
reduce the embryo toxicity/teratogenicity at the 100 and 10%
groundwater concentrations, but the 1% test solution demon-
strated marked improvement: 78% of the embryos that hatched
produced normal larvae while only 11% developed observ-
able terata. This sharply contrasts with that observed with
untreated groundwater (no normal larvae, 20% terata at the
1% solution).
Preliminary studies have shown that the creosote con-
stituents present in groundwater at the ACW site are suscep-
tible to biodegradation. However, the following points must
be considered: 1) studies were performed under well mixed,
aerobic conditions, 2) copious amounts of inorganic nutrients
were available, 3) relatively high concentrations (27 ng bacte-
rial protein/25 ml medium) of surface soil microorganisms
were used to inoculate each flask, and 4) the tests were
performed within a closed system. Therefore, the rates and
extents of degradation observed in the laboratory probably do
not accurately reflect those occurring in situ. Nevertheless, the
potential for treating creosote-contaminated groundwater
through biological processes has been demonstrated.
17
-------
Table 4.1 Chemicals Corresponding to Compound
Identification Numbon
Chemical Compound ID Number
naphthalene
2-methylnaphthalene
1-methylnaphthalene
biphenyl
2,6-dimethylnaphthalene
2,3-dimethylnaphtahlene
acenaphthylene
acenaphthene
fluorene
phenanthrene
anthracene
2-methylanthracene
anthraquinone
fluoranthene
pyrene
benzo[b]fluorene
chrysene
benzo[a]pyrene
benz[a]anthracene
benzo[b]fluoranthena/
benzo[k]fluoranthene
indeno[1,2,3-c,d]pyrene
2,6-xylenol
o-cresol
2,5-xylenol
2,4-xylenol
p-cresol
m-cresol
2,3-xylenol
3,5-xylenol
3,4-xylenol/
2,3,5-trimethylphenol
pen tachlorophenol
2-picoline
3-picoline/
4-picoline
lutidine
thianaphthene
quinoline
isoquinoline
quinaldine
lepidine
dibenzofuran
dibenzothiophene
acridine
carbazole
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
4.4 Solid-Phase Bioremediation
The biological degradation and subsequent removal of
PCP and 42 creosote constituents from contaminated sedi-
ment and surface soil obtained from the ACW site was
monitored for 12 weeks while samples were incubated in
specially designed, closed-system land-farming chambers.
Evidence for biodegradation of targeted compounds was based
primarily on GC analyses of extracted substrates. In addition,
change in microbial populations (total heterotrophic plate
counts, and the number of phenanthrene-degrading bacteria)
was used as a secondary, or indirect, indication of biological
activity towards targeted contaminants.
Table 4.5 presents analytical chemistry data for solid-
phase bioremediation of unamended surface soil. By and
large, contamination was limited to PAHs and PCP. Table 4.6
summarizes the loss of creosote constituents via volatilization
from surface soil during solid-phase bioremediation. Overall,
loss via volatilization was less than 0.01% (ca. 28 (ig organic
creosote constituents recovered from activated carbon trapjv
ca. 30,000 mg total creosote per land-farming chamber;.
Despite this rather low percentage, these data were used in
conjunction with analytical chemistry data to quantify accu-
rately the percent biodegradation of individual components of
creosote. Percent biodegradation data are presented in Table
4.7, but only the data for week 12 have been corrected for the
cumulative loss of individual creosote components by volatil-
ization.
In the absence of inorganic supplements, the first week of
solid-phase bioremediation did not result in a significant loss
of monitored creosote constituents from contaminated surface
soil (Table 4.7). Although biodegradation of most monitored
contaminants continued with further incubation, most of the
biodegradation of monitored contaminants was realized by
the end of the second week of incubation. Exceptions to this
generalization include compounds [5], [11] and [12] whose
biodegradation did not appear to be initiated until week 8.
Hence, the pattern of creosote biodegradation was predictable:
lower-molecular-weight contaminants [compounds 1 through
9] were degraded more readily than the higher molecular-
weight molecules [compounds 10 through 21 and 31], and
creosote constituents containing 4 or more fused rings [com-
pounds 14 through 21] tended to resist biological attack.
Changes in the concentration of monitored creosote con-
stituents during solid-phase bioremediation of surface soils
amended with inorganic nutrients are summarized in Table
4.8, and loss of these contaminants via volatilization is shown
in Table 4.9. Again, loss from surface soils through volatiliza-
tion was less than 0.01%, but quantitation of abiotic loss was
necessary to determine accurately the rate and extent of
creosote degradation attributable to biological activity (Table
4.10).
When compared with data presented in Table 4.7, it is
apparent that both the rate and extent of biodegradation was
stimulated by the addition of soluble nutrients (Table 4.10).
Since nutrient supplementation cannot increase the aqueous
solubility of the more recalcitrant molecules, this stimulatory
effect was most pronounced with the readily biodegradable
components of creosote. With the exception of compounds
[10] and [16 -19], the amount of material biodegraded within
the first week of incubation was greater when treated with
soluble inorganic nutrients. Subsequent additions of inorganic
nutrients appeared to further enhance the loss of biodegrad-
able contaminants. By the end of the study, the extent of
biodegradation in the presence of soluble inorganic nutrients
was greater for ah* monitored contaminants except for com-
pounds [3], [19] and [31].
Changes in soil microbial numbers during solid-phase
bioremediation of creosote-contaminated surface soils with
and without nutrient amendments are presented in Table 4.11.
While analytical chemistry data suggest that the addition of
inorganic nutrients stimulated the rate and extent of creosote
biodegradation, total heterotrophic plate counts obtained with
18
-------
unamended soils and with those that received nutritional
supplements do not reflect such an effect. However, after 4
and 8 weeks of incubation, the number of phenanthrene-
degrading microorganisms was significantly greater in the
soils that had received inorganic nutrients. This increase could
be correlated with higher values for percent biodegradation of
phenanthrene and other higher molecular-weight PAHs ob-
served at these time points with soils amended with soluble
nutrients (Tables 4.7 and 4.10).
Changes in the concentration of monitored chemicals
during solid-phase bioremediation of unamended sediment
are summarized in Table 4.12. On the whole, loss of PCP and
creosote constituents from sediments was only 0.7% (Table
4.13). However, volatilization of individual components
[compounds 1 and 2] was much higher. When analytical
chemistry data were combined with the observed losses via
volatilization, percent biodegradation of individual compo-
nents was calculated accurately (Table 4.14).
As was observed with the unamended surface soils (Table
4.7) the rate of biodegradation was slow and the pattern of
biodegradation was predictable. From the data presented, the
extent of biodegradation (as determined by percent biodegra-
dation after 12 weeks incubation) appears to have been less
with the unamended sediment than with the unamended sur-
face soil. However, since the data are presented on a percent
basis, the actual biodegradation must be considered as a
function of creosote loading rate. Therefore, the actual amount
of carbon turnover in the unamended sediments was greater
than that observed in the unamended surface soils. Neverthe-
less, unamended sediments still contained a very high concen-
tration of creosote after 12 weeks incubation in the land-
farming chambers.
Tables 4.15 and 4.16 summarize respectively creosote
recovery data from creosote-contaminated sediments follow-
ing 12 weeks of solid-phase bioremediation with inorganic
nutrient amendments, and loss of PCP and 42 monitored
creosote constituents via volatilization over this time frame.
Loss of creosote constituents from sediments amended with
inorganic nutrients was 1.9% over the 12 week incubation
time. In combination with the volatilization values reported
above for unamended sediment, it appears that volatilization
was greater with the sediment materials than with the surface
soils. Despite the relative insignificance of these values, abi-
otic losses such as volatilization were considered when calcu-
lating percent biodegradation values (Table 4.17).
In contrast to the results obtained with surface soils, the
addition of inorganic nutrients did not exert a stimulatory
effect on the rate of biodegradation of monitored constituents
in sediments. For the lower molecular weight PAHs, final
values for % biodegradation after 12 weeks incubation were
roughly equivalent with or without nutrient amendments.
However, inorganic nutrient supplementation appeared to have
a positive effect on the extent of biodegradation of the higher-
molecular-weight components of creosote.
For both sediment treatments, the total heterotrophic
populations were equivalent throughout the incubation period
(Table 4.18). At the beginning of the experiments, microbial
counts were very low presumably due to the high pH (pH=10)
and degree of contamination (5% creosote). With continued
incubation, however, microbial populations appeared to have
adapted to this environment as evidenced by a significant
increase in both the total heterotrophic plate counts and
phenanthrene-degrading counts after 8 weeks incubation. This
increase in microbial numbers correlated well with a decrease
in the concentration of monitored contaminants (Tables 4.12
and 4.15). Moreover, the number of phenanthrene-degraders
was approximately 100 times greater in the nutrient-amended
sediment than in the unamended material which may be
related to the greater degradative activity against high-mo-
lecular-weight PAHs observed with this treatment.
4.5 Slurry-Phase Bioremediation
On April 6 and 7, 1990, approximately 100 Ibs of both
creosote-contaminated surface soil from grid 47 and sediment
were washed on site by Chapman, Inc. (Freehold, New Jersey).
The resultant slurry phases devoid of large (>2 mm diam),
uncontaminated solids were to be used for slurry-phase bio-
degradation studies. However, the surfactant used to facilitate
dispersion and the transfer of creosote constituents into the
aqueous phase (Nancy B) was shown to be toxic and
bacteriocidal. Furthermore, it was later discovered that the
washing agent used was considered proprietary. Therefore,
this process was repeated (see APPENDIX A) and a second
batch of slurries was used in these studies.
Changes in the concentration of monitored chemicals
during slurry-phase bioremediation of surface soils are pre-
sented in Table 4.19. While loss via volatilization was insig-
nificant (Table 4.20), relatively high concentrations of the
higher-molecular-weight PAHs [compounds 7 through 21]
and PCP [31] were found in the bioreactor sludge and resi-
dues. Although Triton X-100 was present to enhance the
solubility of these compounds, abiotic loss through physical
adsorption had occured.
Since loss of monitored compounds through abiotic pro-
cesses was quantified, calculations were made to determine
accurately the actual amount of PCP and each monitored
creosote constituent biologically degraded in the bioreactor
over time (Table 4.21). In general, the % biodegradation of
each compound did not increase after 14 days of incubation.
Hence, with the exception of napthalene [1], the extent of the
biological activity against each compound was fully realized
within 14 days of incubation.
As was observed with solid-phase bioremediation of sur-
face soils, indigenous microorganisms readily degraded lower-
molecular-weight PAHs and phenolic components of creo-
sote, but the higher-molecular-weight molecules and PCP
resisted biological attack. After 14 days of incubation, only 35
to 50% of the high-molecular-weight PAHs containing 4 or
more fused rings were biodegraded. With continued incubation
(21 and 30 days), only benzo[b]fluorene [16] underwent fur-
ther degradation. Therefore, slurry-phase bioremediation em-
ploying indigenous microorganisms offers an advantage over
solid-phase bioremediation of these materials in terms of time
(14 days vs. 12 weeks). However, neither approach resulted in
extensive degradation of the more recalcitrant contaminants
when indigenous microorganisms were employed as
biocatalysts.
19
-------
Table 4.2 Recovery of POP and 42 Creoaote Conatltuenta from Spiked Soil and Water Samplea from the ACW Site, Penaacola,
Florida
Compound Background Amount Recovery3
ID' Number Concentration* Added Soil Water
W/mf> \ig/mr> % %
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
6.4
5.6
1.8
U
U
8.5
U
10.3
4.0
16.0
15.7
6.5
9.8
56.1
56.9
10.4
41.3
50.3
13.2
61.7
21.5
U
U
U
U
U
U
U
U
U
1.1
—
—
0.3
0.9
0.05
0.3
7.2
1.7
5.6
3.2
3.3
9.1
52.5
50.0
47.0
49.5
49.5
58.0
48.0
54.5
47.5
55.0
56.0
53.5
51.0
52.5
45.5
49.0
55.5
54.5
5.0
14
2.8
20.0
16.0
18.0
39.0
40.0
60.0
22.0
38.0
94.0
52.0
—
—
30.0
3r.o
28.0
48.0
30.0
46.0
32.0
28.0
16.0
19.0
92
93
107
95
100
85
140
100
116
128
109
108
125
202
169
99
207
116
183
586
665
36
43
50
37
28
39
44
48
47
114
—
—
18
29
9
76
207
130
73
28
57
128
90
87
87
78
80
80
80
78
87
94
80
73
138
100
102
100
100
100
107
97
96
71
71
73
70
71
70
75
76
72
102
—
—
57
74
88
78
165
152
90
101
163
118
' Chemicals identified in Table 4.1.
'Average of duplicate analyses on 10 g samples of soil.
3 Average of triplicate independent analyses.
4 U=undotected (below LOD).
20
-------
Table 4.3
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
Concentration In ng/ml' of PCP and Selected Creosote Constituents In Groundwater Subjected to the Action of
Indigenous Microorganisms (Groundwater Shake Flask Study)
Incubation Time (Days)
Time-Zero
28.7
4.7
9.5
3.0
2.4
1.3
0.6
13.6
11.6
32.8
4.7
5.2
3.3
16.2
10.4
2.5
2.7
2.1
2.9
2.9
1.9
1.1
4.2
0.1
0.2
2.0
2.5
0.2
1.3
0.4
0.1
1
17.2
3.0
5.7
1.7
1.4
0.8
0.3
9.0
7.8
23.5
3.2
3.7
2.1
11.5
7.8
1.7
1.8
0.5
2.0
2.8
1.3
0.6
2.7
U
U
0.1
1.9
0.1
0.5
0.1
0.3
3
0.1
U
2.1
1.2
1.2
0.5
0.4
8.3
8.0
23.1
3.0
3.7
1.9
11.5
7.3
1.7
1.8
U
2.0
2.0
1.4
0.2
0.3
U
U
U
U
U
0.2
0.1
0.1
5
U
U
1.5
U
1.2
0.8
0.6
9.6
5.2
15.4
2.7
4.0
U
13.3
8.2
1.8
2.0
U
2.0
2.1
1.4
0.1
0.2
U
U
U
U
U
0.1
0.1
0.1
8
0.1
0.1
U
U
1.0
0.7
0.6
9.7
1.8
0.3
2.2
4.2
U
13.5
8.3
2.0
2.1
U
2.2
2.1
1.2
0.1
0.2
U
U
U
U
U
U
U
0.1
14
U
U
U
U
0.3
0.2
0.2
1.8
0.1
U
0.5
1.5
U
7.6
4.7
1.2
1.2
0.9
1.3
1.7
0.9
U
U
U
U
U
U
U
U
U
0.1
' Data reported are the averages of duplicate samples.
U=undetected (below LOD).
Changes in the aqueous concentration of monitored con-
stituents over time during slurry-phase bioremediation of
creosote- and PCP-contaminated sediment are summarized in
Table 4.22. Given the high degree of contamination of this
material, data are reported as milligrams (mg) per bioreactor
(all other tables report data in jig). The loss of each monitored
compound via volatilization is reported in Table 4.23. Loss
via volatilization was greatest in this system compared to all
others tested. However, percent loss via volatilization was
small in relation to the high concentration of material in the
sediment slurry. Large amounts (0.5 to 30 mg) of the higher
molecular-weight PAHs were recovered from the sludge and
water-insoluble residues of the bioreactor. Hence, losses via
physical adsorption were quite significant: 36% of the pyrene
[15] originally present in the sediment slurry was recovered
from bioreactor residues. Hence, abiotic removal processes
contributed greatly to the observed decreases in the concentra-
tion of creosote constituents.
Taking into consideration the data quantitating abiotic
losses of individual compounds, percent biodegradation val-
ues were calculated to quantify the precise amount of material
biodegraded over time (Table 4.24). In general, rapid rates of
biodegradation were evident. Within 3 days of incubation, a
majority of the contaminants was degraded, with little change
occurring upon continued incubation. Physical adsorption of
the high molecular-weight components and volatilization of
the lower molecular-weight contaminants may have contrib-
uted to this rapid loss. Nevertheless, data corrected for these
losses still reflect extensive degradation.
Of particular interest is the apparent biodegradation of
high-molecular-weight PAHs with this system. The extent to
which these compounds were degraded in the slurry reactors
was much greater than that observed with solid-phase biore-
mediation. Moreover, the rate of biodegradation of targeted
contaminants was much greater with the slurry-phase
bioreactors: only three days were required for slurry-phase
bioremediation to reduce the concentration to levels achieved
after 12 weeks of solid-phase treatment
21
-------
Table 4.4 Response of Embryonic Mwildla bcrylliiw to Untreated and Blotreated Filtered Groundwater from the ACW Site,
Pentacola, Florida
Criteria
Untreated Groundwater
embryos
% dead(terata)
% dead (no terata)
totals
larvae
% normal
% with terata
totals
Blotreated Groundwater
embryos
% dead (terata)
% dead (no terata)
totals
larvae
% normal
% with terata
totals
Dilution
Water
0
a.
3
97
JL
97
0
14.
14
83
3
86
Concentration (%) of Well No. 320 Groundwater
100
0
m
100
0
a
0
0
m
100
0
Q.
0
10
100
0
100
0
0.
0
97
3
100
0
Q.
0
1
67
12.
80
0
2Q
20
0
&
6
83
11
94
4.6 Sediment Shake Flask Studies
Shake flask studies were performed to evaluate the po-
tential for bioremediation of creosote-contaminated solidi-
fied materials present at the ACW site. Since these studies
were designed to offer a preliminary assessment of the appli-
cability of biological treatment, only PAHs were monitored
(Table 4.2S). Following 14 days incubation, changes in the
concentration of 21 monitored PAHs was minimal with
unamended sediment (SM). Inoculation with indigenous
surface soil microorganisms and/or adjustment to pH=7.0
offered only marginal improvement
Presumably due to a combination of high pH, high
creosote concentration and previous environmental conditions
(anoxic/anaerobic), solidified material had very low counts of
total aerobic heterotrophs (2x10* cells/g sediment). Despite
adjustment to neutrality (pH=7.0), total heterotrophic plate
counts did not increase significantly with time (100 cells/ml
after 7 and 14 days incubation). When 1.0 g surface soil
(SxlO1 cells) was added to supply inoculant in conjunction
with pH amendment, total heterotrophic counts increased
slightly after 14 days (6X103 cells/ml). Nevertheless, the ex-
tremely high creosote concentration in solidified material
suggests that it must be diluted prior to implementation of
biotreatment strategies.
22
-------
Table 4.5 i
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Concentration of PCP and 42 Creosote Constituents during Solid-Phase Bloremedlatlon of Creosote-Contaminated
Surface Soils from the ACW Site, Pensacola, Florida: Unamended Soil
Weeks of Incubation
0
3.0
2.1
3.6
9.9
7.2
4.2
15.6
21.3
9.3
33.6
28.8
41.7
48.6
104.1
148.2
23.7
114.0
84.3
35.7
112.8
29.7
0.2
U
U
U
U
U
0.9
0.1
0.1
123.3
U
0.2
U
0.9
0.1
0.1
6.9
21.6
20.0
47.4
46.8
70.5
1
3.0
2.4
3.3
9.0
6.6
3.6
12.0
11.4
8.7
17.4
32.1
36.6
40.8
103.5
150.0
15.6
84.9
68.4
26.7
115.8
28.9
0.1
U
U
U
U
U
U
0.2
0.3
114.9
U
0.1
U
U
0.1
0.1
5.8
4.2
4.8
32.4
7.8
69.3
2
mg/Land-Farming
2.4
1.2
1.8
4.2
5.7
3.0
8.9
5.4
3.6
26.1
28.8
37.8
36.6
62.4
86.1
14.1
72.9
58.5
29.1
96.6
29.4
U
U
U
U
U
U
U
0.2
0.3
211.1
U
0.1
U
U
0.1
U
5.7
4.2
4.8
7.3
14.4
44.1
4
Chamber (3kg) '
2.7
1.2
2.4
4.5
6.0
U
11.1
8.7
7.2
25.8
27.6
39.3
48.3
81.3
87.3
13.5
78.9
61.2
30.6
106.5
29.1
U
U
U
U
U
U
U
0.1
0.2
80.1
U
0.1
U
U
0.1
U
3.9
5.7
3.2
8.4
12.3
37.5
8
2.4
1.2
1.2
3.9
0.9
U
10.2
4.2
6.9
28.8
23.1
26.1
32.4
78.9
90.0
23.4
88.2
46.5
30.0
105.6
29.0
U
U
U
U
U
U
U
0.1
0.1
41.1
U
0.1
U
U
U
U
2.4
3.3
1.8
2.9
5.7
19.5
12
1.8
U
U
3.9
U
U
9.6
3.3
U
21.6
12.0
8.7
15.3
61.2
69.6
17.1
53.4
63.6
25.2
109.8
29.2
U
U
U
U
U
U
U
0.1
0.1
46.8
U
U
U
U
U
U
2.4
4.5
1.2
3.3
8.0
14.1
' Data reported are the averages of duplicate samples; U=undetected (below LOD).
23
-------
Table 4.6
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Los* (Volatilization) from the Land Farming Chamber Containing Unamended Surface Soil
Presence in Activated Carbon Traps' fu.a/10 a Carbon)
Day 2
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
u
u
u
u
u
u
u
0.1
u
0.2
u
u
u
u
u
u
u
u
u
u
mi
0.4
u
u
u
u
u
0.4
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
0.3
u
u
u
u
u
u
u
Wk3
u
1.0
u
u
u
u
0.8
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
4.8
u
0.5
u
16.1
u
u
677.5
80.4
U
135.3
11.1
U
U
U
U
W(5
U
U
U
U
U
U
1.0
U
U
U
U
U
12.0
U
U
U
U
U
U
U
u
u
u
u
u
u
u
0.3
0.1
0.4
U
U
0.5
U
U
U
U
U
0.8
0.3
0.3
U
U
ma
u
u
0.3
u
0.1
0.1
0.5
0.1
u
u
u
u
u
0.1
u
0.1
0.5
0.1
0.1
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
0.4
u
0.9
u
0.7
mi2
0.5
0.2
0.2
1.1
0.7
u
1.0
0.5
1.5
0.5
U
0.6
0.7
U
U
U
0.4
3.1
0.3
U
U
U
U
0.1
U
U
U
U
U
U
U
U
U
2.3
0.1
U
U
0.2
0.8
1.1
0.3
1.9
U
Totaling)
0.9
1.2
0.5
1.1
0.8
0.1
3.7
0.6
1.5
0.5
U
0.6
12.7
0.1
U
0.1
0.9
3.2
0.4
U
U
U
U
O.1
U
U
U
5.1
0.1
0.9
U
16.1
0.7
2.3
677.6
80.7
U
135.5
13.1
1.4
1.5
1.9
0.7
' Values corrected for presence of individual components in control trap; U=be/ow LOO.
24
-------
Table 4.7 P
C
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
'ercent Blodegradatlon of PCP and 42 Creosote Constituents during Solid-Phase Bloremedlation of Creosote-
'vntamlnated Surface Solla from the ACWSIte, Pensacola, Florida: Unamended Soil
Weeks of Incubation
1
0
0
8
10
13
14
19
46
6
48
0
12
15
1
0
34
25
19
25
0
3
50
—
—
—
—
—
100
0
0
7
—
ND
—
ND
ND
ND
ND
ND
ND
ND
ND
ND
2
20
43
50
57
21
29
43
75
61
22
0
9
25
40
42
41
36
30
19
14
1
100
—
—
—
—
—
700
0
0
0
—
50
—
100
0
100
17
81
76
85
69
37
4
10
43
33
55
17
100
29
59
23
23
4
6
1
22
40
43
31
27
14
5
2
100
—
—
—
' —
—
100
0
0
35
—
ND
—
ND
ND
ND
ND
ND
ND
ND
ND
ND
8
20
43
67
61
85
100
35
80
26
14
20
37
33
23
39
5
23
44
16
6
2
100
—
—
—
—
—
700
0
0
67
—
ND
—
ND
ND
ND
ND
ND
ND
ND
ND
ND
12
40
99
99
61
99
99
39
85
99
36
58
79
69
41
53
28
53
25
29
3
2
100
—
—
—
—
—
99
0
0
62
—
99
—
22
20
100
64
79
94
93
83
80
Week 12 data corrected for volatilization (Table 4.6); ND*not determined.
25
-------
Table 4^
Compound
:D Number
2
3
4
5
6
7
a
9
10
t1
12
:3
14
15
IS
'7
"8
•9
SO
21
22
S3
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Concentration of PCP and 42 Creoaote Conatttuonta during Solld-Phaae Bloromodlation of Cnoaote^ontamlnated
Surface Solla from the AC W Site, Penaaeola, Florida: Plot Nutritional Amendmenta
Weeks o1 Incubation
Q
3.0
2.1
3.6
9.9
7.2
4.2
1S.6
21.3
9.3
33.6
28.8
41.7
48.6
104.1
148.2
23.7
114.0
84.3
35.7
112.8
29.7
0.2
U
U
U
U
U
0.9
0.1
0.1
123.3
U
0.2
U
0.9
0.1
0.1
6.9
21.6
20.0
47.4
46.8
70.5
1
2.7
1.S
0.9
9.0
6.0
2.7
12.3
8.7
3.3
30.9
32.7
17.1
35.7
97.2
'165.3
24.0
95.7
90.6
49.8
111.9
28.8
0.1
U
U
U
U
U
0.1
0.2
0.1
150.9
U
U
U
U
0.1
0.2
1.0
10.5
4.2
21.9
10.2
10.0
2
2.1
0.9
0.9
2.7
3.3
4.5
12.3
7.5
3.3
19.2
15.0
15.9
24.6
73.5
102.6
14.4
113.4
78.0
48.3
110.1
28.2
U
U
U
U
U
U
U
0.1
0.1
261.9
U
0.1
U
U
0.1
0.1
2.0
9.5
4.9
27.9
29.6
49.8
4
ling Chamber (3kg)'
2.1
1.2
0.0
6.3
2.7
1.8
15.3
8.7
2.7
25.4
9.0
15.3
33.6
93.6
164.4
22.5
110.4
93.6
51.6
114.3
29.1
U
U
U
U
U
U
U
0.2
0.3
102.9
U
0.1
U
U
0.1
0.1
2.1
5.1
3.6
3.6
8.7
39.3
8
1.2
0.6
1.2
3.6
0.9
0.6
9.9
4.5
2.1
19.3
5.4
12.6
19.2
61.5
89.1
13.8
51.6
60.9
46.5
96.3
27.6
U
U
U
U
U
U
U
0.2
U
68.4
U
0.1
U
U
0.1
0.1
1.4
4.0
1.7
5.1
6.6
12.6
12
1.2
U
U
U
U
U
8.4
3.6
U
14.4
3.3
9.9
11.1
45.6
55.2
11.4
46.2
47.7
31.8
81.3
24.3
U
0.1
U
U
U
U
U
0.2
U
71.7
U
U
U
U
U
0.1
U
3.9
1.0
4.2
6.3
9.9
Data reported are the averages of duplicate samples; U~undetected (below LOD); A/0-nor determined.
26
-------
Table 4.9
Compound
ID Number
1
2
3
4
5
6
7
a
9
**>
;*
?
13
***
15
;6
17
18
20
11
'2
23
,J4
"'$
*6
27
28
29
30
31
32
.3
34
35
36
37
38
J*
?0
<.' i
42
*3
Lot* (Volatilization) from the Land Faming Chamber Containing Nutrient-Amended Surface Soil
' Presence in Activated Carbon Traps' (g/10 a Carbon)
Day 2
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.01
U
U
U
U
U
U
U
U
U
U
U
U
Wkl
U
U
U
U
U
U
1.0
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.02
U
U
U
U
0.9
0.6
1.1
0.9
0.4
0.8
U
U
Wk3
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
1.0
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.1
U
0.3
0.4
0.2
0.9
0.3
U
0.4
WkS
U
U
1
U
U
U
1.0
U
U
U
U
U
6.0
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.3
U
U
U
U
U
U
U
0.5
U
1.5
0.3
U
U
me
0.9
u
u
0.1
u
u
u
u
u
u
u
u
u
u
u
u
0.4
0.2
1.4
0.1
u
u
u
u
u
u
u
u
u
u
u
u
0.1
u
u
u
u
u
u
u
u
u
u
mi2
1.0
u
u
u
u
u
u
u
0.2
0.3
0.8
u
u
u
u
u
u
1.5
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
0.6
2.5
u
Total frg)
1.9
u
1.0
0.1
u
u
2.0
u
0.2
03
0.8
U
b.O
U
u
u
0.4
1.7
;* -
O.'t
u
u
u
u
u
u
u
u
u
0.3
0.03
U
0.1
u
0.1
0.9
0.9
2.0
1.1
2.8
2.0
2.5
0.4
Values corrected for presence of individual components in control trap; U=bolow LOO.
27
-------
Table 4.10 ,
i
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
1B
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Percent Blodegradatlon of PCP and 42 Creosote Constituents during Solid-Phase Bloremedlation of Creosote-
Contaminated Surface Soils from the ACWSIte, Penaecoia, Florida: Plua Nutritional Amendments
Weeks of Incubation
1
10
29
75
10
17
36
21
59
65
8
0
59
27
7
0
0
16
0
0
1
3
SO
—
—
—
—
—
89
0
0
0
—
NO
—
NO
ND
NO
ND
ND
ND
ND
ND
ND
2
30
57
75
73
54
50
21
65
65
43
48
62
49
29
30
39
1
7
0
1
5
100
—
—
—
—
—
100
0
0
0
—
50
—
100
0
0
71
56
76
43
37
29
4
30
43
100
36
63
57
2
59
71
24
69
63
31
11
0
S
4
0
0
0
3
100
—
—
—
—
—
100
0
0
17
—
ND
—
ND
ND
ND
ND
ND
ND
ND
ND
ND
a
60
71
67
64
85
86
37
79
77
43
81
70
61
41
40
42
54
28
0
14
7
100
—
—
—
—
—
100
0
100
45
—
ND
—
ND
ND
ND
ND
ND
ND
ND
ND
ND
12*
60
99
99
99
100
100
46
83
99
57
89
76
77
56
63
52
59
43
11
28
18
100
—
—
—
—
—
100
0
100
42
—
100
—
100
100
0
100
82
95
91
87
86
Week 12 data corrected tor volatilization (Table 4.9); ND*not determined.
28
-------
Table 4.11
Time
Change* In Soil Ulcroblal Number* during Solld-Pha*e Bloremedlatlon of Creosote-Contaminated Surface Soil*
Obtained from the ACW Site, Penaacola, Florida
Unamended Plus Nutrients
Total
Heterotrophs
Initial
counts
Week 2
Week 4
Week 8
Week 12
Table 4.1 2
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Phenanthrene-
degraders
i— or-i i/.
Total
Heterotrophs
. o—a
Phenanthrene-
degraders
7.8
8.1
8.2
6.2
7.6
0
0
0
0
5.3
7.8
8.1
8.2
7.3
7.9
0
0
5.7
5.7
4.4
Concentration of PCP and 42 Creosote Constituent* during Solid-Phase Bloremedlatlon of Creosote-Contaminated
Sediments from the ACW Site, Penaacola, Florida: Unamended Sediment
Weeks of Incubation
0
11773.5
4356.9
1869.9
995.7
889.2
502.5
148.2
4103.1
5376.3
13301.4
9111.3
1549.3
1229.7
4886.1
3047.7
864.9
1443.6
246.6
513.6
418.8
67.8
6.3
29.1
27.0
60.3
65.1
63.3
15.0
83.1
37.5
127.5
0.6
8.3
5.4
377.4
170.7
90.9
2244.9
1312.8
3793.5
1426.5
14569.7
5191.8
1
8325.6
3429.9
1471.2
816.6
730.5
453.9
110.1
3447.6
4484.4
11055.6
7614.0
1223.7
1274.4
4062.6
2530.2
688.8
1032.3
191.7
509.4
489.S
75.3
5.1
30.6
29.7
74.4
42.6
62.7
12.0
78.9
32.1
68.1
0.4
1.8
4.8
133.2
78.3
84.3
1765.2
1260.9
32S9.S
1104.6
14322.3
5357.4
2
7764.9
3413.4
1433.6
816.9
727.8
436.8
117.0
3546.3
4792.2
11892.3
9097.2
1290.6
1080.0
4375.8
2615.1
725.1
1188.6
205.2
486.9
423.9
67.5
4.2
21.9
17.4
42.9
20.1
37.2
11.1
57.0
21.0
141.6
U
U
U
265.5
709.5
57.3
1752.6
904.2
3300.6
1196.1
12655.8
4846.5
4
ig Chamber (3 kg)'
7022.7
3294.3
1411.8
810.9
730.8
424.5
117.9
3497.3
4694.1
11730.9
7683.3
1284.3
1050.3
4373.7
2606.4
724.5
1185.6
208.5
426.6
386.4
60.3
3.3
15.6
14.7
29.4
20.1
32.4
7.2
43.2
18.6
176.4
U
U
U
208.5
140.4
82.5
1622.9
930.0
2853.5
945.7
7928.7
2692.2
8
5137.2
2886.6
1240.5
726.0
654.9
397.8
102.0
3175.5
4263.9
10677.3
7365.0
1225.2
1 168.8
4035.6
2409.0
670.8
1080.6
192.6
443.7
384.6
67.5
0.5
0.4
3.3
14.1
U
1.4
4.2
29.4
10.2
154.8
U
U
U
201.6
36.4
72.3
1227.6
978.6
2337.0
934.8
8439.3
2841.3
12
1845.0
2673.0
1191.9
714.6
650.1
390.3
100.5
3129.3
4286.7
10698.9
7453.2
1206.3
1 122.9
3279.0
2326.8
657.6
1 146.6
183.6
446.1
345.6
54.0
0.4
0.4
2.4
6.3
U
1.4
3.9
27.9
8.7
195.6
U
U
U
161.4
25.2
63.0
1318.2
1023.6
2601.6
1051.2
9949.8
2900.1
' Data reported are the averages of duplicate samples; U=undetected (below LOD); ND=not determined.
29
-------
Table 4.13
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
: *^
i £.
13
14
,'&
16
17
IB
19
20
21
"-,'£
23
24
•5
2S
27
IS
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Loaa (Volatilization) from th» Land Farming Chambar Containing Unamandad Sediment
Presence in Activated Carbon Traos'. u.a/10 a Carbon
Day 2
0.5
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.01
U
U
U
U
U
U
U
U
U
U
U
U
mi
7.0
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
1.4
1.5
0.7
U
U
U
0.6
U
U
Wk3
10.0
0.8
0.6
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.9
1.2
2.7
4.5
3.9
1.5
0.2
U
0.4
WkS
0.9
38.0
3.0
13.0
7.0
2.0
1.0
10.0
U
U
U
U
9.0
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
1.0
0.9
U
U
2.2
U
U
U
U
me
34
28.0
16.0
8.0
2.0
2.0
6.0
3.0
0.5
0.3
0.2
0.2
U
0.1
0.1
0.1
0.2
0.3
2.0
U
0.1
a 7
0.4
U
0.2
0.2
0.3
U
0.2
U
U
U
8.7
6.5
U
U
U
U
3.0
0.9
1.1
0.2
1.4
miz
626
34.0
30.0
7.0
4.0
2.0
1.0
8.0
0.9
0.8
U
U
U
U
U
0.1
U
0.2
U
U
U
f.9
0.4
U
U
U
U
0.3
U
0.3
U
U
0.8
U
6.7
1.7
0.5
2.1
0.5
04
U
U
U
Tola/, pg
677.4
100.8
49.6
28.0
13.0
6.0
8.0
21.0
1.4
1.1
0.2
0.2
9.0
0.1
0.1
0.2
0.2
0.5
2.0
U
0.1
2.6
0.8
U
0.2
0.2
0.3
02
02
0.3
0.01
U
as
6.5
10.0
5.3
3.9
6.1'-
9.8
28
1.S
0.2
1.8
' Values corrected for presence of individual components in control trap; U=below LOD.
30
-------
7tbl«4.14 Pt
Cc
Compound
ID Number
7
2
S
4
S
6
7
a
9
10
11
12
13
14
;5
16
',7
?S
*9
?0
?1
?2
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
rcont Blodegndatton of POP and 42 Creototo <
mtamlnated Sediment from the ACW Site, Pont
1
29
21
21
18
18
10
24
16
17
17
16
21
0
17
17
20
29
22
1
2
0
19
0
0
0
35
1
22
5
14
23
NO
ND
NO
ND
ND
ND
ND
ND
ND
ND
ND
ND
2
34
22
23
18
18
13
20
14
11
11
1
17
12
10
14
16
18
17
5
0
0
33
25
36
17
70
41
26
31
44
0
100
100
100
30
36
37
22
31
13
16
13
7
2ofiftfifKMnte durinti SAflrf*PfU4* Bloimsn&dt* If/in of f.
•cola, Florida: Unenwnded Sediment
Weeks of Incubation
4
40
24
24
18
18
16
20
15
13
12
16
17
15
11
14
16
18
15
17
8
9
48
46
47
51
70
49
52
48
50
0
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
8
56
34
34
27
26
21
31
23
21
20
19
21
5
17
21
23
25
22
12
8
0
92
99
88
77
100
98
72
65
73
0
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
^no»ote-
12
84
39
36
28
27
22
32
24
20
20
18
22
7
33
24
24
21
24
12
W
13
52
96
91
89
99
98
72
66
77
0
100
100
100
57
85
31
41
22
31
26
32
44
' Week 12 data corrected for volatilization (Table 4.13); WD-nof determined
31
-------
Table 4.1 5
Compound
ID Number
1
2
3
4
5
6
7
a
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Concentration of PCP and 42 Creoaote Constituent* during Solld-Phaae Bloremedlatlon of Cnototo-Contamlnated
Sediment* from the ACW Site, Penaacola, Florida: Nutrient-Amended Sediment
Weeks of Incubation
0
11733.5
4356.9
1869.9
995.7
889.2
502.5
148.2
4103.1
5376.3
13301.4
9111.3
1549.2
1229.7
4886.9
3047.7
864.9
1443.6
246.6
513.6
418.7
67.8
6.3
29.1
27.0
60.3
65.1
63.3
15.0
83.1
37.5
127.5
0.6
8.3
5.4
377.4
170.7
90.9
2244.9
1312.8
3793.5
1426.5
14569.5
5191.8
1
8151.9
3333.9
1460.7
792.9
709.5
438.3
107.7
3342.0
4392.6
9616.5
4778.7
613.8
1273.2
4286.7
2613.6
711.9
1032.9
192.0
456.9
426.0
60.9
4.7
27.1
22.3
43.2
36.9
56.1
10.2
68.7
29.6
57.3
0.5
0.9
3.9
632.1
153.1
113.7
2151.9
1146.3
3638.1
1382.1
14991.0
3565.8
2
4
— mg/Land Farming Chamber (3kg) '
9843.6
3967.5
1660.5
908.4
808.5
478.2
128.4
3951.9
5161.5
12519.6
8970.3
1461.6
1135.5
4786.8
2870.4
815.1
1413.0
219.6
454.8
365.7
68.1
1.8
18.5
15.0
29.2
28.0
38.0
7.4
56.1
21.8
140.7
U
U
4.8
332.7
182.7
81.1
1833.6
1108.5
2933.4
1119.9
10001.1
4563.0
8278.5
3525.6
1504.2
847.8
753.9
441.0
122.7
3564.9
4942.2
12362.4
9186.0
1332.3
1209.6
4358.7
2633.4
612.3
1112.7
219.0
504.0
435.6
55.2
1.5
18.5
15.0
30.3
20.9
35.7
7.4
54.2
21.8
141.9
U
U
U
341.4
173.4
90.1
1869.9
1188.6
2582.1
978.9
10128.3
3988.2
8
6144.6
3468.0
1492.5
869.7
785.1
466.2
128.7
3728.1
5003.4
12534.6
8949.0
1402.2
1309.5
4575.0
2707.2
741.3
1281.0
222.0
471.3
418.5
57.3
0.8
0.6
3.9
12.0
0.8
2.6
5.3
39.2
12.9
173.1
U
U
U
282.2
61.2
82.9
1420.0
1183.7
3263.9
1181.0
9936.1
3298.2
12
380.4
1084.8
501.0
313.5
290.4
178.8
99.8
2887.8
3938.4
10050.6
6706.8
1 180.8
1202.6
3832.8
2316.0
622.2
992.4
178.8
278.4
351.6
47.4
1.2
0.4
2.1
2.4
0.3
0.9
6.3
28.8
18.3
172.8
U
U
0.6
115.2
22.8
53.4
1200.6
903.6
2920.5
1044.0
9619.5
2892.9
' Data reported are the averages of duplicate samples; U=undetected (below LOD).
32
-------
Table 4.16
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Loaa (Volatilization) from the Land Farming Chamber Containing Nutrient-Amended Sediment
Presence in Activated Carbon Traos1 Aio/f 0 o Carbon)
Day 2
3.0
U
0.4
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.02
U
U
U
U
U
U
U
U
U
U
U
U
Wk1
3.0
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
2.2
2.2
0.8
U
U
U
U
U
U
Wk3
U
3.0
6.0
U
U
U
U
0.1
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.03
U
U
U
750.9
39.5
16.6
34.2
10.9
3.4
U
0.2
0.4
WkS
0.1
0.1
0.2
0.1
U
0.1
0.1
0.2
U
0.1
U
0.2
3.0
U
U
U
U
0.3
0.4
U
U
0.1
U
U
U
U
U
U
U
U
U
U
U
U
60.0
5.7
3.3
2.1
0.2
U
0.4
U
0.4
WkS
510.1
66.0
42.0
7.0
3.0
3.0
6.0
7.0
0.1
0.1
0.1
0.2
U
0.1
0.1
U
0.1
0.1
0.2
U
U
2.3
0.9
U
0.8
U
0.4
U
U
U
U
1.4
49.6
U
279.9
43.5
13.6
3.6
11.3
7.4
U
U
1.2
Wk12
720.2
845.2
358.0
67.0
44.0
U
U
59.0
1.4
U
0.6
0.2
0.1
0.3
U
U
0.2
U
U
U
U
U
0.6
0.5
1.4
0.8
0.9
U
0.4
U
U
0.2
12.1
U
657.6
153.6
U
4.3
87.7
U
1.0
1.3
1.8
Totaling)
1288.3
914.3
406.6
74.1
47.0
3.1
6.1
66.3
1.5
0.2
0.7
0.6
3.1
0.4
0.1
U
0.3
0.4
0.6
U
U
2.4
1.5
0.5
2.2
0.8
1.3
U
0.4
U
0.05
1.6
61.7
U
1750.6
244.5
34.3
10.3
110.1
10.7
1.4
1.5
3.8
Values corrected for presence of individual components in control trap; U=below LOD.
33
-------
T»bi»4.1? Pe
Co
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
IS
16
17
18
19
20
£«
2Z
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
roent Blodegredatlon of PCP and 42 Creoeote Constituent* during SoHd-Phaee Bloremedlatlon of Creosote-
^terminated Sediment from the ACWSIte, Peneacola, Florida: Nutrient-Amended Sediment
Weeks of Inmhation
1
31
23
22
20
20
13
27
19
18
28
48
60
0
12
14
18
29
22
11
0
9
25
7
17
28
43
11
29
17
21
54
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
2
16
9
11
8
9
4
12
4
4
6
2
6
7
2
6
6
2
11
12
12
0
71
36
44
52
57
40
51
32
42
0
100
100
7
12
0
11
18
16
23
22
31
12
4
30
19
20
15
15
12
18
13
8
7
0
14
2
11
14
29
23
11
2
0
15
76
36
44
50
68
44
51
35
42
0
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
8
48
20
21
12
12
7
12
9
7
6
2
10
0
6
11
14
11
11
8
0
7
87
98
86
80
99
96
65
53
66
0
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
121
97
75
73
6$
67
65
33
30
27
24
26
24
2
22
24
28
31
46
46
16
31
48
93
90
89
99
97
58
65
51
0
100
100
89
69
87
41
47
31
23
27
34
44
' Week 12 data comcted for volatilization (Table 4.16); ND=not determined.
34
-------
Table 4.1$ Change* In Soil Ulcroblal Number* during Solid-Phase Bloremedlatlon of Creosote-Contaminated Sediments
Obtained from the ACW Site, Penaacola, Florida
Time Unamended Plus Nutrients
initial counts
Week 2
Week 4
WeekB
Week 12
Total
Heterotrophs
2.9
2.9
3.2
8.3
7.7
Phenantftrene-
degraders
Inn f.t
0
1.5
2.3
5.4
5.7
Total
Heterotrophs
•tt/n
-------
Table 4.20 Abiotic Lo**e* during Sluny-Pha*e Blonmedlatlon of Creotote-Contamlnated Surface Soil* from theACW Site,
Penaacola, Florida
Compound
ID Number
1
2
3
4
S
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Activated Carbon Traos fuo/Trao')
7
0.1
U
0.4
0.1
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
0.02
U
U
U
U
U
U
U
U
U
U
U
U
21
0.2
U
U
U
U
U
U
0.3
U
0.4
U
U
U
U
U
0.1
1.5
0.4
U
U
U
U
12.5
U
U
U
U
1.6
4.7
11.3
0.02
U
0.1
0.1
U
U
U
U
U
0.2
U
U
U
30
U
U
U
U
U
U
U
0.3
U
U
U
U
U
U
U
U
0.4
U
U
U
U
U
6.2
U
U
U
U
41.7
21.4
66.7
0.03
U
0.1
0.1
U
U
U
U
U
U
U
U
U
Sludge
Residue (Day 30)
US
0.3
0.2
0.2
0.2
U
U
47.0
7.0
10.0
33.0
13.0
14.0
30.0
145.0
182.0
37.0
167.0
483.0
5.0
11.0
8.4
U
U
0.1
U
U
U
U
1.5
1.2
3.8
U
U
U
U
U
U
U
U
U
U
1.5
1.2
Total
H9
0.3
0.2
0.6
0.3
U
U
47.0
7.6
10.0
30.4
13.0
14.0
30.0
145.0
182.0
37.1
168.9
483.4
5.0
11.0
8.4
U
18.7
0.1
U
U
U
43.3
27.6
79.2
4.5
U
0.2
0.2
U
U
U
U
U
0.2
U
1.5
1.2
' Volatilization data corrected tor background; U=below LOD.
36
-------
Table 4.21
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Percent Bhdegradatlon of POP and 42 Monitored Creoaote Constituent* during Slurry-Phase Bloremedlatlon of
Creosote-Contaminated Surface Soils from the ACWSIte, Penaacola, Florida
Days of Incubation
1
20
10O
0
29
—
100
0
0
0
10
0
0
0
0
4
11
8
16
0
13
25
23
12
—
—
—
6
100
0
SO
56
—
—
—
50
0
65
51
49
68
22
41
30
3
20
100
0
57
—
100
0
0
0
10
2
0
20
5
9
11
12
18
0
11
IS
46
3
—
—
—
0
40
17
57
33
—
—
—
50
0
67
40
60
55
14
55
30
5
40
100
30
65
—
100
14
30
36
10
50
33
20
26
22
11
19
26
0
43
28
82
0
—
—
—
0
100
32
80
56
—
—
—
50
100
61
S3
27
59
17
41
40
7
40
100
70
79
—
100
29
30
36
10
50
33
20
21
22
44
31
29
3
10
24
100
100
—
—
—
100
100
45
100
45
—
—
—
58
100
67
44
49
62
28
43
42
14
20
100
100
100
—
95
100
100
65
40
75
33
40
42
35
44
46
45
16
14
23
100
100
—
—
—
too
100
59
100
23
—
—
—
73
100
73
36
73
66
39
46
44
21
40
100
100
100
—
100
100
100
65
40
88
66
40
47
52
56
54
48
13
31
24
100
100
—
—
—
100
100
67
100
45
—
—
—
73
100
73
60
96
83
34
63
44
30'
99
100
99
99
—
700
94
93
65
37
86
62
55
46
41
74
52
41
15
15
23
100
45
—
—
—
100
61
28
28
40
—
—
—
73
100
83
60
96
83
44
72
53
' Day 30 values corrected for abiotic losses (Table 4.20).
37
-------
Table 4.22 Concentration of POP and 42 Monitored Creoaote Conatituentt during Slurry-Phaae Bloremedlatlon of Creosote-
Contaminated Sediment from the AC W Site, Penaacola, Florida
Compouri
ID Numbt
1
2
3
J
5
6
7
8
9
10
11
12
13
14
15
16
17
13
19
20
21
22
23
>4
?5
~%
7?
•eS
0.7
U
0.2
0.1
1.4
0.9
0.4
1.2
0.9
19
1.1
1.8
2.2
0.2
4.0
0.6
U
U
U
U
U
\J
0.:
0.1
0?
1.1
U
U
U
U
U
U
U
U
U
0.3
1.3
0.4
'Data reported are the averages of duplicate samples; U*undetected (below LOD).
38
-------
Table 4.23 A
/>,
Compound
ID Number
1
2
3
4
5
6
7
8
9
W
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
blotlc Losses during Slurry-Phase Bloremedlation of Creosote-Contaminated Sediments from the ACW Site,
ansacola, Florida
Sludge
Activated Carbon Traps fog/Trap') Residue (Day 30) Totai
7
2474
422
399
133
83
45
5
300
1
18
1
0.8
0.7
U
U
1.1
1.5
U
U
U
U
31.0
78.8
37.6
216.7
9.5
112.7
9.1
49.5
5.7
U
3.3
U
6.9
310.8
211.1
201.6
341.9
73.0
456.2
27.5
2.8
10.3
21
21
23
U
14
17
25
U
245
50
31
12
4
2
0.2
U
U
2
0.2
U
U
U
26.0
12.9
5.0
4.7
4.2
26.4
129.6
14.3
142.2
U
U
1.3
1.5
16.5
17.3
7.9
2.1
1.1
4.2
0.7
U
U
30
3
24
U
U
U
U
U
44
34
15
24
11
18
3
2
0.2
0.6
0.7
U
1.0
U
8.9
11.4
2.3
1.2
1.6
5.4
9.0
4.7
73.2
U
U
U
0.8
5.8
9.7
4.7
8.5
17.5
35.1
14.2
12.1
22.7
M
420
617
67
203
187
259
541
1039
4219
14265
2043
5418
5828
29903
30214
5986
9582
2569
465
506
313
U
0.7
0.5
0.7
0.6
1.1
2.5
3.2
3.9
404
U
U
U
U
U
U
14.8
6.3
35.0
36.3
125.3
438.8
US
2.918
L086
0.465
0.350
0.287
0.329
0.546
1.628
4.304
14.329
2.080
5.434
5.849
29.906
30.216
5.9Bf
9.586
2.57C
0.465
0.506
0.313
006B
0.104
0.045
0.217
0.016
0. 146
0.151
0.072
'J.225
0.40-"
0.003
O.OC'f
c-oos
0.333
0.23f
0.2U
0.367
0.098
0.53?
Q.787
0.140
0.472
' Volatilization data corrected for background; U=below LOD.
39
-------
Table 4.24
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
Percent Blodegradatlon of PCP and 42 Monitored Creosote Constituent* during Slurry-Phase Bloremedlatlon of
Creosote-Contaminated Sediments from the ACW Site, Penaacola, Florida
Davs of Incubation
1
42
39
39
46
42
41
30
39
37
36
57
37
50
39
40
38
44
48
0
2
30
95
61
58
75
66
55
93
55
86
56
—
—
—
fir
10
17
2
37
8
5
3
0
3
99
95
84
72
71
65
65
67
55
54
49
55
63
55
57
55
59
65
21
6
10
95
49
79
75
88
77
94
88
94
52
—
—
—
69
82
66
55
53
29
6
10
0
5
99
97
95
87
81
83
79
71
67
66
62
61
67
58
58
55
59
59
21
13
40
95
91
95
98
97
91
97
67
96
56
—
—
—
73
94
83
83
74
56
13
28
6
7
99
98
100
100
92
86
56
74
85
95
97
53
67
51
52
52
59
63
29
2
60
95
97
95
98
97
97
87
85
96
84
—
—
—
87
98
94
97
S3
90
74
SO
51
14
99
99
99
99
98
89
100
90
99
98
98
55
74
55
52
48
56
59
14
4
60
98
97
95
\
97
98
90
88
98
64
—
—
—
91
98
97
99
68
96
84
63
71
21
99
99
100
100
100
92
100
99
99
99
99
98
94
99
64
91
94
55
86
6
40
98
97
95
98
97
98
97
97
97
84
—
—
—
99
100
100
100
95
99
90
98
98
30'
98
99
99
99
99
91
87
98
96
95
98
85
77
78
41
67
66
36
57
15
10
99
97
89
99
94
97
99
97
96
40
—
—
—
96
94
94
98
95
99
93
98
98
' Day 30 values corrected for abiotic losses (Table 4.23).
40
-------
Table 4.25 BlodegradaUon In [ig/ml of 21 PAHt during Slurry-Pha»e Bloremedlatlon of Solidified Material from theACW Site,
Peruiacola, Florida
Compound
ID Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
Time-
zero
951.5
459.7
187.2
96.3
103.7
53.7
18.8
476.8
550.4
1704.9
380.8
174.8
139.7
722.9
411.5
86.6
49.6
39.5
22.4
62.0
5.8
SM
918.5
424.3
175.9
87.5
92.4
47.8
17.3
448.8
513.0
1636
368.1
163.3
131.5
688.3
393.5
81.1
47.8
37.8
21.1
50.1
5.8
Day 7
SM7
554.9
330.7
133.6
70.9
79.1
42.4
15.8
383.2
455.0
1521
325.1
142.1
124.6
668.3
361.0
80.6
44.3
37.1
23.0
60.3
5.0
Dav14
SM7+
542.5
289.4
126.0
67.7
69.5
38.4
15.0
342.1
400.0
1339
282.5
125.0
113.3
563.2
320.2
67.9
34.8
32.7
17.3
48.4
5.0
SM
805.6
424.4
174.S
91.8
96.9
51.5
18.3
450.4
532.0
1704
377.7
174.2
142.3
713.6
415.0
81.5
46.1
38.7
21.0
47.9
5.7
SM7
835.7
418.6
175.8
90.4
95.7
51.6
18.0
462.8
525.7
1701
364.9
158.0
140.7
703.3
397.4
83.8
40.3
38.4
21.3
58.9
5.1
SM7+
621.1
350.4
150.5
79.8
84.5
45.1
15.9
409.9
461.9
1507
329.8
156.9
120.6
630.9
363.7
73.6
42.7
35.7
20.1
51.0
5.0
Killed
879.3
452.1
189.3
95.0
100.8
53.3
18.4
481.9
537.6
1717
367.4
177.3
139.6
716.7
406.9
87.4
47.3
39.2
22.3
59.6
5.8
SM=unamended solidified material (SM), pH= 10-11.
SM7=SM adjusted to pH=7.0.
SM7+=SM adjusted to pH=7.0 plus surface soil inoculum.
Killed=killed cell control (3.7% formaldehyde).
Data reported represent the average of duplicate analyses.
41
-------
5. Conclusions
5.1 Solid-Phase Bioremediation: Surface Soils
i. Solid-phase bioremediation of creosote-contaminated
surface soil from the ACW site resulted in predictable patterns
of biodegradation: lower-molecular-weight contaminants were
biodegraded more readily than higher-molecular-weight com-
pounds, and PAHs containing 4 or more fused rings resisted
biological attack by indigenous microorganisms. However,
land-farming chambers excluded the effects of photodegrada-
tion which may have resulted in more extensive degradation
of these compounds.
ii. The addition of soluble inorganic nutrients acceler-
ated the rate, and enhanced the extent, of biodegradation.
However, the process was still slow and inefficient (8 weeks
required to degrade ca. 50% of the pollutants present).
iii. Volatilization of creosote constituents was low and
relatively insignificant in terms of abiotic losses under the
conditions of these experiments. However, soils were not
exposed to extremes in temperature or other climatic vari-
ables, such as high winds, as would occur in the field.
5.2 Solid-Phase Bioremediation: Sediment
i. Solid-phase bioremediation of sediment was basi-
cally non- effective. The biodegradation process was slow and
inefficient (12 weeks required to biodegrade ca. 50% of the
pollutants present), and the pattern of biodegradation was
predictable. However, materials were used as they occur in situ
(pH=10) hence pH adjustment to neutrality may enhance the
activity of indigenous microorganisms.
ii. The addition of soluble inorganic nutrients to sedi-
ment did not accelerate rates of biodegradation, but the extent
of biodegradation of the higher-molecular-weight PAHs was
enhanced.
iii. Volatilization of creosote constituents was more sig-
nificant, and even greater losses would be expected to occur in
situ as a result of temperature changes and prevailing air
movements determined by climate.
5.3 Slurry-Phase Bioremediation: Surface Soil
i. Slurry-phase bioremediation employing indigenous
microorganisms offered an advantage over solid-phase biore-
mediation of these materials in terms of time (14 days vs. 12
weeks). However, neither approach resulted in extensive deg-
radation of the more recalcitrant contaminants when indig-
enous microoganisms were employed as biocatalysts.
ii. Volatilization during slurry-phase bioremediation was
insignificant, but physical adsorption accounted for 1 to 17%
of the observed losses.
5.4 Slurry-Phase Bioremediation: Sediment
i. Slurry-phase bioremediation of sediment offered sip
nificant advantages over solid-phase bioremediation i; ;e:T:
of time and effectiveness (3 to 5 days slurry-phase \ $ i
weeks solid-phase to degrade >50% of the targeted poi ,_ia .
ii. Slurry-phase bioremediation of sediments a- ,,-.::
to pH=7.1 resulted in relatively rapid and extensive biC'/.:;:
dation of higher-molecular-weight PAHs which typ:c~ .
sist biological attack (14 days required to biodegrads c. ^
of the higher-molecular-weight PAHs).
iii. Abiotic losses of monitored constituents of creosc;
were significant: volatilization of naphthalene accounted fr •
1.5% of the observed loss, and physical adsorption ace > >iui!e ;
for 36% of the observed loss of pyrene.
5.5 Site Specific Factors
i. Regardless of the biotreatment strategy selec'-c,: ,t.
pH of the sediment must be adjusted to neutrality rno' •,
implementation.
ii. Microorganisms indigenous to the ACW .
effectively degrade the lower-molecular-weight c ,
components. However, efficient removal oi the more
trant, high-molecular-weight PAHs will require ad' .t ;
incubation time (> 12 weeks using land farming or <30 : ,
slurry treatment), or the use of microbial inocula with i
strated abilities to degrade these pollutants.
iii. If solid-phase bioremediation is selected
remediation, efforts to contain volatile emiss.ons she,
undertaken.
5.6 Preliminary Studies
i. Bioremediation represents a potentially e-f-Cw
means for removing creosote constituents from groun • ;v;sx
present at the ACW site.
ii. Bioremediation represents a potentially e.iiec'<.
means of treating creosote-contaminated solidified mauvi.u
However, the pH of the substrate must be adjusted to relics
ity, and the addition of indigenous microorganisms app; _:n'
accelerate the rate of biodegradation.
42
-------
Appendix A
43
-------
PILOT SOIL WASHING AT
AMERICAN CREOSOTE WORKS
PENSACOLA FLORIDA
OVERVIEW
by
CHAPMAN. INC.
FREEHOLD, NJ 07728
Purchase Order # 9003A075
To Technical Resources, Inc.
EPA Contract No. 68 - 03 - 3479
May 30,1990
U. S. ENVIRONMENTAL PROTECTION AGENCY
ENVIRONMENTAL RESEARCH LABORATORY
SABINE ISLAND
GULF BREEZE, FLORIDA 32561
45
-------
OVERVIEW
BACKGROUND
Soil at the old American Creosote Woiks Site in Pensacola Florida is contaminated as a resuii
of past wood treating operations. Bioremediation is a treatment option being investigated by the US
EPA, and in one of the approaches under evaluation, EPA researchers biotreat dispersed creosote and
creosote residuals in an aqueous slurry. Reverse osmosis is used to polish the wash water prior to
discharge. In order to obtain slurries for lab and pilot scale tests, Chapman, Inc. was engaged to was! •,
surface soil and sandy sediment from beneath an unlined waste lagoon. Soil washing was performed
both at the site and at a Chapman, Inc. facility.
BENCH TESTS
Approximately six pounds of surface soil, taken from site grid #47, was sent to Chapman for
preliminary bench washing tests. These tests were conducted to determine an effective dispersing wash
solution. Using the theory that 90 to 99% of the contamination is in the fine fraction of this otherwise
sandy soil, no effort was made to determine solubilization of creosote from sand surfaces. Effectiveness
was based on settling rates and cumulative volumes of the coarse fraction in Imhoff cones, At first
three solutions were used: water alone, CitrikleenR, and Moncosolve" 100. Both products were used
at 1 -pound/ton soil (500-mg/kg.) Water washing produced an unstable dispersion containing the finer
soii fraction that represented 23% of the soil. Citrikleen" dispersed some fine grain sand and producer
a stable dispersion containing 50% of the finer soil fraction. A 27% moderately stable dispersion v.as
produced using Moncosolve". Subsequently a third product was evaluated. Because of successtu,
washing tests on another project using a laundry product (brand name Nancy B"), this powdered
detergent was included. It produced a very stable dispersion containing 27% fine material Nr
sediment material was available for bench testing.
PILOT SOIL WASHER
The pilot soil washer used to produce wash slurries for biotreatment and reverse osmosis
studies consists of three unit operations. They are:
A single deck screen to remove material considered oversize for this study
A single shaft paddle mixer to blend the washing solution and screened soii
An up-flow separator designed to elutriate the suspended material from the coarser
settled soil fractions.
Both the screen and mixer are designed for continuous operation. The separator is a batch unit and
designed for this particular job. All three units are mounted on a 12-foot long trailer. Figure 1 is a
picture of the unit at the American Creosote Works Site. In the configuration shown the unit can handle
sand and loam soils that have weak aggregates.
FIELD WORK AT AMERICAN CREOSOTE WORKS SITE
Both contaminated surface soil and the sandy sediment matrices were washed at the American
Creosote Works Site. The surface matrix had very similar characteristics to the sample studied during
46
-------
the bench tests. (This was not the case with the surtace soil used in a second round of pilot tests.)
I; was a moist sandy loam with approximately 12% debris - mostly broken stone and brick. The
sediment matrix was heavily contaminated sand with no debris other than aggregates of sand and fines
held together by creosote. Free creosote that drained out of the sediment as it was removed. In total
200 pounds of soil were washed resulting in 165 gallons of wash slurry or 0.83-gallons/pound of soil.
WASHING THE SURFACE SOIL
When washing the surface matrix soil all three process units were used. Nancy BR detergent,
a powder, was added to the feed hopper of the single deck screen at a rate of 1-pound/ton of soil.
A total of 125 pounds of soil was weighed out incrementally on a platform scale. Because the 1-
pound/ton dosage rate was based on the total soil the actual rate, after the oversized material was
removed, was 1.15-pound/ton.
After passing through the screen the soil entered the paddle mixer through a neoprene
interconnect tube. Inside the mixer water was added to the soil at .25-gallon/minute. Since there was
only a small quantity of soil being tested, the mixer operated only five minutes. In that time 85-pounds
mixed soil/water was discharged to provide slurry for biotreatment and RO studies.
The roughly 74-pounds of soil (mix less the water) was then separated in the up-flow separator
shown in Figure 2. This produced a total of 60-gallons of slurry. Thirty-five gallons were placed in a
55 gallon drum, 5-gallon in each of two 5-gallon pails, and the balance discharged back to the site.
The water usage rate was 0.8-gallon/pound of soil. Slurry and washed soil samples were taken for
analysis by the EPA laboratory, Gulf Breeze.
WASHING THE SEDIMENT
Of the three units in the pilot system only the up flow separator was used when washing the
sediment matrix. No screening was necessary. And, since there was a limited amount of material, hand
mixing was judged to make more efficient use of what was available. Two sediment wash tests were
done: a preliminary test, and the one reported below.
Twenty-five pounds of sediment, six grams of Nancy BH and 400-milliliters of water were blended
in a 5-gallon pail to a uniform consistency. After mixing sediment was incrementally added to the up-
flow separator. The wash slurry volume was approximately 38-gallons which represents a rate of 1.5
gallons/pound of soil. Wash slurry and washed sediment samples were taken for analyses by the EPA
Lab at Gulf Breeze. The majority of the wash slurry was placed in a 55-gallon drum (along with wash
slurry from the preliminary sediment wash test.) Five gallons of slurry were taken for biotreatment tests.
TOXICITY TESTS
Toxicity tests performed at the Gulf Breeze Lab showed that the detergent Nancy BR is toxic to
tne bacteria intended for use in biotreatment at the site. Chapman, Inc. was notified and requested to
supply an alternate product(s) and submit it (them) for toxicity testing. Two products were formulated
and tested. One of the two was found acceptable.
Because of an EPA requirement that all formulations must be fully disclosed and that it would
oecome public information, Chapman chose not to disclose the new acceptable formulation. A second
round of soil washing was requested by EPA using a nonproprietary dispersing agent such as Triton
X-100.
47
-------
SECOND PILOT SOIL WASHING TESTS
Two separate washing tests were repeated. For each of two 34-pound samples Triton X-100
(@ 1-pound/ton) was added and mixed by hand. No additional water was added to the sediment
matrix since there was free water present. The surface soil matrix required more liquid so the Triton
X-100 was dissolved in 1-liter of water before being added to the soil. An additional 0.6-liter of water
was required during mixing. Thirty-five to thirty seven-gallons of wash slurry was produced from each
of the samples using the up-flow separator. Because of the small size of the samples, the only unit
process used from the pilot system was the up-flow separator.
The sediment matrix did not require screening and a Gilson vibratory screen was used to screen
the surface soil. One observation of the surface soil sample used in the repeat work was that it had
a low bulk density of 62-pound/ft3. Excavated soil is most often in the 75 to 95-pound/ft3 range.
Another unusual characteristic of the surface soil was the consistency of the mix. It was like a granular
butter cake icing.
SUMMARY
The work reported above was totally restricted to the physical/mechanical aspects of soil
washing and specifically to the production of a wash slurry/sludge that could be used for biotreatment
and reverse osmosis treatment studies. No chemical analyses were performed as part of this work and
for this reason are not reported.
General observations of the behavior of the contaminated matrices in terms of partitioning and
wettability during washing are:
1. The sediment soil, although evidently containing high quantities of
creosote, is easily dispersed.
2. Hand mixing did not shear the frequently encountered aggregates held
together by nondispersed viscous creosote residuals. These aggregates
would deform when mixed but were not dispersed. They were visible
in the mix, and when individually sliced with the edge of the trowel, they
dispersed easily. This characteristic, encountered in the sediment matrix
only, could be overcome by a kneader mixer which would apply greater
shear force to the aggregates than the single paddle mixer.
3. The surface soil is easily dispersed and the fine fractions can be easily
separated from the sand and coarse fractions.
4. The up-flow separator was not adequate in removing fine material from
coarse. Fine material that was loosely associated with coarser material
was "piggy-backed" to the clean soil collector.
General operational characteristics of the pilot work are presented in Table 1. These values are
presented in a per ton basis in Table 1(A). In 1(B) these conditions have been converted to a per
minute basis for a 20-ton/hr washing system.
48
-------
TABLE I PILOT STUDY OF SOIL WASHING FOR AWC SITE
Sediment
Soil
(A) GENERAL OPERATIONAL
CHARACTERISTICS
Dispersing Agent
Mixing Water
Total Process Water
1.0#/ton
0-9 gal/ton
1600-3000 gal/ton
1.0#/ton-1/2#/ton
25 gal/ton
1600-2000 gal/ton
(B) BASED ON A 20-TON PER
HOUR SYSTEM
Agent
Mixing Water
Total Process Water
Sludge @ 15% Solids
20#/hr
0-3 gpm
530-1000 gpm
110 gpm
20-24#/hr
8.5 gpm
530-670 gpm
135 gpm
49
-------
FIGURE 1. Chapman Mobile Soil Washer pilot unit at the American
Creosote Site, Pensacola, Florida
50
-------
SOIL SLURRY
FRESH WATER
FIGURE 2. An up-flow separator used for pilot treatment studies
at the American Creosote Site, Pensacola, Florida
51
-------
Appendix B
53
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
REGION IV, ATHENS, GEORGIA
MEMORANDUM
'\YTE:
SEP 12 1990
SUBJECT: American Creosote Works, Pensacola, Florida, Treatability Study
Analytical Results
!'?OM: Dan Thoman, Regional Expert
Hazardous Waste Section
Environmental Compliance Branch "\7~l^T T ^~^~\A7"
Environmental Services Division •*• *-JJLjL^\J VV
Date
,>,^-"
Originator
Natalie Ellington Initials
Souch Site Management Section
Superfund Branch
Waste Management Division
Unit Chief
William R. Bokey, Chief
Hazardous Waste Section W.R. Bokey Chief
Environmental Compliance Branch
Environmental Services Division
Attached are the analytical results for the treatability study samples submitted
by the Gulf Breeze Environmental Research Laboratory.
If you have any questions, please call me at FTS 250-3172.
Attachment
Finger/Wright
Bokey/Hall
Knight
YELLOW COPY THOMAN:dpt:September 11, 1990:ECB/HWS:3351
55
-------
AMERICAN CREOSOTE WORKS
PENSACOLA FLORIDA
DATA SUMMARY TABLE
TREATABILITY STUDY
1-BR 2-BR 6-BR 7-BR 8-BR 9-BR 10-BR 11-BR
06/14/90 06/14/90 07/09/90 07/09/90 07/09/90 07/09/90 07/09/90 07/09/90
EXTRACTABLE ORGANIC COMPOUNDS
UG/L
in
CD
Quinolinol
Methylphenanthrene (3 -isomers)
Benzofluorene (2-isomers)
Methylfluoranthene (5 isomers)
Benzanthracenone (2 isomers)
Benzofluoranthene (not B or K)(3 isom
Methylbenzoanthracene
Anthracenecarbonitrile 8JN
Methylfluoranthene (2 isomers)
Benzanthraceneone (2 isomers)
Benzofluoranthene (not B or K)(4 isom --
Methylbenzanthracene
Naphthacenedione
Petroleum Product
DimethyInaphthalene (3 isomers)
(Propenyl)naphthalene (2 isomers)
Methylbiphenyl (2 isomers)
Methylfluorene
Benzofluoranthene (not B or K)
1-MethyInaphthalene
Ethenylnaphthalene
EthyInaphthalene
DimethyInaphthalene (4 isomers)
TrimethyInaphthalene
(Propenyl)naphthalene (3 isomers)
Methyldibenzofuran (2 isomers)
Methylfluorene (2 isomers)
Dibenzothiophene
Benzoquinoline
Carbazole
Methylphenanthrene (4 isomers)
Cyclopentaphenanthrene
PhenyInaphthalene
Benzofluorene (2 isomers)
UG/L
UG/KG
UG/KG
UG/KG
UG/KG
2000JN
800JN
300JN
20000JN
7000JN
30000JN
4000JN
3000JN 3000JN
5000JN
7000JN
30000JN
4000JN
2000JN
N N
- -
. .
. .
. -
. .
- -
. .
- -
500000JN - -
200000JN - -
200000JN
90000JN
900JN
700JN
200JN
300000JN 300000JN
200000JN 200000JN
60000JN 50000JN
300000JN
200JN
700JN
300JN
200000JN
100000JN
300000JN
70000JN
600000JN
500000JN
300000JN
100000JN
200000JN
200000JN
300000JN
70000JN
600000JN
500000JN
300000JN
90000JN
200000JN
UG/KG
10000JN
UG/KG
300000JN
200000JN
70000JN
600000JN
60000JN
200000JN
300000JN
200000JN
300000JN
80000JN
700000JN
500000JN
300000JN
100000JN
200000JN
-------
en
AMERICAN CREOSOTE WORKS
PENSACOLA FLORIDA
DATA SUMMARY TABLE
TREATABILITY STUDY
1-BR 2-BR 6-BR 7-BR 8-BR 9-BR 10-BR 11-BR
06/14/90 06/14/90 07/09/90 07/09/90 07/09/90 07/09/90 07/09/90 07/09/90
EXTRACTABLE ORGANIC COMPOUNDS
2-METHYLNAPHTHALENE
NAPHTHALENE
ACENAPHTHENE
DIBENZOFURAN
FLUORENE
N-NITROSODIPHENYLAMINE/DIPHENYLAMINE
PHENANTHRENE
ANTHRACENE
FLUORANTHENE
PYRENE
BENZO(A)ANTHRACENE
CHRYSENE
BENZO(B AND/OR K)FLUORANTHENE
BENZO-A-PYRENE
INDENO (1,2, 3-CD) PYRENE
DIBENZO(A.H)ANTHRACENE
BENZO(GHI)PERYLENE
2-METHYLPHENOL
(3-AND/OR 4-)METHYLPHENOL
PHENOL
2,4-DIMETHYLPHENOL
PENTACHLOROPHENOL
Diphenylcyclopropenone
Benzofluoranthene (not b or k) ( 2-is
Carboxybenzeneacetic Acid
Ethenylmethylbenzene
DimethyIphenol (not 2,4)
Benzothiophene
Isoquinoline (2-isomers)
PropyIphenol
Benzeneacetonitrile
Methylisoquinoline (4-isomers)
Dimethylnaphthalene (3-isomers)
Naphthalenecaronitrile
Propenylnaphthalene
Methyldibenzofuran (2-isomers)
UG/L
6JN
30JN
UG/L
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
840J
2800
720J
1500
4700
100JN
200JN
2000JN
1000JN
4000JN
1000JN
600JN
2000JN
1000JN
200JN
100JN
500JN
120000
110000
190000
UG/KG
9.5J
_ _
5.2J
5.1J
9.8J
35J
13J
13J
14J
2000
6300
1700
1400
1600
—
4000
500J
1400
940J
260J
260J
—
--
—
2500J
1900J
19000
24000
13000J
21000
49000
17000
11000J
11000J
--
1900J
1900J
16000
22000
11000J
21000
48000
16000
9900J
2900J
9700J
700000
390000
880000
8-20000
1.1E6
2.3E6
1.9E6
1.2E6
730000
170000J
280000J
110000J
630000
190000J
870000
810000
1.1E6
37000J
2.3E6
1.8E6
950000
640000
170000J
290000J
100000J
--
--
--
--
11000J
31000J
37000J
14000J
25000J
49000J
15000J
--
--
750000
250000J
940000
880000
1.2E6
2.6E6
2.1E6
1.2E6
780000
180000J
310000J
120000J
-------
PURGEABLE ORGANIC COMPOUNDS
TRICHLOROFLUOROMETHANE
CHLOROMETHANE
ACETONE
METHYL ETHYL KETONE
CHLOROFORM
BENZENE
TOLUENE
ETHYL BENZENE
(M- AND/OR P-)XYLENE
0-XYLENE
STYRENE
TETRAHYDROFURAN
g PINENE
ETHYLMETHYLBENZENE
TRIMETHYLBENZENE (2 ISOMERS)
Pinene
Ethylmethylbenzene (2 isomers)
Trimethylbenzene
Propynylbenzene
Petroleum product
AMERICAN CREOSOTE WORKS
PENSACOLA FLORIDA
DATA SUMMARY TABLE
TREATABILITY STUDY
1-BR
06/14/90
UG/L
1.1J
--
3.0J
20JN
2-BR
06/14/90
UG/L
430
84J
12 J
34
18 J
66
34
21J
80JN
40JN
100JN
6-BR
07/09/90
UG/KG
5.7J
7-BR
07/09/90
UG/KG
8-BR
07/09/90
UG/KG
—
—
9-BR
07/09/90
UG/KG
—
—
—
—
—
10 -BR
07/09/90
UG/KG
_ _
11-BR
07/09/90
UG/KG
34J
- - .
_ _
_ _
_ _
_ _
_ _
- -
. -
N
N
100JN
N
N
5000JN
700JN
1000JN
20000JN
N
****************************************************************
***FOOTNOTES***
J - ESTIMATED VALUE
N - PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
- - - MATERIAL WAS ANALYZED FOR BUT NOT DETECTED
BR - SURFACE SOIL SLURRY
-------
PURGEABLE ORGANICS DATA REPORT
SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS. GA.
07/09/90
««* *PROJECT*NO.*90-654 * * SAMPLE NO. 47346
«« SOURCE: AMERICAN CREOSOTE
«* STATION ID: 1-BR SURFACE SOIL SLURRY
**
UG/L* * * ANALYTICAL RESULTS
en
SAMPLE TYPE: WATER
1 J
0U
0U
0U
.0U
5.0U
50U
50U
5.0U
5 OU
5.C"
50U
5.0U
5.0U
SOU
5.CJJ
3.0J
.0U
.0U
OU
.
5.
5.
5
5.0U
5 oij
5 Oo
5 . OU
5 OU
C.CU
CHLOROMETHANE
VINYL CHLORIDE
BROMOMETHANF
CHLOROETHANE
TK1CHLOROFLUOROMETHANE
1 . 1-DICHLOROETHENE( 1 , 1-DICHI OROETHYLENE)
ACETONE
CARBON D TSUI. FIDE
METHYLENE ClILORIDC
TKONS-! ,2-DICHLCP.OtTHENE
1 , l-DICiiLOROCTHAWE
VINYL ACETATE
CIS-1.2-DICHLOROETHENE
2. 2-C I CHLOROPROP ANC
Mtiwvu tTHVL K.EiONE
BRCJnOCHLOROmcTriAWE
CHLOROFORW
i.i. 1-TRIOHI.OftriETHANt
1 . 1-DICHLOROPROPENiE
r.ARBON TETRACHLORIDE
1 .2-DICHLOROtTHANE
TRICriLOKOETHFNei TK1CHLOROETHYLENE)
1 . 2-D I CHLOROPROP ANE
niBROMOMETHANE
BKuBiODICriLOROMETHANc
PROG ELEM: SSF COLLECTED BY: D THOMAN
CITY: PENSACOLA ST: FL
COLLECTION START: 06/14/90 STOP: 00/00/00
**
**
* * * * ***
UG/L ANALYTICAL RESULTS
SOU CIS-1.3-DICHLOROPROPENE
50U METHYL ISOBUTYL KETONE
5.0'J TOLUENE
5 OU TRANS-1 .3-DICHLOROPROPCN!!
5'OU 1 1 ,2-TRICHLOROETHANE
5'OU TETRACHLOROETHENE(TETRACHLOROETHYLENE)
^ OU 1 3-DICHLOROPROPANE
SOU METHYL BUTYL KETOWF
5 OU DIBROMOCHLORCMETIIAWE
5 OU CHLORORFM2EME
5'OU 1,1,1,2-TCTRACHLOROETHANE
b UU ETHYL BENZENE
5.0U (M- AND/OR P-)XYLENF
5 OU 0-XYLENE
5 OU STYRFNF
5 OU SRC'.10rOR?«
"=, OU BROM05EN2ENE
501) 1 1 . 2.2-TETRAf.HLOROETHANE
^ OU 1 2,3-TRICHLCROPROPANE
5.0U O-CHLOftOTOL'.'tNt
5.0U P-CHLOROTOLUENE
c, nu 1 ^-DUJHL'JKOBENZENE
5.0U 1 '. 4-DICriLOROBEMZcNE
5.0'.l 1,2-DICHLCRCBENZENE:
.
KtD.iMMtNDhD HOLDING TIME EXCEEDED PURGEABLC ORGANICS
'*
***»A-AVERAGE*VALUE »NA-NOT ANALYZED .MAI-INTERFERENCES *J-EST!MATED VALUE «N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
•K-ACTUAL VALUE IS KNOWN TO BE LESS THAN VALUE GIVEN *L-ACTUAL VALUE IS KNOWN TO BE GREATER THAN VALUE GIVEN
*U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
-------
SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD, ATHENS, GA. 07/09/90
MISCELLANEOUS PURGEABLE ORGANICS - DATA REPORT
»***************•»*«„.„„,,.„,_. .»..*_? *»«»»**»******»*«»»»***.».»«»»»»»«»
»* SOURCE1 AMERICAN5CREOSOTEPLE N°' ^^^ SAMPLE TYPE: WATER PR°G ELEM: SSF COLLECTED BY: u I HUMAN
*« STATION ID: 1-BR SURFACE SOIL SLURRY COLLECTIO^START: 06/14/90 ^ FL STOP: 00/00/00
»** * * T *
**
*»
ANALYTICAL RESULTS UG/L
20JN TETRAHYDROFURAN
en
o
t*fREMARKS*»* ««»REMARKS*»*
RECOMMENDFO HOLDING TIME EXCEEDED-PURGEABLE ORGANICS
*-*FOOTNOTES'»»
„ nr. T.-^T^^ ^ ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
*R-OC INDICATES THAT DATA UNUSABLE. COMPOUND MAY OR MAY NOT BE PRESENT. RESAMPLING AND REANALYSIS IS NECESSARY FOR VERIFICATION.
-------
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UJUJH
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61
-------
SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA. 07/12/90
MISCELLANEOUS EXTRACTABLE COMPOUNDS - DATA REPORT
xx* x**x*******x***xx*xxx***x*x****x*xx*x*t*******'*****«********** ***
«« PROJECT NO. 9O-654 SAMPLE NO. 47346 SAMPLE TYPE: WATER PROG ELEM- SSF COLLECTED BY: D THOMAN **
»» SOURCE: AMERICAN CREOSOTE CITY: PENSACOLA ST: FL • «*
** STATION ID: 1-BR SURFACE SOIL SLURRY COLLECTION START: 06/14/90 STOP: 00/00/00 «*
»» **
XX* *X******»»»******X***»»»*»***»*X*X*X********** •*'*'*"t**f*t**X**** ***
ANALYTICAL RESULTS UG/L
8JN AnthracenecarbonHMle
6JN Diphenylcyclopropenone
30JN Benzofluoranthene (not b or k) ( 2-isomers)
N Petroleum product
o>
ro
***FOOTNOTES*»»
*A-AVERAGE VALUE «NA-NOT ANALYZED «NAI-INTERFERENCES *J-ESTIMATED VALUE *N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
*K-ACTUAL VALUE IS KNOWN TO BE LESS THAN VALUE GIVEN *L-ACTUAL VALUE IS KNOWN TO BE GREATER THAN VALUE GIVEN
• U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT ,,„„.,„,,,.-„„..,
*R-QC INDICATES THAT DATA UNUSABLE. COMPOUND MAY OR MAY NOT BE PRESENT. RESAMPLING AND REANALYSIS IS NECESSARY FOR VERIFICATION.
-------
PURGEABLE ORGANICS~DATA REPORT
SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD, ATHENS, GA.
O7/09/90
***
**
* *
PROJECT NO. 90-654 SAMPLE NO. 47347
SOURCE: AMERICAN CREOSOTE
STATION ID: 2-BR SEDIMENT SLURRY
SAMPLE TYPE: WATER
PROG ELEM: SSF COLLECTED BY: D THOMAN
CITY: PENSACOLA ST: FL
COLLECTION START: 06/14/90 STOP: 00/00/00
UG/L
25'J
25U
25U
25U
25U
25U
430
250U
25U
25U
25U
26OU
25U
25U
8• M'* ME
TRICHLOROETHF.NF(TRICHLOROETHYLENE)
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25U
1»0
66
34
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25U
25U
25U
2bU
25U
25U
2s?"
25U
25U
ANALYTICAL RESULTS
CIS-1,3-DICHLOROPROPENE
METHYL ISOBUTYL KETONE
TOLUENE
TRANS-1,3-DICMLCROPROPCNC
1,1,2-TRICHLOROETHANE
TETRACHLOROETHENE( TETRACHLOROETHYLENE)
1.3-DICHLOROPROPANE
METHYL BUTYL K-tTONF
DIBROMOCHLCRCMETIIAMC
CHI.ORORFNZENE
1.1,1.2-TCTRACHLOROETHANE
ETHYL BENZENE
(M- AND/OR P-)XYLENF
0-XYLENE
STYftFNF
*****
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1.1.2. 2-TETRACHLOftOETHAME
1,2. 3-TR I CHLOROPROPANE
0-f.HLOROTULUtNt
P-CHLOROTOLUENE
i!4-iCHLOROBtNZENE
1.2-DICHLCRCBENZENE
. __
DROMOD i CHLOROMETHANE
KttUVMtNDED HOLDING TIME EXCEEDED PURGEAOLC ORGANICS
•A-AVERAGE VALUE »NA-NOT ANALYZED »NAI-INTERFERENCES .J-ESTIMATED VALUE «N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
•K-ACTUAL VALUE IS KNOWN TO BE LESS THAN VALUE GIVEN «L-ACTUAL VALUE IS KNOWN TO BE GREATER THAN VALUE GIVEN
»U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
-------
SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD, ATHENS. GA. 07/09/90
MISCELLANEOUS PURGEABLE ORGANICS - DATA REPORT
**T **»*»********»***»*»»»
nnprF iFRrpFAC °- 47347 SAMPLE TYPE: WATER PROG ELEM: SSF COLLECTED BY: D THOMAN
»* SOURCE: AMERICAN CREOSOTE CITY- PENSACOLA «iT- Fl
** STATION ID: 2-BR SEDIMENT SLURRY COLLECTION START: 06/14/90 STOP. 00/00/00
ANALYI1CAL RESULTS UG/L
80-JN PINENE
40JN ETHYLMETHYLBFN7FMF
100JN1 TRIMETHYLBENZENE (2 ISOMERS)
*»»REMARKS»»»
RECOMMENDFD HOLDING TIME EXCEEDED-PURGEABLE ORGANICS
*»*FOOTNOTES»»»
'A-AVERACE VALUE *MA-NOT AMALVZED *NAI-INTFRFFK£NCtS «J-ESTIMA1ED VALUE »N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
»K-Af.TuAL VALUt IS KNOWN TO BE LESS THAN VALUE GIVEN *L-ACTUAL VALUE IS KNOWN TO BE GREATER THAN VALUE GIVEN
•U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
*R-QC INDICATES THAT DATA UNUSABLE. COMPOUND MAY OR MAY NOT BE PRESENT. RESAMPLING AND REANALYSIS IS NECESSARY FOR VERIFICATION
-------
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA.
07/12/90
MISCELLANEOUS EXTRACTABLE COMPOUNDS -
*x* xxxxxxxxxxxxxxxxxxxx
«» PROJECT NO. 90-654 SAMPLE NO. 47347
»* SOURCE: AMERICAN CREOSOTE
** STATION ID: 2-BR SEDIMEMT SLURRY
* *
XX* XX**XXXXXXXX*X*XXXXX
DATA REPORT
SAMPLE TYPE: WATER
PROG ELEM: SSF COLLECTED BY: D THOMAN
CITY: PENSACOLA ST: FL
COLLECTION START: 06/14/90 STOP: 00/00/00
XX
XX
CD
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ANALYTICAL RESULTS UG/L
100JN Carboxybenzeneacetlc Add
200JN Ethenyimethylbenzene
2000JN Dimethylphenol (not 2.4)
1000JN Benzotniophene
4000JN Isoqulnoline (2-1somers)
1000JN Propylphenol
600JN BenzeneacetonHMle
2000JN MethylIsoqu1no11ne (4-1somers)
900JN 1-Methyl naphthalene
700JN Ethenyinaphthalene
200JN Ethylnaphthalene
1000JN Dimethylnaphthalene (3-1somers)
200JN Naphthalenecaronltr He
100JN Propenylnaphthalene
500JN Methyldlbenzofuran (2-1somers)
2000JN Quinollnol
200JN Benzoqu1nol1ne
700JN Carbazole
800JN Methylphenanthrene (3-1somers)
300JN Cyclopentaphenanthrene
300JN Benzofluorene (2-isomers)
*»»FOOTNOTES»««
»A-AVERAGE VALUE »NA-NOT ANALYZED »NAI-INTERFERENCES »J-ESTIMATED VALUE *N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
*K-ACTUAL VALUE IS KNOWN TO BE LESS THAN VALUE GIVEN *L-ACTUAL VALUE IS KNOWN TO BE GREATER THAN VALUE GIVEN
•U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
»R-QC INDICATES THAT DATA UNUSABLE. COMPOUND MAY OR MAY NOT BE PRESENT. RESAMPLING AND REANALYSIS IS NECESSARY FOR VERIFICATION.
-------
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-------
SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA. 07/25/90
MISCELLANEOUS EXTRACTABLE COMPOUNDS - DATA REPORT
»»*»»**»*»***********»*»»**»»****«*»»****»*»«»*» »'»»»»*»***»*»***»»*»
»» PROJECT NO. 90-715 SAMPLE NO. 48154 SAMPLE TYPE: SOIL PROG ELEM: SSF COLLECTED BY: D TROMAN «»
»* SOURCE: AMERICAN CREOSOTE CITY: PENSACOLA ' ST: FL »«
«» STATION ID: 6-BR COLLECTION START: 07/09/90 1500 STOP: 00/00/00 »*
»* **
**»*»*«***»****«*****»»*»*»»«***»*»»»*•*»»******»»'*'***'»*********»»**»
ANALYTICAL RESULTS UG/KG
3000JN AnthracenecarbonHMle
20000JN Methylfluoranthene (5 isomers)
7000JN Benzanthracenone (2 Isomers)
30000JN Benzofluoranthene (not B or K)(3 Isomers)
4000JN Methylbenzoanthracene
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD, ATHENS, GA. 07/25/90
MISCELLANEOUS EXTRACTABLE COMPOUNDS - DATA REPORT
«» PROJECT NO. 90-715 SAMPLE NO. 48155 SAMPLE TYPE: SOIL PROG ELEM: SSF COLLECTED BY: D THOMAN
** SOURCE: AMERICAN CREOSOTE CITY: PENSACOLA ST: FL
** STATION ID: 7-BR COLLECTION START: 07/09/90 1500 STOP: 00/00/00
ANALYTICAL RESULTS UG/KG
3000JN AnthracenecarbonltMle
5000JN Methylfluoranthene (2 Isomers)
7000JN Benzanthraceneone (2 Isomers)
30000JN Benzofluoranthene (not B or K.H4 Isomers)
4000JN Methylbenzanthracene
2000JN Naphthacenedlone
N Petroleum Product
***FOOTNOTES»»*
*A-AVERAGE VALUE *NA-NOT ANALYZED »NAI-INTERFERENCES »J-ESTIMATED VALUE *N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
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«U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA. 07/26/90
MISCELLANEOUS PURGEABLE ORGANICS - DATA REPORT
*
AUPp?RlM1^Pn^TpPLE m~ 48156 SAMPLE TYPE: SOIL PROG ELEM: SSF COLLECTED BY: OTTOMAN
ATI™ AKER£CA:D CREOSOTE CITY: PENSACOLA ST: PL
STATION ID: 8-BR COLLECTION START: 07/09/90 1500 STOP: 00/00/00
ANALYTICAL RESULTS UG/K.G
N Petroleum product
»**FOOTNOTES*»*
*A~A^lR,AGE,,yAL^E *NA-NOT ANALYZED »NAI-INTERFERENCES 'J-ESTIMATED VALUE 'N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD, ATHENS. GA.
07/25/90
MISCELLANEOUS EXTRACTABLE COMPOUNDS - DATA REPORT
PROJECT NO. 90-715 SAMPLE NO.
SOURCE: AMERICAN CREOSOTE
STATION ID: 8-BR
48156 SAMPLE TYPE: SOIL
PROG ELEM: SSF COLLECTEDBY: D THOMAN
CITY: PENSACOLA ST: FL
COLLECTION START: 07/09/90 1500 STOP: 00/00/00
* *
*•*
**
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ANALYTICAL RESULTS UG/KG
300000JN 1-MethylnaphthaTene
200000JN Etheny(naphthalene
60000JN Ethyl naphthalene
500000JN Dlmethylnaphthalene (3 Isomers)
200000JN (Propenyl)naphtha1ene (2 Isomers)
200000JN Methylcnbenzofuran (2 Isomers)
100000JN Methvlfluorene (2 Isomers)
300000 JN D1t>enzothlophene
70000JN Benzoquinoline
500000JN Methylphenanthrene (4 Isomers)
300000JN Cyclopentaphenanthrene
100000JN Phenylnaphthalene
2OOOOOJN Benzofluorene (2 Isomers)
600000JN Carbazole
»*«F001 NOTES'"
•A-AVERAGE VALUE »NA-NOT ANALYZED »NAI-INTERFERENCES *J-ESTIMATED VALUE »N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
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•U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
*R-OC INDICATES THAT DATA UNUSABLE. COMPOUND MAY OR MAY NOT BE PRESENT. RESAMPLING AND REANALYSIS IS NECESSARY FOR VERIFICATION.
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA. 07/31/90
MISCELLANEOUS PURGEABLE ORGANICS - DATA REPORT
*« PROJECT NO. 9O-715 SAMPLE NO. 48157 SAMPLE TYPE: SOIL PROG ELEM: SSF COLLECTED BY: D THOMAN
** SOURCE: AMERICAN CREOSOTE CITY: PENSACOLA ST: FL
«* STATION ID: 9-BR COI LECTION START: 07/09/90 1500 STOP: 00/00/00
**
fff ********************»*»««*»****»«*»**»****»*»****»*****»»»
ANALYTICAL RESULTS UG/KG
100JN TMmethyl benzene
N Petroleum product
***FCXJTNOTES«»»
*A-AVERAGE VALUE *NA-NOT ANALYZED *NAI-INTERFERENCES *J-ESTIMATED VALUE *N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD, ATHENS, GA.
MISCELLANEOUS EXTRACTABLE COMPOUNDS - DATA REPORT
*** ******************************
«* PROJECT NO. 90-715 SAMPLE NO. 48157 SAMPLE TYPE: SOIL
** SOURCE: AMERICAN CREOSOTE
** STATION ID: 9-BR
PROG ELEM: SSF COLLECTED BY: D THOMAN
CITY: PENSACOLA ST: FL
COLLECTION START: 07/09/90 1500 STOP: 00/00/00
*» *
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ANALYTICAL RESULTS UG/KG
300000JN 1-Methyl naphthalene
200000JN Ethenyinaphthalene
50000JN Ethyl naphthalene
300000JN Dimethylnaphthalene (4 Isomers)
200000JN Methylblphenyl (2 Isomers)
200000JN Methyldlbenzofuran (2 Isomers)
90000JN Methvlfluorene
300000JN Dibenzothlophene
70000JN Benzoquinol me
600000JN Carbazole
500000JN Methylphenanthrene (4 Isomers)
300000JN Cyclopentaphenanthrene
90000JN Phenylnaphthalene
200000JN Benzofluorene (2 Isomers)
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA. 07/31/90
MISCELLANEOUS PURGEABLE ORGANICS - DATA REPORT
** PROJECT NO. 90-715 SAMPLE NO. 48158 SAMPLE TYPE: SOIL PROG ELEM: SSF COLLECTED BY: D THOMAN «»
»* SOURCE: AMERICAN CREOSOTE CITY: PENSACOLA ST: FL **
»* STATION ID: 10-BR COLLECTION START: 07/09/90 1500 STOP: 00/00/00 »»
** **
*** **»*»**»»**»**»*»»**»*«»»*»»»**««»»*»»»»**»****»************«* *»»
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N Petroleum product
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA. 07/25/90
MISCELLANEOUS EXTRACTABLE COMPOUNDS - DATA REPORT
*t* *»******»***»*************»*»»*»*»*******»**»***»*»«*»**»«»»»» ***
«» PROJECT NO. 90-715 SAMPLE NO. 48158 SAMPLE TYPE: SOIL PROG ELEM: SSF COLLECTED BY: D THOMAN *«
»» SOURCE: AMERICAN CREOSOTE CITY: PENSACOLA ST: FL »«
«» STATION ID: 10-BR COLLECTION START: 07/09/90 1500 STOP: 00/00/00 «»
*» **
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ANALYTICAL RESULTS UG/KG
10000JN Benzofluoranthene (not B or K)
»*«FOOI'NOTES»*»
*A-AVERAGE VALUE »NA-NOT ANALYZED *NAI-INTERFERENCES *J-ESTIMATED VALUE *N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
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«U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT. ^T^.-T™,
*R-QC INDICATES THAT DATA UNUSABLE. COMPOUND MAY OR MAY NOT BE PRESENT. RESAMPLING AND REANALYSIS IS NECESSARY FOR VERIFICATION.
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD. ATHENS, GA. 07/26/90
MISCELLANEOUS PURGEABLE ORGANICS - DATA REPORT
*** ft****************************************** »"* ******»**»«»»*»» ***
»* PROJECT NO. 90-715 SAMPLE NO. 48159 SAMPLE TYPE: SOIL PROG ELEM: SSF COLLECTED BYc D THOMAN **
*» SOURCE: AMERICAN CREOSOTE CITY: PENSACOLA ST: FL ««
** STATION ID: 11-BR COLLECTION START: 07/09/90 1500 STOP: 00/00/00 «
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5000JN P i nene
700JN Ethylmethylbenzene (2 Isomers)
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20000JN Propynylbenzene
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SAMPLE AND ANALYSIS MANAGEMENT SYSTEM
EPA-REGION IV ESD, ATHENS, GA.
07/25/90
MISCELLANEOUS EXTRACTABLE COMPOUNDS -
*** *****************
** PROJECT NO. 90-715 SAMPLE NO 48159
** SOURCE: AMERICAN CREOSOTE
** STATION ID: 11-BR
DATA REPORT
SAMPLE TYPE* SOIL*
* » *
00
00
PROG ELEM: SSF COLLECTED BY: D THOMAN
CITY: PENSACOLA ST: FL
COLLECTION START: 07/09/90 1500 STOP: 00/00/00
«**
**
* *
**
* *
ANALYTICAL RESULTS UG/KG
300000JN 1-Methylnaphthalene
200000JN Ethenyinaphthalene
70000JN Ethyl naphthalene
600000JN Dimethylnaphthalene (4 Isomers)
60000JN TMmethylnaphthalene
200000JN (Propenyl)naphthalene (3 Isomers)
300000JN Methyl ciibenzofuran (2 isomers)
200000JN Methylfluorene (2 Isomers)
300000JN Dibenzothlopnene
80000JN Benzoqu\no11ne
700000JN Carbazole
500000JN Methylphenanthrene (4 Isomers)
300000JN Cyclopentaphenanthrene
100000JN Phenylnaphthalene
200000JN Benzofluorene (2 Isomers)
«**FOOTNOTES»*«
*A-AVERAGE VALUE *NA-NOT ANALYZED *NAI-INTERFERENCES *J-ESTIMATED VALUE *N-PRESUMPTIVE EVIDENCE OF PRESENCE OF MATERIAL
•K-ACTUAL VALUE IS KNOWN TO BE LESS THAN VALUE GIVEN *L-ACTUAL VALUE IS KNOWN TO BE GREATER THAN VALUE GIVEN
•U-MATERIAL WAS ANALYZED FOR BUT NOT DETECTED. THE NUMBER IS THE MINIMUM QUANTITATION LIMIT.
*R-QC INDICATES THAT DATA UNUSABLE. COMPOUND MAY OR MAY NOT BE PRESENT. RESAMPLING AND REANALYSIS IS NECESSARY FOR VERIFICATION.
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