Bioremediation Treatability Study forRemedial Action at Popile, Inc., Site, ElDorado. Arkansas.

Phase II. Pilot-scale Evaluation

by Lance Hansen, Cathy Nestler, Mike Channell, Dave Ringelberg, Herb Fredricksonand Scott Waisner

U.S. Army Corps of EngineersWaterways Experiment Station3909 Halls Ferry RoadVicksburg,MS39180-6199

For Ted Eilts, Joseph Sensebe, Gary Brouse, and Reuben Mabry

U.S. Army Corp of EngineersNew Orleans DistrictThe Foot of Prytania StreetNew Orleans, LA, 70160

Ju^ m •

Contents

1 Introduction ..............................................................................................10

1 . 1 Site History.................................................................................... 10

1.2 Objectives of Study .......................................................................11

2 Literature Review.....................................................................................12

2.1 Contaminants of Interest...............................................................12

2.1.1 Pentachlorophenol (PCP)...................................................12

2.1.2 Polycyclic Aromatic Hydrocarbons (PAH)........................... 12

2.1.3 Benzo(a)pyrene (BaP) Equivalents ....................................13

2.2 Landfarming ..................................................................................14

3 Experimental Design................................................................................18

3.1 Land Treatment Units (LTD).......................................................... 18

3.1.1 LTU Design......................................................................... 18

3.1.2 Experimental Design...........................................................19

3.2 Metabolic Analysis......................................................................... 20

4 Materials and Methods............................................................................. 21

4.1 LTU Construction ..........................................................................21

4.1.1 Secondary Containment System ........................................21

4.1.2 Primary Containment System and LTUs.............................22

4.2 Sample Collection .........................................................................23

4.2.1 Soil Sample Collection........................................................23

4.2.2 Respiration Analysis ...........................................................24

4.2.3 Cultivation...........................................................................25

4.3 Sample Analysis............................................................................ 25

4.3.1 Physical Analysis................................................................ 25

4.3.2 Leaching and Leachability..................................................26

4.3.3 Chemical Analysis ..............................................................26

4.3.4 Metabolic Analysis.............................................................. 27

in

4.3.5 Data Analysis ..................................................................... 28

5 Results and Discussion............................................................................ 30

5.1 Physical Characteristics of the Popile Soil.................................... 30

5.1.1 Atterberg Limits.................................................................. 30

5.1.2 Particle Size Distribution..................................................... 30

5.1.3 Soil moisture and field moisture capacity........................... 31

5.1.4 Leachability........................................................................ 33

5.2 Chemical Characteristics of the Popile Soil................................... 36

5.2.1 Nutrients and TOC ............................................................. 36

5.2.2 Metals................................................................................. 37

5.2.3 pH....................................................................................... 37

5.2.4 Contaminants..................................................................... 40

5.2.5 BaP Equivalents................................................................. 43

5.3 Metabolic Characteristics of Popile Soil........................................ 45

5.3.1 Biomass.............................................................................. 45

5.3.2 Community Composition ....................................................48

5.3.3 Respiration Gas Analysis ................................................... 52

5.4 Data Analysis................................................................................ 56

5.4.1 Contaminant reduction ....................................................... 56

5.4.2 Degradation Kinetics.......................................................... 58

6 Summary and Conclusions...................................................................... 61

7 Recommendations................................................................................... 62

Appendix A Contaminant Structures ................................................................ 65

Appendix B LTU Data....................................................................................... 71

IV

List of Figures

Figure 1. Design of primary and secondary containment.................................................18

Figure 2. Construction of the secondary containment system ..........................................22

Figure 3. Construction of the primary containment system and LTUs.............................23

Figure 4. LTU random sampling grid...............................................................................24

Figure 5: Conceptual Dry Well Design ............................................................................25

Figure 6. Particle size distribution....................................................................................31

Figure 7. LTU 1. The relationship between soil moisture and field moisture capacity.....32

Figure 8. LTU 2. The relationship between soil moisture and field moisture capacity..... 3 3

Figure 9. SBLT leachability results for LTU 1 .................................................................34

Figure 10. SBLT leachability results for LTU 2...............................................................35

Figure 11. LTU 1. The relationship between soil pH and PCP concentration.................38

Figure 12. LTU 2. The relationship between soil pH and PCP concentration.................39

Figure 13. A comparison of PAH and PCP concentrations in LTU 1 and 2 ...................40

Figure 14. LTU 1. PAH and PCP comparison by compound..........................................41

Figure 15. LTU 2. PAH and PCP comparison by compound.........................................^

Figure 16. LTU 1 and 2. Comparison of total BaP equivalents.......................................43

Figure 17. LTU 1. The BaP equivalent compounds .........................................................44

Figure 18. LTU 2. The BaP equivalent compounds.........................................................44

Figure 19. The coefficients of variation for LTU viable microbial biomass ....................47

Figure 20. Microbial biomass in LTU 1 and LTU 2.........................................................47

Figure 21. Relative abundance of Gram-negative bacteria...............................................49

Figure 22. Relative abundance of Gram-positive bacteria.................................................50

Figure 23. Microbial community composition in both LTUs at Day 168........................51

Figure 24. LTU 1. Respiration.........................................................................................53

Figure 25. LTU1. Water and nutrient addition, and tilling............................................54

Figure 26. LTU 2. Respiration.........................................................................................55

Figure 27. LTU 2. Water and nutrient additions, and tilling ...........................................56

VI

List of Tables

Table 1. The Toxic Equivalency Factors (TEFs) for environmental PAHs...................... 14

Table 2. Sample Analysis Plan .........................................................................................19

Table 3. Atterburg Limits .................................................................................................30

Table 4. Concentrations of the Contaminants in the LTU Leachate.................................33

Table 5. The SPLP Leach Test .........................................................................................35

Table 6. Initial Nutrient Analysis......................................................................................36

Table 7. Metal Concentrations in Popile Soil ...................................................................37

Table 8. Microbial Biomass and Community Composition.............................................46

Table 9. Microbial Biomass and Community Composition in LTU 1 and LTU 2...........48

Table 10. Reduction (%) from Initial Concentrations of PAHs and BaP Equivalents .....57

Table 11. The Degradation Kinetics of PAHs in LTU 1 and 2.........................................59

Table 12. The Degradation Kinetics of BaP Equivalent Compounds in LTU 1 and 2..... 5 9

vn

Preface

The work reported herein was conducted for the US Army Corps of Engineers, New

Orleans. Funding for this project was provided through the New Orleans District, by

U.S. Environmental Protection Agency (EPA), Region 6.

This report is the second in a multi-phase project. The first report, "Land Farming

Bioremediation Treatability Studies for the Popile, Inc., Site, El Dorado, Arkansas",

detailed a study conducted to evaluate contaminant degradation at a micrcosm-scale level.

This report details work conducted to evaluate design information applicable to the full-

scale remediation of the process area soil from the Popile site.

This report was prepared by Mr. Lance Hansen, Environmental Restoration Branch

(ERB), Environmental Laboratory (EL), U.S. Army Engineer Waterways Experiment

Station (WES). Chemical analyses were performed by the Environmental Chemistry

Branch of WES. Physical analyses were performed by the Geotechnical Laboratory,

WES. We gratefully acknowledge the special assistance provided by Mr. Karl Konecny

and the participation of the students of the George Washington University, Science and

Engineering Apprentice Program.

This study was conducted under the direct supervision of Mr. Norman Francingue, Chief,

EED, and under the general supervision of Dr. John Harrison, Director, EL.

At the time of publication of this report, Col. R. Cababa was Acting-Director and

Commander of WES.

Vlll

This report should be cited as follows:

Hansen, Lance D., Nestler C., Chaimell, M., Ringelberg, D., Fredrickson, H., and

Waisner, S., (1999). "Bioremediation Treatability Study for Remedial Action at Popile,

Inc., El Dorado, Arkansas. Phase II. Pilot-scale Evaluation Plan." Technical Report EL-

99-xx, U.S. Army Engineer Waterways Experiment Station, Vicksburg, MS.

1 Introduction

1.1 Site History

The Popile, Inc., site is a former wood-treatment facility located in El Dorado, Arkansas.

The primary contaminants found at the site include pentachlorophenol (PCP) and

creosote compounds associated with wood treatment, including polycyclic aromatic

hydrocarbons (PAHs). Wood treatment operations ceased in July 1982. The site was

purchased by Popile, Inc. In 1984, Popile consolidated three impoundment ponds into

one. This closure activity was administered by the Arkansas Department of Pollution

Control and Ecology. In 1988 and 1989, an Environmental Protection Agency (EPA)

field investigation revealed contaminated soils, sludges and groundwater at the site. EPA

determined that an emergency removal action was necessary. This was conducted from

September 1990 to August 1991. The emergency action consisted of modifying the site

drainage, placing and seeding topsoil, and solidifying and placing sludges into an onsite,

soil-holding cell.

The EPA's design contractor. Camp, Dresser and McKee, Federal Programs, was tasked

with the development of the Remedial Investigation/Feasibility Study for the Popile site.

The remedy that was approved involves the excavation and treatment of approximately

165,000 cubic yards of contaminated soils and sludges in onsite land treatment units

(LTUs). Indigenous microorganisms were expected to break down the target

contaminants to less harmful and less mobile constituents.

Two types of contaminated soils exist on the site. The first is the soil-holding-cell

material, consisting of soils stabilized with rice hulls and fly ash (pH approximately 10)

under previous emergency remedial activities. The second is the process area which

consists of soils that were contaminated by spills, leaks and open air drying during wood

treatment activities. Results of Phase I indicated that it was unlikely that material from

10

the soil cell could not be succesfully treated using landfarming techniques. Therefore, the

Phase II evaluation was conducted on contaminated material only from the process area.

1.2 Objectives of Study

The objectives of the present study were:

1) to determine if the treatment goals specified in the Record of Decision (ROD) are

achievable for the process area soil through land farming technology (these goals are: 5

ppm benzo(a)pyrene (BaP) equivalents and 3 ppm pentachlorophenol (PCP)),

2) to evaluate the contaminant degradation kinetics associated with the landfarming

treatment, and

3) to evaluate the leaching potential of the treated soil.

11

2 Literature Review

2.1 Contaminants of Interest

Pentachlorophenol (PCP)

Because of its potency as a biocide and its persistence in the environment, PCP has been

widely used as an insecticide, fungicide, and disinfectant. It's now a restricted-use

pesticide and although it's no longer available for residential use, PCP is still a common

component of industrial wood preservative for power line poles, railroad ties and fence

posts (Appendix A). PCP is not a particularly volatile chemical. It will undergo

photolysis, especially in surface water. It is relatively hydrophobic and tends to adsorb

onto soil particles, but the strength of the bond depends on the pH of the soil. At lower

pH, it may dissociate into the water, leaching through contaminated soil and entering the

groundwater in that manner. PCP, and several of its breakdown intermediates ( for

example, tetrachloro-p-hydroquinone), are considered possible carcinogens (ATSDR

1994).

Polycyclic Aromatic Hydrocarbons (PAH)

Polycyclic aromatic hydrocarbons are multi-ringed, organic compounds,

characteristically nonpolar, neutral and hydrophobic. They have two or more fused

benzene rings in a linear, stepped or cluster arrangement (Appendix A). PAHs occur

naturally as components of incompletely burned fossil fuels and they are also

manufactured. A few of these are used in medicines, dyes, and pesticides, but most are

found in coal tar, roofing tar, and creosote, a commonly used wood preservative. The

Popile site is contaminated with high concentrations of a wide range of PAHs, including

the recalcitrant, higher molecular weight PAHs. Some lower molecular weight PAHs are

volatile, readily evaporating into the air. Others will undergo photolysis. Because they

12

are hydrophobia and neutral in charge, PAHs are strongly adsorbed onto soil particles,

especially clays. Park et al. (1990) studied the degradation of 14 different PAHs in two

soils. They found air phase transfer (volatilization) an important means of contaminant

reduction only for naphthalene and 1-methylnaphthalene (the 2-ring compounds).

Abiotic mechanisms accounted for up to 20% of the total reduction, but only involved 2-

and 3-ring compounds. Biotic mechanisms handled reduction of PAHs over 3-rings. The

persistence of PAHs in the environment, coupled with their hydrophobicity, gives them a

high potential for bioaccumulation. PAHs are considered to be both mutagenic and

carcinogenic (ATSDR 1995).

Benzo(a)pyrene (BaP) Equivalents

Different PAHs each have different toxic potencies which vary widely. Some PAHs

appear to be non-toxic, while others have been classified as probable or possible

carcinogens. BaP is often used as an indicator for risk assessment of human exposure

because it is highly carcinogenic, persistent in the environment, and is toxicologically

well understood. This level of knowledge doesn't exist for most of the other PAH

compounds.

Because PAHs generally occur in mixtures, toxic equivalency factors (TEFs) were

proposed, similar to those used in the risk assessment of mixtures ofpolychlorinatd

biphenyls (PCBs). The Environmental Protection Agency (EPA) took the first step in

1984 by separating the PAHs into carcinogenic and non-carcinogenic compounds. All of

the PAHs were rated, using BaP as a reference and giving it a value of 1.00. However,

this method led to an over-estimation of exposure risk since the carcinogenicity of the

compounds was unknown. In an attempt to overcome this liability, Nisbet and LaGoy

(1992) developed a new method based on the compounds' response while testing one, or

more, PAHs concurrently with BaP in the same assay system (usually lung or skin cell

carcinoma). BaP was still the reference carcinogen and given the value of 1.00. Sixteen

other PAHs were ranked in comparison to BaP carcinogenicity.

13

This system was tested by Petry et al.(1996) who assessed the health risk ofPAHs to

coke plant workers. There are drawbacks to any system that uses equivalency factors.

The uncertainties in this case arise primarily from dealing with inconsistent mixtures.

Carcinogenic potency could be affected by differences in bioavailability, a competition

for binding sites, co-carcinogenic action, or the effects of metabolism. Nevertheless,

Petry and his co-workers found that the BaP equivalents developed by Nisbet and LaGoy

were valid markers for PAH health risk assessment.

Environmental risk assessment, in a slight contrast to human health risk, looks at the

PAHs that usually occur in contaminated environmental systems and that have the

highest TEFs (by the Nisbet and LaGoy system). This gives us seven PAHs with the

highest environmental risk (Table I): benzo(a)anthracene, chrysene,

benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, indeno(l,2,3-cd)pyrene,

dibenzo(a,h)anthracene. Because BaP was stipulated in the ROD, we used this method to

evaluate the effectiveness of contaminant degradation.

Table 1. The Toxic Equivalency Factors (TEFs) for environmental PAHs

Compound

(abbreviation)

Benzo(a)anthracene (BAANTHR)Chrysene (CHRYSE)Benzo(b)fluoranthene (BBFLANT)Benzo(k)fluoranthene (BKFLANT)Benzo(a)pyrene (BAP)Indeno(l,2,3-c,d)pyrene (I123PYR)Dibenzo(a,h,)anthracene (DBAHANT)

TEF

(by Nisbet and LaGoy, 1992)

0.10.010.10.11.00.11.0

2.2 Landfarming

According to the Federal Remediation Technologies Roundtable (1998), there are several

EPA-accepted processess to remediate the waste from wood treatment sites. These

include thermal desorption and incineration as well as landfarming, or bioremediation.

14

The choice ofremediation technology is based on the concentration of the contamints,

cost, intended use of the land after remediation and other factors. Landfarming

technology remediates contaminated soil in an above-ground system using conventional

soil mangement practices. The contaminant is converted to a less toxic or non-toxic form

either abiotically (ex. photolysis) or biotically, through the metabolism of the indigenous

microbial population (Golueke and Diaz 1989, Harmsen 1991). Landfarming as a form

of applied bioremediation is the cultivation of contaminated soil at properly engineered

sites to stimulate the naturally-ocurring microorganisms to degrade the organic

contaminants. The landfarming operational goal then, is to manage the parameters that

optimize conditions for microbial activity. Typically these include the soil carbon to

nitrogen ratio, soil moisture, pH and oxygen content, temperature and cultivation

frequency. The type of soil being remediated, and the type and concentration of

contaminant, are also factors that shape landfarming management. The rate of

biodegradation can be monitored through the rate of CO; evolution and by chemical

analysis of the hydrocarbons (King 1992, Reisinger 1995).).

With the current "land ban" on hazardous waste disposal and the restrictive regulations

on incineration, landfarming as a way of treating waste has become increasingly attractive

(US EPA 1995). Generally, the degradation process can destroy the organic

contaminants in place without the high cost of excavation and material handling. The

release of volatile contaminants into the air is minimized. The site is monitored on a

continuous basis so the potential for hazardous waste leakage is reduced. The costs

associated with landfarming are generally much lower than ex situ treatment alternatives.

In most instances, the treatment is accepted by the community and the site can be put to

other uses when the treatment is complete (US EPA 1995). This last point has become

increasingly important in the 1990's with the EPA Superfund policy changes towards

"brownfields" development.

When weighing treatment options, however, the disadvantages of landfarming must be

considered. It is land and management intensive. An improperly designed system could

15

lead to adverse environmental effects such as groundwater contamination. Air and odor

emissions may also be hazardous or simply a nuisance. Even dust could be a problem if

the toxic chemical is one that adsorbs to soil particles. Finally, landfarming is not

suitable for all kinds of hazardous wastes (for example, radioactive wastes).

Because landfarming involves a biological system, the limits to this biological system are

also limits to landfarming. The bacteria found most often associated with successful

landfarming are either obligate or facultative aerobes, therefore the soil oxygen content is

an important parameter. The tilling (cultivation) frequency is an important aspect of

maintaining the oxygen level as well as exposing the bacteria to renewed sources of the

contaminant. Most of the microbial communities involved with landfarming are

mesophilic. The pH range that will support their growth is relatively narrow, usually in

the 6.0 to 7.5 range. They prefer a moisture level that is 30-90% of the water-holding

capacity of the soil. Also, most hazardous wastes are nutrient deficient. Some kinds of

wastes are lethal (heavy metals), or inhibitory (in high concentrations) to the microbial

communities. The degradation process should be studied in the laboratory to determine

that it doesn't produce intermediates or end-products that are as harmful as the

contaminants being remediated. However, all of these limitations to landfarming can be

overcome, with the exception of the presence of heavy metals and/or radioisotopes in the

contaminant mixture (Golueke and Diaz 1989, US EPA 1995).

Landfarming of soils contaminated with PAHs and PCP has been studied several times,

but not usually at the concentrations found at the Popile site. The GRACE Daramend™

SITE evaluation report (1996) cites initial concentrations of 352 mg/kg total chlorinated

phenols (TCP) and 1710 mg/kg total PAH reduced in 254 day to 43mg/kg (TCP) and 98

mg/kg (PAH), dark and Michael (1996) used "enhanced" landfarming to achieve

degradation goals in 15 months. McGinnis et al. (1994) studying "aged" PCP, found that

concentrations up to 300 mg/kg weren't inhibitory to the bacteria if soil phosphorus and

oxygen concentration levels were maintained. Hurst et al. (1997) have found microbial

activity in soil containing up to 500 mg/kg PCP. Again, the oxygen concentration in the

16

soil was a significant factor in successful degradation, although anaerobic degradation of

PCP has been reported (Frisbie and Nies, 1997).

Successful bioremediation through landfarming has to meet these three criteria:

(1) there must be a loss of the contaminant over time,

(2) there must be a demonstrated ability of the indigenous microorganisms to degrade the

contaminant over time

(3) there must be evidence that this biodegradation potential is expressed in the field.

3 Experimental Design

3.1 Land Treatment Units (LTU)

LTD Design

The pilot-scale land treatment units (LTUs) were built to simulate the full-scale LTU

design being implemented on-site at Popile. The pilot-study LTU consisted of a bottom

impermeable liner, a sand-bed leachate collection system, and hard standing walls to

withstand impact from cultivation. To provide environmental security for this study, a

secondary containment cell was constructed similar in concept to landfill liner (modified

ASTM D-l 973-91). This secondary system was back-filled with clean sand to provide a

base for the LTUs. Figure 1 illustrates the design of the primary and secondary

containment systems and the leachate collection system. Actual construction is shown in

Figure 3 and Figure 4 in Materials and Methods (Section 4).

Contaminated Soil

Geotextile Membrane

Stee or Wood Wa11s

Clean sand leachate system

Figure 1. Design of primary and secondary containment

18

Experimental Design

The study was designed to evaluate two cultivation management strategies. LTU 1 was

cultivated on an oxygen dependent basis. When the oxygen concentration in the pore

space was reduced to 5%, the lift was to be tilled. LTU 2 was cultivated on a fixed

schedule, every two weeks, independent of the oxygen concentration.

Soil samples were taken every two weeks. The parameters included in the bimonthly soil

analysis were contaminant concentration, nutrient concentration (TKN, TP, TOC), pH

and moisture content. Microbial biomass was evaluated intermittently throughout the

study. At the initial and final sampling events, leachability, particle size distribution

(PSD) and Atterberg limit tests were performed. At the initial sampling only, metal

concentrations and total volatile solids were examined. The analysis schedule is shown

in Table 2.

Table 2. Sample Analysis Plan

DayO

PCP concentrationPAH concentration

Nutrient and TOC concentrationpH

Moisture contentleachability

Microbial biomassPSD

Atterberg limitsmetals

Total volatile solids

Bimonthly

PCP concentrationPAH concentration

Nutrient and TOC concentrationPH

Moisture content

Day 168

PCP concentrationPAH concentration

Nutrient and TOC concentrationpH

Moisture contentleachability

Microbial biomassPSD

Atterberg limits

19

3.2 Metabolic Analysis

Respiration, measured by soil gas analysis, was monitored twice each week to follow

changes in the oxygen and carbon dioxide concentrations.

Microbiol characterization of the indigenous microbiota was conducted to assess the

biomass and community composition in each LTU. This analysis was performed on

contaminated soil directly from the Popile site, soil after it was transferred to the two

LTUs (day 0), and intermittently throughout the study on days 14, 42, 84, 126 and 168.

20

4 Materials and Methods

4.1 LTU Construction

Secondary Containment System

The secondary containment liner of 36 mil Cooley Coolguard®, was purchased from

Colorado Lining, International. The leachate collection system was constructed from 4-

inch perforated PVC pipe covered with a gravel base (mean size 1 inch by seiving). This

was covered with geotextile and '/i-inch thick aluminum sheets, with '/2 inch holes in a

grid pattern 6 inches on center. A backhoe was used to excavate a pit measuring

approximately 3 0 f t x 3 0 f t x 3 f t . I t was divided into two sections using a row of

sandbags. One side of the pit area was used for the LTUs and the other side for the

leachate containers. The 36 mil liner, used for both sides of the pit, was molded into the

comers, over the divider, and extended beyond the edge of the pit (Figure 2).

A leachate collection system was installed in each side of the pit to collect rainwater.

This system, similar for both sides of the pit, consisted of 4-inch perforated PVC pipe that

was connected to a sump. A Vi hp sump pump was installed in each sump to remove the

water from the site. Next, ten inches of washed gravel was placed in each side. A

geotextile was placed on top of the gravel to keep sand from filtering down and plugging

up the leachate collection system. The half of the pit that supports the tanks was filled in

with sand and covered with another layer of geotextile.

21

Figure 2. Construction of the secondary containment system

Primary Containment System and LTUs

The liner for the primary containment was also 36 mil Cooley Coolguard®. Standard Vi

hp sump pumps were used in the leachate collection system. The LTU walls were

constructed from ^ in. thick aluminum sheets. Sandbags were used as structural

supports, separating the two containment areas.

Rainfall at the pilot site was monitored electronically with a Rainwise ® tipping bucket.

In addition, a direct-reading, see-through rain gauge served as back-up.

A stable base for the LTUs was formed in the second half of the pit by filling it about

halfway with sand. Two sheets of aluminum (4 ft x 10 ft) were laid end-to-end for each

LTU (20 ft total length). The aluminum had '/2-inch holes drilled on 6-inch centers to

allow for drainage of water from the LTU. Sandbags were used to form the support walls

for the LTUs. With the walls in place, the aluminum sheets were removed and replaced

~i~i

with more of the 36 mil containment liner. A sump was installed at each end of the LTU

with 4-inch perforated PVC pipe connected to the sump. Gravel was again placed over

the leachate collection system and covered with geotextile. The bottom sheets of

aluminum were replaced in each LTU and pre-formed aluminum walls were positioned

against the sandbags to make the sides. The last step was to fill in the area around the

outside of the LTUs with sand. Each completed LTU was approximately 18-inches deep,

4 feet wide and 20 feet long (Figure 3)

Figure 3. Construction of the primary containment system and LTUs

4.2 Sample Collection

Soil Sample Collection

As shown in Figure 4each LTU was subdivided into 20 sections, each one 2-feet x 2-feet.

These were lettered "A" through "T". A sampling grid was constructed from a 2 x 2 ft

section of plexiglass drilled with 36 equidistant holes for the soil corer. At each sampling

interval, five randomly-located cores were collected from each of the 20 sections. The

23

five soil cores for each single grid were combined in a 950 cc amber jar and manually

homogenized into a single sample. A random number generating computer program

selected seven of these 20 grids for analysis. The remaining 13 samples were archived at

4°C in their original collection jar. The stainless steel corer (3/4 inch x 19 inch) was

purhased from Forestry Suppliers, Inc.

Figure 4. LTU random sampling grid

Respiration Analysis

Drywells, installed in each LTU for respiration analysis, were designed at WES and made

by PSI, Inc., of Jackson, MS. They were constructed from a 6-inch upper ring and cap of

PVC superimposed on a 12-inch vertical dry well made of standard 2-inch slotted PVC

(Error! Reference source not found.). The cap was equipped with a 3-way plastic

stopcock purchased from Cole-Parmer®.

24

Figure 5: Conceptual Dry Well Design

Cultivation

LTU 2, only, was tilled after soil sampling. When necessary, water and/or nutrients were

added to the unit before tilling. The surface of LTU 1 was raked lightly after sampling, to

fill in the sample holes. Cultivation of LTU 2 was accomplished with a rear-tine rotary

cultivator, with a 12 inch cultivation depth.

4.3 Sample Analysis

Physical Analysis

Atterberg limit analysis and particle size distribution (PSD) were used to evaluate the

physical structure of both the untreated and treated soils. The Atterberg limit test was

performed by the Geotechnical Laboratory at the WES-USAERDC (Corps of Engineers

Laboratory Testing Manual, EM-1110-2-1906, Appendix 3, III: Liquid and Plastic

Limits). Particle size distribution was measured on a Coulter LS100Q particle counter

25

according to instrument protocol. Soil moisture was analyzed on a Denver Instrument

IR-100 moisture analyzer and validated by oven- drying atl05°C for 24 hrs.

Leaching and Leachability

Water that leached through the LTUs was contained on site and tested for presence of the

contaminants on Day 14 and again on Day 168. Chemical analysis of the leachate was

performed by the Environmental Chemistry Branch ofWES.

Two different leachability tests were conducted, the sequential batch leaching test

(SBLT) and the synthetic precipitate leaching procedure (SPLP). The SBLT consists of

four repeat extractions of the same sample using distilled-deionized water in a 4:1

(watersoil) ratio. The slurry is mixed for 24 hours, centrifuged, filtered and the water

fraction analysed for the contaminants. The SPLP consists of a single extraction using a

dilute acid solution. The specific acid solution is a function of the geographic area of

interest. For the Popile analysis, the SPLP used a 20:1 (liquid:soil) ratio, pH 4.8.

Maximum extractant concentration for a known solid-phase concentration is controlled

by equilibrium partitioning. This can be determined from the single point analyses in the

SPLP or the SBLT. The SBLT is thought to be more aggresive due to the fact that the

water has no ions in it and is looking to absorb ions and come to equilibrium with the

sample. This information is useful and has regulatory acceptance, however it is

incomplete because it precludes analysis of residual contaminant in the solid matrix

which may be eluted under repeated or changing equilibrium conditions such as observed

in repeat rain events. To comply with necessary regulatory requirements and meet the

information needs of the project sponsor, both leachability tests were conducted with five

sample replicates at Day 14 and Day 168.

26

Chemical Analysis

Contaminant concentrations, metals, nitrogen, phophate and total organic carbon analyses

were performed by the Environmental Chemistry Branch of the Waterways Experiment

Station on both treated and untreated soil. PAH and PCP concentrations were determined

using SW846 EPA Method 8270c for GC/MS after extraction by Method 3540c. Total

organic carbon was measured after drying the soil at 60° C. The dried soil was

homogenized. An acid slurry was prepared by lowering the pH to less than 2 with

phosphoric acid. The slurry was sparged for 15 min. with nitrogen to remove the

inorganic carbon, redried, ground and homogenized. Three samples, each between 40

and 60 mg, were analyzed on a Zeilweger Analytic TOC analyzer, according to

instrument specifications. The nitrogen and phosphate analysis was performed using the

Lachat 8000 Flow Injection Analyzer (FIA). The preparation methods were modified

versions ofEPA-600/4-79-020 (1983 revision), 365.1 and 351.2, respectively. Metals

and total volatile solids were determined according to standard methods (SW 846). Soil

pH was determined for a soil-distilled water slurry (1:1, wt/vol) using a Cole-Farmer®

pH meter.

Metabolic Analysis

Gas analysis in the landfarming units was accomplished using an LMSx Multigas

Analyzer® from Columbus Instruments. Oxygen, carbon dioxide and methane

concentrations in the soil were monitored. The drywells were centered in each LTU grid

section. Following gas sampling, the drywells were lifted from LTU 2, soil samples were

taken, the soil was tilled, and the drywells were re-inserted. The drywells remained in

place in LTU 1.

Microbial biomass was determined at 0, 14, 42, 84, 126 and 168 study days. Two grams

(wet weight) of soil /sample were subjected to an organic solvent extraction to

quantitatively recover bacterial membrane lipid biomarkers (ester-linked phospholipid

fatty acids or PLFA) as outlined in White and Ringelberg (1998).

27

Data Analysis

The chemical analytical data were reduced to develop average sums of the concentrations

of total PAH, individual PAH compounds and total PCP. To calculate the magnitude of

reduction and the rate of degradation of these contaminants, the initial and final

concentration values were used. Zero order (concentration independent) removal rates

were assumed due to the high concentrations of the contaminants (Shane 1994).

The total % PAH and total % PCP reductions were calculated using Equation 1:

% Rcontanunant = [C,nitial] - [CfinJ / [C»,,J X 100 EqU 1

where,

"^contaminant= removal of contaminant, percent of initial

[Cinitiai] = average initial contaminant concentration in the LTU

[Cfinail = average final contaminant concentration in the LTU

The rate of elimination (k) of the contaminants was calculated as a concentration-

dependent, zero-order reaction (k = concentration change / time).

k=- (dC/dt) Equ 2

Equ 3

where,

Ci = concentration at Day 0

28

C; = concentration at Day 168

ti=0

t2=168

The time required to acheive the ROD goals can be calculated by substituting the goal (5

ppm for PAH) for the final concentration^), and solving for "t^"

C^Ci-k^-t,) Equ4

so that,

t2=(C2-Ci)/k-ti Equ5

Because t, = 0, this simplifies to,

t = (C^ - C,)/k Equ 6

The microbiological data was subjected to a Tukey HSD to determine if there was a

significance to the differences between the data for the two LTUs, taking into account

that more than two samples were taken (Ringelberg et aL 1989). The hierarchal cluster

analysis was used because there was no a priori hypothesis being tested. It attempts to

minimize the the sum of squares of any two clusters found at each step of an algorithim.

It was used to try to determine if a significant relationship existed between sets of data for

the two LTUs (Ringelberg et al. 1997).

29

5 Results and Discussion

5.1 Physical Characteristics of the Popile Soil

Atterberg Limits

The Atterberg limits (Table 3), are the values where the moisture content of the soil will

allow the soil to change state from a solid to a semi-solid, to a plastic, and then a liquid.

These limits also establish the soil type (clay, silt, sand etc.). LTU 1 initially had a liquid

limit of 23% and a plastic limit of 17%. The soil type was designated clay/clay-silt. LTU

2 demonstrated a liquid limit of 26%, a plastic limit of 17%, and was classified as a clay

soil.

Table 3. Atterburg Limits

Characteristic

Liquid limitPlastic limit

Plasticity index

Soil type

LTU1DayO

23176

clay/silt

Day 16824195

silt

LTU 2DayO

261710

clay

Day 16823194

silt

Particle Size Distribution

The initial PSD reinforced the results of the initial Atterberg limits (Table 3). Based

on the Corps of Engineers particle size classification, LTU 1 consisted of 68% fines

(clay/silt) and LTU 2 was 76% fines (Figure 6). At Day 168, these values were not

significantly different. Dust is a drawback to landfarming that can be countered by

keeping the soil surface moist or covered, for example with plants. Dust production

results in a loss of fines, the clay/silt fraction, from the land treatment area.

30

Figure 6. Particle size distribution

Although LTU 1 was cultivated only once (for nutrient homogenization), and LTU 2 was

cultivated 17 times throughout the 168 day study, this does not appear to have had a

significant impact on the physical structure of the soil.

Soil moisture and field moisture capacity

The field moisture capacity (FMC), as defined by the USDA - Natural Resources

Conservation Service, is the moisture content of the soil, expressed as a percentage of the

ovendry weight, after the gravitational, or free, water has drained away. More simply,

this is the moisture content 2 to 3 days after a soaking rain. It is also known as the

normal field capacity, the normal moisture capacity or the capillary capacity. The Popile

soil delivered to the pilot facility had a field moisture capacity of 23%. In general,

landfarming as bioremediation requires that the moisture content be maintained between

30 to 90% of the FMC in order to sustain microbial growth. For Popile soil, this

31

correlates to 6.9 to 20.7% moisture. At the initial sampling (Day 0), LTU 1 was at 15%

and LTU 2 was 14% moisture. The SOW denoted maintaining the moisture content

between 50 and 80% ofFMC, translating to a soil moisture content between 11.5% and

18.4% (Figure 7and Figure 8). The FMC was retested at Day 112 (after a soaking rain).

At this time, the LTUs showed an increase in capacity, to 28% for LTU 1 and 30% for

LTU 2 (an increase of 21% and 30% for LTU 1 and 2, respectively). Maintaining 50-

80% FMC, this correlates to a soil moisture content of 14-22% for LTU 1 and 15-24% for

LTU 2. When soil moisture content fell below the 50% FMC minimum, water was added

to bring the moisture content up to the 80% of FMC. Maintaining the soil moisture level

over 50% FMC proved problematic. The high fraction of tightly sorbed hydrophobic

hydrocarbons directly competed with moisture sites in the soil. High temperatures and

winds accelerated the evaporative losses.

75 100

Time (study days)

Figure 7. LTU 1. The relationship between soil moisture and field moisture capacity

32

0 75 100 125 150 175

Time (study days)

Figure 8. LTU 2. The relationship between soil moisture and field moisture capacity

Leachability

The initial LTU leachate results are shown in Table 4. The primary contaminant of

the leachate was PCP.

Table 4. Concentrations of the Contaminants in the LTU Leachate.

Contaminant

PCPphenol

2-methyljphenol4-metlrylJihenol

i NAPHTHdibenzofuran

Concentration (mq/l)Day 14

1973.13

1.82 (estimated)5.3

IJlJestjmated^1.28 (estimated)

Day 16850.3

*

•*•

*

*

*

below the detection limit

33

The results of the SBLT leaching test in LTU 1 at Day 14 and Day 168 are shown in

Figure 9. The SBLT for LTU 1 on Day 168 showed that only 7.9% of the available PCP

was leached from the sample during the test. As time increases, the concentration of PCP

decreases. The SBLT indicates that probably less than 10% of the PCP is in a form

available for microbial degradation. LTU 2 performed ina similar manner as illustrated in

Figure 10. In both LTUs, there was less than 0.5% of the PAHs leached from the

samples.

SBLT LTU1

Figure 9. SBLT leachability results for LTU 1

34

SBLT LTU 2

Figure 10. SBLT leachability results for LTU 2

The results of the SPLP are shown in Table 5. Both LTU 1 and LTU 2 demonstrated a

dramatic decrease in PCP leachability from the beginning to the end of the study. Under

these slightly acidic conditions, less than 5% of the PCP was leached from the soil during

the SPLP. The PAHs were below detection limits

Table 5. The SPLP Leach Test

Compound

PCP

NAPHTH

DayO

34.4±3.0

5.8±0.5

Day 168LTU1

3.63±0.67

0.0

LTU 2

4.7U0.81

0.0

35

5.2 Chemical Characteristics of the Popile Soil

Nutrients and TOO

A typical soil should have total nitrogen values around 1500 ppm and total phosphate

around 400 ppm (Lyon et al., 1952). As expected from the landfarming literature

(Dibble and Bartha 1979,Golueke and Diaz 1989), the nitrogen in the Popile soil is

low (Table 7). The target concentrations for C:N:P of 100:10:1 would correlate to

28000:2800:280 in the Popile soil. This initial nitrogen, then, is an order of

magnitude lower than our optimal targets. Nitrogen, as NN4, was added in aqueous

form to increase the nitrogen concentration in the system. The aqueous addition was

problematic due to the high hydrophobic hydrocarbon concentrations. Solid nitrogen

addition was attempted with some success when it coincided with a natural rain event.

Phosphate was not limiting in this system. Low initial nitrogen, may have been a

limiting nutrient. Following nitrogen (fertilizer) addition there was a burst of growth

and gas production.

Table 7. Initial Nutrient Analysis

Nutrient

TKNNO;-NNC>3-NNHa-N

TPOP04

TOC

Concentration

158.5±18.131.88 *estimated values

17±3.54±1.1

456±8932±10

28,671.5±3244.5

(mg/kg)

36

Metals

As indicated in Table 7, there were no metals present in the Popile soil at

concentrations that would inhibit microbial growth.

Table 7. Metal Concentrations in Popile Soil

Metal

PbNiZnFe

Fe-2Fe-3MgMnAsBaCdCrHgSe

Average Concentration (mg/kg)

LTU1

12.8911.1434.33

10,457.1422.10

10,420.003768.57

45.575.14

682.570 (below measurable limits)

17.640.39

0 (below measurable limits)

LTU2

13.0310.6734.16

10,371.430 (below measurable limits)

10,371.433687.14

45.044.93

673.430 (below measurable limits)

16.570.38

0 (below measurable limits)

pH

Soil pH affects the contaminant chemistry and interactions with the soil particles. The

initial soil pH for both LTUs was 9. This immediately began decreasing (7.4 at Day 84).

However, by Day 168 the pH had returned to 8. Figure 11 and Figure 12 illustrate the

interaction between pH and PCP in LTU 1 and 2, respectively. As outlined by Lee et al.

(1990), at neutral pH PCP can be found as both a phenolate anion and in its neutral form.

Below pH 7, the neutral species adsorbs to the soil with increasing strength as the pH

drops and/or the organic carbon increases. Above pH 7, the ion adsorbs to the soil

particles and also can form complexes with soil metals. With Popile soil, we have a

situation in which the pH is above 7 at the beginning, the organic carbon content is quite

high (Table 6), and there is a high iron content (Table 7). We suggest that the PCP

37

high iron content (Table 7). We suggest that the PCP initially is complexed to the iron

and adsorbed to the organic components of the soil. As the pH decreases, this PCP is

released back into the soil, becoming available for degradation and, thus, appearing to

increase in concentration.

3000

2500

0)

o

2000

1500

1000

500

Figure 11. LTU 1. The relationship between soil pH and PCP concentration

38

Figure 12. LTU 2. The relationship between soil pH and PCP concentration

Contaminants

Figure 13 illustrates the general decrease in the concentration ofPAHs in LTU 1 and 2.

LTU 2 showed a greater reduction in the contaminant. No decrease in PCP concentration

was seen in either LTU.

15000

f 100000)

0 5000U

75 100

Time (days)

Figure 13. A comparison of PAH and PCP concentrations in LTU 1 and 2

40

When the PAH reduction is examined by individual compound (Figure Hand Figure 15,

Appendix A), decreases are evident in both LTUs for naphthalene and 2-

methylnaphthalene (2-ring compounds). Removal of the 2-ring PAHs generally occurs

through a combination of physical (ex. volatilization) and biological processes. LTU 1

also shows a slight decrease in acenaphthalylene, fluoranthene, and phenanthrene (2 and

3-ring compounds). Removal of 3-ring compounds is generally accepted as evidence of

biological degradation of PAH. This is due to the low volatility of these compounds.

0 — — n _ . _ i — — _ __|^B_1_ HBI ^M BM BM HMn IIMH KM I ^ — — — ^^n-i fflfBI I I I ! I 1 1 1 1 1 1 1 I I 1 I

^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ -^ ^ <^ ^

////////////////

PAH/PCP

Figure 14. LTU 1. PAH and PCP comparison by compound

////////////////^PAH/PCP

Figure 15. LTU 2. PAH and PCP comparison by compound

In LTU 2, these decreases in concentration of the 2 and 3-ring compounds are greater and

include anthracene (3-rings). The increase in PCP concentration is more marked in LTU

2, especially between Day 0 and Day 84, the same period in which the pH was

decreasing.

42

BaP Equivalents

When the BaP equivalents are calculated (Figure 16), LTU 2 demonstrated a greater

overall decrease.

0 14 28 42 56 70 84 98 112 126 140 154 168 182

Sample Time (days)

Figure 16. LTU 1 and 2. Comparison of total BaP equivalents

Figure 17 and Figure 18 examine the BaP equivalent PAH compounds in each LTU.

LTU 2 shows a more pronounced decrease in benzo(a)pyrene.

Figure 18. LTU 2. The BaP equivalent compounds.

5.3 Metabolic Characteristics of Popile Soil

Biomass

As shown in Table 9and Figure 19 and Figure 20, viable biomass increased in both LTUs

over time. The greatest increase in LTU 1 occurred between Days 42 and 84 . In LTU 2,

the greatest increase occurred between Days 84 and 126. Biomass estimates at the

endpoint, 168 Days, averaged 4.5xl08 and 5.5xl08 cells/g in LTUs 1 and 2, respectively,

representing a 2 and 4-fold increase over the Day 0 values (Table 8). However, the 2-fold

increase in LTU 1 was found to be insignificant (Tukey HSD, p<0.05) whereas the 4-fold

increase in LTU 2 was significant (Day 84 through 168 versus Day 0). Biomass

differences between LTUs, at common time points, were also insignificant at all time

points except Day 126. At this point, the biomass in LTU 2 was significantly greater than

that in LTU 1. Viable microbial biomass estimates for the original delivered soil and

LTU Day 0 soil were not significantly different.

45

Table 9. Microbial Biomass and Community Composition.

Viable Biomass Community Composition

(cells/g)1 (mole %)Sample ubiquitous Gram-positive Gram-negative Micro-eukaryoteDump-1Dump-3Dump-5Dump-7

Dump-9

avg. (cv)2

TO-L1DTO-L1LTO-L1MTO-L1NTO-L1PTO-L1Savg. (cv)

TO-L2DTO-L2KTO-L2LTO-L2MTO-L2NTO-L2PTO-L2Savg. (cv)

2.1E+088.4E+071.9E+087.6E+07

6.5E+07

1.3E+08(56%)

7.0E+081.0E+087.3E+071.9E+082.4E+081.8E+08

2.5E+08 (93%)

5.5E+071.6E+081.7E+088.1E+073.0E+086.3E+071.1E+08

1.4E+08(63%)

85.8 2.5 10.1 1.658.5 4.5 31.1 5.881.8 4.0 12.4 1.747.0 12.1 37.4 3.6

58.5 4.7 32.2 4.6

66(25%) 6(67%) 25(51%) 3(53%)

53.9 5.9 35.2 5.078.9 2.5 17.6 1 .162.7 3.6 31.4 2.286.5 1.8 10.5 1.290.5 1.6 7.2 0.783.4 2.7 12.8 1.2

76(19) 3(53%) 19(61%) 2(84%)

62.6 5.1 29.8 2.581.7 3.3 13.7 1.388.5 1.7 8.9 0.875.0 2.3 20.5 2.391.4 1.3 6.7 0.653.9 8.4 34.1 3.554.2 8.3 32.8 4.7

72 (22%) 4 (69%) 21 (55%) 2 (66%)

1 assuming 1 pmole PLFA is equivalent to 2.5x104 cells2 coefficient of variation, (cv%)

T6

Sample Interval

Figure 19. The coefficients of variation for LTU viable microbial biomass

LTD Microbial Biomass

25000

20000

15000

10000

5000

T3 TC T9

Sample Interval

Figure 20. Microbial biomass in LTU 1 and LTU 2

Community Composition

No significant differences existed between the major bacterial classifications examined.

An important observation was the magnitude of the coefficients of variation (CV) at the

beginning of the study and the steady decline in these magnitudes over the time course

(Table 10). This result indicates that, although the contaminant distribution may have

been homogeneous at Day 0, microbial community distribution was not. Spatial

heterogeneity in microbial biomass and community composition was apparent in the

original delivered soil and in both LTUs.

Table 10. Microbial Biomass and Community Composition in LTU 1 and LTU 2.

o/monoViable Biomass Community Composition

(pmol PLFA/g) (cells/g)1 (mole %)Sample ubiquitous Gram-positive Gram-negative

TO-L1TO-L2

T3-L1T3-L2

T6-L1T6-L2

T9-L1T9-L2

T12-L1T12-L2

9805 2.5E+08 (93%)2

5401 1.4E+08 (63%)

9416 2.4E+08(50%)9746 2.4E+08(21%)

15189 3.8E+08(22%)13665 3.4E+08(23%)

17275 4.3E+08(24%)19326 4.8E+08(15%)

17925 4.5E+08(26%)21889 5.5E+08(28%)

76 (19%) 3 (53%) 19 (61 %)72 (22%) 4 (69%) 21 (55%)

57 (6%) 3 (27%) 39 (8%)55 (4%) 3 (29%) 41 (5%)

47 (5%) 3 (42%) 50 (6%)50(6%) 4(51%) 46(7%)

50 (4%) 4 (48%) 45 (3%)51 (9%) 3 (40%) 45 (9%)

45 (7%) 4 (25%) 51 (6%)41 (5%) 3 (24%) 55 (4%)

1 assuming 1 pmole PLFA is equivalent to 2.5x104 cells2 coefficient of variation, (cv%)

Over the time of the study, both LTUs showed significant increase in the percentages of

PLFA that are indicative of Gram-negative bacteria (Figure 21). In contrast, PLFA

descriptive of Gram-positive bacteria remained at the Day 0 levels or declined slightly

48

(Figure 22). The Gram-negative increase correlated with the biomass increase in both

LTUs (r=0.777 for LTU 1 and 0.895 for LTU 2). Significant differences between Day 0

and all subsequent time points were measured.

Figure 21. Relative abundance of Gram-negative bacteria

Gram-positive Bacterial Relative Abundance

60.00

50.00

40.00

ss'5E 30.00<

20.00

10.00

0.00 -

TO T3 T6 T9

Sample Interval

T12

Figure 22. Relative abundance of Gram-positive bacteria

The community composition showed signs of divergence from Day 84 onward. The

divergence was first identified by hierarchial cluster analysis. Using the results of this

analysis, five of the seven replicate sub-samples from each LTU were identified which

showed a definable similarity (i.e. all were linked at a euclidean distance of 2.0 or less).

PLFA profiles of the five repicate samples are presented in Figure 23 which shows only

the Day 168 endpoint analysis since the community differences identified at day 84 were

also identified at Day 168 with only the magnitude of the divergence changing (i.e.

increasing). Six PLFA were found to differ significantly between the two LTUs. Within

the ubiquitous PLFA classification, normal saturated 14:0 or myristic acid and 18:0 or

stearic acid were identified. Within the Gram-negative classification, two cyclopropyi

PLFA (cyl7:0 and cyl9:0) and two trans monounsaturated PLFA (16:lw7t and 18:lw7t)

were identified. Since none of the PLFA within the Gram-positive classification differed

significantly between LTUs, it can be assumed that the input of these organisms (Gram-

positive) to the overall functioning of the LTUs is negligible. The Gram-negative input

was, however, found to be highly significant.

50

Microbial Community Composition in LTUs 1&2 at T12

45.00

40.00

35.00

30.00

a?"5 25.00

20.00

15.00

10.00

5.00

0.00

,.0 ,.0 .0 ,.0 ,.0 .,0 A'. ,.0 n0 ,,0 A<- .0• ^\^ -^y\^ ^ <?- <?• <^ <?•

PLFA

Figure 23. Microbial community composition in both LTUs at Day 168

Increased percentages ofmyristic and trans PLFA in LTU 1 are conducive to the

pressence of the Pseudomonas sp. of bacteria. Pseudomonas sp. are consistently isolated

from PAH contaminated sites and a number of species have been demonstrated to have

the capacity to mineralize some of these compounds. The increased percentages of

cyclopropyi PLFA in LTU 2 is also conducive to the presence of Pseudomonas species,

but reflects a physiological response to changing environmental conditions. In fact, both

trans and cyclopropyi PLFA are synthesized by Gram-negative bacteria in response to

changing environmental conditions, and the divergence seen with the analyses described

above likely incorporates this phenomenon as well as any taxonomic differences.

Trans acids have been shown to increase in prevalence inside the bacterial membrane in

response to toxic exposures. Cyclopropyi PLFA have been shown to occur at different

concentrations throughout the bacterial growth phase. Typically, high cyclopropyi PLFA

concentrations are taken as a sign of an old and tired Gram-negative bacterial community.

In order to measure the impact of the environment on the formation of these two PLFA

51

classes (trans and cyclopropyi), the respective concentrations need to be normalized to a

related factor such as the parent compound.

The ratio of 16: Iw'/'(trans) to 16:lw7(c^), product to parent compound, suggests an

increasing bacterial response by the indigenous bacteria to the presence of the xenobiotics

in the soil. The increased response was significant in both LTUs at all time points,

compared to the Day 0 values. Only Day 168 (final) values showed a significant

difference between LTUs. These results are consistent with bioslurry microcosm studies

where PAH concentrations often exceed initial values by 20-30% after a relatively short

period of incubation. An increase in the bioavailability of the toxicant would induce an

increase in the trans/cis ratio.

Cy 17:0 is also derived from the parent monounsaturate 16:lw7c, and statisticaly

significant increases in this ratio were also observed at all time points (with respect to the

Day 0 values). There was, however, no significant difference between the two LTUs at

any of the time points. This is interesting since the total cyclopropyi abundance was

found to be greater in LTU 2. This suggests that differences in taxonomy are also a

contributing factor to the divergence between LTUs. Nevertheless, the increasing

prevalence of cyclopropyi PLFA likely indicates the occurrence of "old age" in at least a

portion of the Gram-negative bacterial population. If the microorganisms in the LTUs

become stimulated (for example, due to tilling), then nutrient pools (if not supplemented)

will become limiting and cell growth will be slowed. Once in the stationary phase of the

growth cycle, bacteria, in particular Gram-negative bacteria, will synthesize cyclopropyi

PLFA.

Respiration Gas Analysis

Figure 24and Figure 26depict the concentrations of oxygen and carbon dioxide in the

soil of LTU 1 and 2, respectively. In both LTUs, the peaks ofCO^ production

correspond to 0^ depletion. Especially evident in LTU 2, the trend during the final

two months of sampling was toward an increase in CO^ production and a decrease in

52

the soil 0; concentration. The effects of water, the addition of nitrogen, and the

effects of tilling on respiration in LTU 1 and LTU 2 are depicted in Figure 25 and

Figure 27, respectively. Cultivation and nitrogen addition both appear to have a

positive effect on the production of carbon dioxide .

21

19

_ iL^^^•r T" \

f17

Figure 24. LTU 1. Respiration

• Rain/Vteter Addition (cn^•Nitrogen Addition (kg)

•Tilled

III i. .

Time (study days)

Figure 25. LTU 1. Water and nutrient addition, and tilling

—ft—Oxygen ••0--Oxygen-Upper —X— Oxygen-Lower

—ft— Carbon Dioxide • • 0 - - Caiton Dioxide-Upper —X— Caribon Dioxide-Lower

10

0 01

ir- -tfN M 3

ilS

•

•

-tHti-(Wat

(Nitre

iTIIIe

S ?

er Addition

ogen Addit

d

-u-: r: s a

(c

do

m

nO.kg)

u>01

Till

CiJ

ne (study days)

-p-^,,8 01

y-

1 llS eo o f-4 u> r- •«-

N rt r» M M <»

1 , ,. -4-

3 & 0» (010 (D

Figure 27. LTU 2. Water and nutrient additions, and tilling

5.4 Data Analysis

Contaminant reduction

When the percent reduction from the initial concentration is calculated, they indicate an

8% greater reduction in overall PAH in LTU 2 than LTU 1 (Table 12). This difference is

even more apparent when the BaP equivalents are calculated. Then it becomes an 11.3%

difference in reduction.

56

Table 12. Reduction (%) from Initial Concentrations ofPAHs and BaP Equivalents

Contaminant

PAH (overall, avg)

NAPHTH (2-ring)

ANTRAC (3-ring)

PHENAN (3-ring)

PYRENE (4-ring)

B-GHI-PY (6-ring)

BaP Equivalents

CHRYSE (4-ring)

BAANTHR (4-ring)

BAP (5-ring)

I-123-PY (6-ring)

% Reduction

LTU1

27.21

95.95

37.12

27.66

19.89

16.32

4.45

19.40

22.63

10.88

17.30

LTU2

35.5

99.17

17.26

29.10

12.37

17.79

15.76

8.31

13.76

17.85

18.86

57

Degradation Kinetics

The degradation kinetics (Table 13 and Table 14) show that, based on zero-order

degradation, at the present rate of decrease, it will take 1.69 years to reduce the overall

PAH burden of the Popile soil to 5 ppm if it's given no treatment (LTU 1). To reach the

goal of 5 ppm BaP equivalents, however, will take 9.86 years. For LTU 2, the average

PAH reduction will require 1.3 years. The BaP goal, however, will only take 2.79 years.

Degradation ofPCP described in Section 5.2.3 (p. 36-38) of this report discusses the

relationship between soil pH and PCP concentration. The PCP concentration in LTU-1

reached a peak after 126 days and then declined throughout the duration of the study (Day

168). In LTU 2, the peak of PCP concentration was attained earlier in the study (at 42

days) and maintained until Day 126, when it began a slow decline. The apparent rise and

fall in PCP concentration in the LTUs appears to be an artifact of soil pH changes. The

time elapsed between the respective PCP peak concentrations and Day 168 was

insufficient to separate artifact from true degradation and attain reliable kinetic data.

58

Table 11. The Degradation Kinetics ofPAHs in LTU 1 and 2

Contaminant

PAH (avg)

NAPHTH (2 ring)

PHENAN (3 ring)

ANTRAC (3 ring)

PYRENE (4 ring)

I-123-PYR (6 ring)

Degradation Kinetics

k (ppm/day)

20.36

12.98

6.28

4.60

1.46

0.03

Time (yr)

1.69

0.48

1.66

1.24

2.31

2.20

xnrm

k (ppm/day)

28.02

12.42

5.95

1.53

0.85

0.03

Time (yr)

1.3

0.46

1.58

2.66

3.70

1.98

59

Table 12. The Degradation Kinetics ofBaP Equivalent Compounds in LTU 1 and 2

Contaminant

BaP EquivalentsCHRYSE (4 ring)

BAANTHR ((4 ring)BAP (5 ring)

B-GHI-PY (6 ring)

Degradation Kinetics

k (ppm/day)

0.0280.370.390.050.02

Time (yr)

9.862.362.013.702.42

k (ppm/day)

0.0990.150.220.070.02

Time (yr)

2.795.363.332.392.01

60

6 Summary and Conclusions

Based on the objectives of treatment goals, kinetics and leaching potential, this study

suggests:

• the ROD treatment goals will not be met using a six-month lift design in a

landfarming system

• the ROD treatment goals for BaP may be met by extending the duration of each lift

treatment. The duration of the study was too short to demonstrate conclusive

biodegradation ofPCP.

• the cultivation associated with landfarming did not increase the leachability of

contaminants in the Popile soil. The leach data supports the groundwater model

showing that the contaminant is not moving from the site under these test conditions.

However, in time some change could occur that would render the conraminant mobile

and it could migrate to the groundwater.

Beyond meeting the stated objectives of the study, the following pertinent observations

were made:

The high concentration ofhydrophobic contaminants inhibited aqueous phase nutrient

additions. Slow-release nutrients applied in a solid form should be a more effective

method of maintaining appropriate C:N:R: ratios.

The increase in microbial biomass and the change in community makeup in LTU 2 by the

end of the study suggest biodegradation of the more recalcitrant PAHs since LTU 2 saw a

greater reduction in benzo(a)pyrene and other 4 and 5-ring PAHs. Cultivation had a

positive impact on the degradation kinetics shown by the greater overall decrease in

contaminant in LTU 2 over LTU 1.

61

7 Recommendations

The Waterways Experiment Station (WES) recommends that New Orleans District

consider continued leveraged funding ofPopile, Phase III, pilot scale activities. The

WES is the center of the Federal Integrated Biotreatment Research Consortium (FIBRC),

a research and development project of the Strategic Environmental Research and

Development Project (SERDP). Remediation of PAH contaminated material is a thrust

of FIBRC. Dr. Hap Pritchard of the Naval Research Laboratory (NRL) is the Thrust Area

Leader. Dr. Pritchard has observed the development of pilot scale landfarming expertise

between the WES and the USACE-New Orleans District. This has resulted in a request

for a collaborative continuation between WES, FIBRC, and USACE-N.O. of the Popile

study.

The FIBRC plan is to innoculate the treated Popile soil with known PAH-degrading

bacteria from NRL. These microorganisms have been isolated and cultured as part of the

SERDP-FIBRC effort. The FIBRC will contribute to the cost of this effort.

The benefit to New Orleans District, EPA and the State of Arkansas, Department of

Environmental Quality is a potential treatment protocol that will meet the ROD goals and

further develop an emerging technology consistent with the objectives of the USACE

Innovative Technology Advocate Initiative.

62

References

Agency for Toxic Substance and Disease Registry (ATSDR). 1994. Toxicological profile forpentachlorophenol (update). Atlanta, GA: U.S. Department of Health and Human Services, Public HealthService.

Agency for Toxic Substances and Disease Registry (ATSDR). 1995. Toxicological profile for polycyclicaromatic hydrocarbons. Atlanta, GA: U.S. Department of Health and Human Services, Public HealthService.

ASTM D-1973-91. Standard Guide for Design of a Liner System for Containment of Wastes.

dark, A.J. and Michael, J. 1996. Regulatory Programs Enhance Use ofBioremediation for ContaminatedEnvironmental Media. J.Soil Contam.5(3):243-261.

Dibble, J.T. and Bartha, R. 1979. Effect of Environmental Parameters on the Biodegradation of OilSludge. AppI.Environ.Micro. 37(4): 729-73 9.

Environmental Protection Agency (EPA). 1984. Health Effects Assessment for Polycyclic AromaticHydrocarbons (PAH). EPA 549/1-86-013. Cincinnati, OH. Environmental Criteria and Assessment Office.

Federal Remediation Technologies Roundtable. Remediation Technologies Screening Matrix andReference Guide. 1998. http://www.frtr.gov/matrix/sectionl/toc.html

Frisbie, A. and Nies, L. 1997. Aerobic and Anaerobic Biodegradation of Aged Pentachlorophenol byIndigenous Microorganisms. Bioremediation Journal 1:65-75.

Golueke, Clarence G. and Diaz, Luis F. 1989. Biological Treatment for Hazardous Wastes. Biocycle: 58-63.

Harmsen, Joop. 1991. Possibilities and Limitations of Landfarming for Cleaning Contaminated Soils InOn-Site Bioreclamation. Processes for Xenobiotic and Hydrocarbon Treatment. R.E. Hinchee and R.F.Olfenbuttel (eds.) pp. 255-272. Battelle Memorial Institute. Butterworth-Heinemann, Stoneham,Massachusetts

Hurst, C.J, Sims, R.C., Sims, J.L., Sorensen, D.L., McLean, J.E. and Huling, S. 1997. Soil Gas OxygenTension and Pentachlorophenol Biodegradation. J.Environ.Eng.4:364-370.

King, B. 1992. Applied Bioremediation-An Overview In Practical Environmental Bioremediation, pp.11-27. Lewis Publishing, Ann Arbor, Michigan

Lee, L.S., Rao, P.S.C., Nkedi-Kizza, P. and Defmo, J.J. 1990. Influence of Solvent and SorbentCharacteristics on Distribution of Pentachlorophenol in Octanol-Water and Soil-Water Systems.Environ.Sci.Technol. 24:654-661.

Lyon, T.L., Buckman, H.O., and Brady, N.C. 1952. The Nature and Properties of Soils. McMillan Inc.,New York.

63

McGinnis, G.D., Borazjani, H., Hannigan, M., Hendrix, F., McFarland, L., Pope, D., Strobel, D. andWagner, J. 1991. J.Haz.Mat. 28:145-158.

McGinnis, G.D., Dupont, R.R., Everhart, K. and St. Laurent, G. 1994. Evaluation and Management ofField Soil Pile Bioventing Systems for the Remediation ofPCP Contaminated Surface Soils.Environ.Technol. 15(8):729-740.

Nisbet, C., and LaGoy, P. 1992. Toxic Equivalency Factors (TEFs) for Polycyclic AromaticHydrocarbons (PAHs). Reg. Toxicol. Pharmacol. 16:290-300.

Park, K.S., Sims, R.C., Dupont, R.R., Doucette, W.J. and Matthews, J.E. 1990. Fate of PAH Compoundsin Two Soil Types: Influence of Volatilization, Abiotic Loss and Biological Activity.Environ.Toxicol.Chem. 9:187-195.

Petry, Thomas, Schmid, Peter, and Schlatter, Christian. 1996. The Use of Toxic Equivalency Factors inAssessing Occupational and Environmental Health Risk Associated With Exposure to Airborne Mixturesof Polycyclic Aromatic Hydrocarbons (PAHs). Chemosphere 32 (4): 639-648.

Reisinger, H.J. 1995. Hydrocarbon Bioremediation-An Overview In Applied Bioremediation ofPetroleum Hydrocarbons. R.E. Hinchee, J.A. Kittel, H.J. Reisinger (eds), pp. 1-9. Battelle Press,Columbus, Ohio.

Ringelberg, D.B., Davis, J.D., Smith, G.A, Pfifmer, S.M.,Nichols, P.D., Nickels, J.S., Hensen, M.J.,Wilson, J.T., Yates, M., Kampbell, D.H., Read, H.W., Stocksdale, T.T. and White, D.C. 1989. Validationof Signature Polar Lipid Fatty Acid Biomarkers for Alkane-Utilizing Bacteria in Soils and SubsurfaceAquifer Materials. FEMS Microbiol. Ecol. 62:39-50.

Ringelberg, D.B., Stair, J.O., Almeida, J., Norby, R.J., O'Neill, E.G., and White, D.C. 1997.Consequences of Rising Atmospheric Carbon Dioxide Levels for the Belowground Microbiota AssociatedWith White Oak. J. Environ. Qual. 26(2): 495-503.

Shane, B. 1994. Principles ofEcotoxicology In Basic Environmental Toxicology. L.G. Cockerham andB. Shane (eds)., p. 11-47. CRC Press, Boca Raton, Florida.

United States Environmental Protection Agency. 1995. Presumptive Remedies for Soils, Sediments, andSludges at Wood Treater Sites. EPA/540/R-95/128.

United States Environmental Protection Agency. 1996. GRACE Bioremediation TechnologiesDaramend™ Bioremediation Technology. Innovative Technology Evaluation Report. EPA/540/R-95/536.

White, D.C. and Ringelberg, D.B. 1998. Signature Lipid Biomarker Analysis In: Techniques InMicrobial Ecology. R.S. Burlage, R.Atlas, D. Stahl, G.Geesey, and G. Sayler, eds. Oxford UniversityPress, Inc. New York. p. 255-272.

64

Appendix A Contaminant Structures

Pentachlorophenol

Name Abbreviation Structure

pentachlorophenol PCP

Polycyclic Aromatic Hydrocarbons

2-Ring Compounds

Name Abbreviation Structure

Napthalene NAPHTH

2-methylnaphthalene 2-MeNAPH

66

3-Ring Compounds

Acenaphthylene ACENAY

Acenaphthene ACENAP

Fluorene

Phenanthrene

FLUORE

PHENAN

Anthracene ANTRAC

4-Ring Compounds

Name Abbreviation Structure

Fluoranthene FLANTHE

Pyrene PYRENE

Chrysene CHRYSE

Benzo(a)anthracene BAANTHR

68

5-Ring Compounds

Name Abbreviation Structure

Benzo(b)fluoranthene BBFLANT

Benzo(k)fluoranthene BKFLANT

Benzo(a)pyrene BAP

Dibenzo(a,h,)anthracene DBAHANT

6-Ring Compounds

Name Abbreviation Structure

Benzo(g,h,i)perylene B-GHI-PY

Indeno(l,2,3-c,d)pyrene I123PYR

70

Appendix B LTU Data

£~PA FILE

AR5oe1

US Army Corps of Engineers

SCAPS Investigation ReportPopile, Inc. Superfund SiteEl Dorado, Arkansas

November 17, 1997

Table Of Contents

1.0 Introduction.......................................................................................................22.0 Site Description..................................................................................................23.0 Investigation Equipment and Procedures.............................................................44.0 Field Investigation..............................................................................................45.0 Results and Discussion ......................................................................................66.0 Conclusion......................................................................................................... 8

Table Of Figures

Figure 1.1 Site Map Showing SCAPS Grid Point Locations........................................3Figure 5.1 View of Soil Classification Cutting Plane at Elevation 177 ft..................... 9Figure 5.2 View of Soil Classification Cutting Planes from the Northeast................. 10Figure 5.3 View of Soil Classification Cutting Planes from the Northwest..._.............. 11Figure 5.4 View of fluorescence intensity at isosurfaces of 400 and 1000 counts from

the ground surface........................................................................................... 12Figure 5.5 View of Fluorescence Intensity at Isosurfaces of 400 and 1000 Counts

from the Northwest........................................................................................... 13Figure 5.6 View of Fluorescence Intensity at Isosurfaces of 400 and 1000 Counts "

from the Northeast...........................................................................................14Figure 5.7 View of Soil Classification Cutting Planes from the Northeast with

fluorescence isosurface at 400 Counts Embedded in It...................................... 15Figure 5.8 LIF Shots on Soil Samples at OG ...........................................................16Figure 5.9 LIF Shots on Soil Samples at OK............................................................ 16Figure 5.10 LIF Shots on Soil Samples at ID .........................................................17

List of Tables

Table 4.1 SCAPS Grid Locations and Elevations.......................................................5Table 5.1 Results of Laboratory Analysis of Soil Samples........................................ 17

SCAPS Investigation Report Popile Superfund SiteNovember 1997 El Dorado, AR

1

1.0 Introduction

The New Orleans District Corps of Engineers (CEMVN) tasked the Tulsa District Corpsof Engineers (CESWT) to perform site characterization activities at the PopileSuperfund Site in El Dorado, AR. El Dorado is located in southeastern Arkansas andthe site is an inactive wood preserving operation that used creosote,pentachlorophenol and petroleum distillates in its processes. A site map is shown inFigure 1.1

The Site Characterization and Analysis Penetrometer System (SCAPS) was deployed atPopile from 9 September through 18 September. Data from a total of 52 subsurfacepenetration events (49 for sensing and 3 for sampling) were collected in this timeperiod. Total footage pushed was 1924 feet and the maximum depth pushed was 70feet.

The investigation activities were generally performed according to the SCAPS FieldSampling Plan for Groundwater Investigation and Modeling, Remedial Action atPopile, Inc. Site, August, 1997 (SCAPS Field Sampling Plan}. The objective of theinvestigation activities was to use the SCAPS rapid site assessment capabilities tocollect additional hydrogeologic and analytical site data to support groundwaterinvestigation and modeling for the site. The data would be used by a Corps TotalEnvironmental Restoration Contract (TERC) contractor in developing a detailedsubsurface stratigraphic map of the aquifer immediately underlying the site. Inaddition the SCAPS data would be used by the contractor to detect and delineate anypotential non-aqueous phase liquid plume(s) within the aquifer.

2.0 Site Description

The Popile Inc. site is an inactive wood preserving operation that used creosote,pentachlorophenol and petroleum distillates in its processes. Past product and wastehandling practices resulted in contamination to surface and subsurface soil,groundwater, surface water and sediments. The site is located on South WestAvenue, approximately */4 mile south of the intersection of South West Avenue andU.S Highway 82 near El Dorado, Union county, AR. The property comprises about 41acres, bordered on the west by South West Avenue, the Ouachita Railroad on the eastand Bayou de Loutre on the north. These three boundaries intersect on the north endof the site. A forested highland area borders the site on the south. The site isapproximately % mile south of the El Dorado city limits. El Dorado has a populationof approximately 25,000. The surrounding area is rural and residential/commercial,although no homes are located along the site perimeter.

A summary of the previous site investigations as well as an assessment of the geologyat the site may be found in Section 1.3 of the SCAPS Field Sampling Plan prepared byNew Orleans District in August 1997.

SCAPS Investigation Report Popile Superfund SiteNovember 1997 El Dorado, AR

2

Figure 1.1 Site Map Showing SCAPS Grid Point Locations

SCAPS Investigation ReportNovember 1997

Popile Superfund SiteEl Dorado, AR

3.0 Investigation Equipment and Procedures

The SCAPS is based on a custom-engineered 20 ton truck capable of hydraulicallypushing an instrumented probe to a maximum depth of 100 feet. The truck housestwo separate, protected work spaces to allow access to contaminated sites withminimal risk to the work crew. One of the work spaces contains the pcnetrometertool, pushpipe, and hydraulic controls for leveling the truck and advancing thepenetrometer tool. The other work space houses optical systems (laser sources andspectrometers), chemical analysis equipment, and the digital data acquisition,processing and display equipment. The focus of this study was to use the SCAPSLaser Induced Fluorescence (LIF) sensor to detect creosote contamination in soils.

The SCAPS LIF probe consists of a nitrogen laser source of pulsed ultraviolet light(337 nm, 1.4mJ at 0.8 ns pulse width, lOHz) located in the SCAPS instrumentationcompartment; a fiber optic link to deliver the laser energy to the soil adjacent to theprobe window; a collection fiber to transmit fluorescence emission signals to thesurface for spectral analysis via a spectrometer/optical multichannel analyzer system;and a microcomputer for data acquisition, analysis display and storage. In additionto the optical sensors, the probe also incorporates geophysical sensors that providecontinuous soil classification and stratigraphy during the penetrometer push. Whenoperated at a 2 cm per second push rate, the LIF probe collects contaminantinformation and soil classification data with a spatial resolution of 4 cm.

4.0 Field Investigation

The SCAPS was deployed at El Dorado from 8 September through 19 September (12days). Nine working days were devoted to site investigation using the SCAPS LIFsensor, one day was devoted to obtaining verification samples and two days weredevoted to mobilization and demobilization. The SCAPS pushed at a total of 53locations. LIF and CPT data were collected at 49 locations and soil samples werecollected from 3 locations. Total footage pushed was 1924 feet and the maximumdepth pushed was 70 feet below ground surface.

During the investigation, the site was visited by two gentlemen from ArkansasDepartment of Pollution Control and Ecology. These were Devon Hobbie and RyanWakeland. Three individuals from EPA Region VI also visited the site. These were JoeKordzi, Glenn Celerier and Bruce Pivet.

Prior to the SCAPS investigation, the sampling locations were laid out on a 100 foottriangular grid. A map of the sample points and their locations is shown in Figure1.1. A table showing the grid point designation and location, the surface elevationand the depth pushed is shown in Table 4.1.

The LIF probe was operated with the soil classification sensors to collect subsurfacestratigraphy data in accordance with procedures described in ASTM Method D3441.Normal operating procedures include calibration of both the soil classification and LIFsensors. The soil classification sensors consist of strain gauges mounted in the conepenetrometer (CPT) tip and sleeve. These gauges are calibrated at the beginning of

SCAPS Investigation Report Popile Superfund SiteNovember 1997 El Dorado, AR

4

Table 4.1 8CAPS Grid Locations and Elevations

ShofthflndDQBiQMtion

1AOA1BOB•2B2C1Coc••1C.2C2DID00-ID-203E2EIEOE-IE2FIFOF4G~3G2G1GOG5H4H3H2H1HOH5141015JUOJ5KOK5L1L5M2M5N4N3N

GridpointCoorcRrote

1-»OO.A0+OO.A1+OO.B0+OO.B-2+OO.B2+OO.C1+OO.C0+00,C-1+OO.C-2*OO.C2-»OO.D1-*OO.D(W».D•1+OO.D-2*OO.D3+OO.E2+OO.E1+OO.E0*00,E-1+OO.E2*00,F1+OO.F0+OO.F4+OO.G3+OO.G2+OO.G1+OO.G0+OO.G5*00,H4+OO.H3+OO.H2+OO.H1+OO.H0*00,H&»00,14*00,1&»00.1&HXI.J1*00,J0+OO.J5+OO.K0+OO.K5*00,L1+OO.L5+OO.M2+00,M5+OO.N4+OO.N3+OO.N

SurfaceEtevtion

(tart)1K18518518818518618618718418518718718818718718B186188190189191193192196194194196191206200197198199195208205192211197192212193210198210200202201201

Offcetrelative to

take location20ftE

50HW

30RE

30HNW60ftNW

40ftW20ftE

30ftE

25BNE

20HNW

NofthinQ

cfa-)1501185150119015010651501095150110515009651500990150099515010001501010150069015006951500900150090515009101500785150079015007951500600150081015006951500700150070515005851500590150059515006001500610150048015004801500495150050015005251500550150038515003901500415150029015003151500320150019015002201500095150012015000001500020149992014999101499925

Eating

,M1106300110639511062901106455110669011062901106405110652011066351106750110635011064701106580110670011068151106330110641511065301106645110676011064801106590110671011063101106425110654011088801106770110626011063701106490110660511067001106790110632011064351106900110638511068451106950110644511069651106530110697011066001106920110665511067501106851

Depth ofPwh(tart)

3128165436342558595941363962651842761343527273939433443192

31373470393029353837403745374132453435

Elevation atBottom ofPuahNGVD (feet)

154157169132147152161129125126146151149125122171165161129155156166166157155151162146187198166161165125170175163176159155172156165161169166157167166

1———3+OO.F 192 1500690

•^—^SSSSEL—

1106360

37.2

Power failure prevented data [acquisition.

156.9 1

SCAPS Investigation ReportNovember 1997

Popile Superfund SiteEl Dorado, AR

each site investigation and checked periodically during normal operations. The LIFsensor is calibrated using an aqueous solution of Rhodamine before and after eachpenetration event to monitor LIF system response and document any system drift.

After each penetration was completed, the push rods were decontaminated with theonboard hot water pressure washer, and the open penetration holes were eithergrouted through the probe tip during sensor retraction or tremie pipe.

CPT and LIF sensor responses were displayed in real-time during each penetration.These data allowed the operator to observe the soil classification and fluorescenceresponse as the probe advanced into the soil. At the end of each penetration, thesensor data were then plotted as a function of depth and archived. Plots for allpenetrations performed at Popile are found in Appendix A. A zip disk of the data filesfor these pushes was provided to CEMVN on 20 October 1997. The sensor data wereprocessed at Waterways Experiment Station to produce three-dimensional graphicalrepresentations of subsurface stratigraphy and contaminant distribution. These arediscussed in detail in Section 5 of this report.

Standard operating procedures for the SCAPS LIF sensor include verification of thefluorescence response for some of the data collected at the site. Verification isaccomplished by collecting soil samples and conducting traditional laboratoryanalyses for semi-volatile organic compounds (SVOCs) and total petroleumhydrocarbons (TPH). Soil samples were obtained with a direct push soil sampler(Mostap™) advanced to the desired sampling depth using the SCAPS truck. Soilsamples were obtained at depths that had previously exhibited high fluorescenceintensity immediately adjacent to sensor penetrations (approximately 1.5 feethorizontally offset).

Verification samples were homogenized in the field by mixing with a stainless steelspatula in a stainless steel pan. Samples were placed in precleaned 250- or 500-mlglass jars equipped with Teflon-lined caps and stored at 4°C until analyzed. TheSCAPS LIF response was obtained for each homogenized soil sample by pressing thesoil against the sapphire window of the SCAPS sensor probe and collecting tenreplicated emission spectra. This procedure was carried twice for each soil sampleobtained. In addition soil analyses for SVOCs (EPA Method 8270) and TPH as diesel(EPA Method 801.5) were performed at an analytical laboratory. These analyticalresults and their comparison to LIF output are presented in Section 5.

The SCAPS investigation resulted in the generation of six drums of decontaminationwater. The drums were labeled, placed on pallets, covered with a plastic tarp and leftat the site for future disposal.

5.0 Results and Discussion

The soil classification data obtained from the cone penetrometer indicates that the sitegenerally consists of layers of sands and gravel and gravelly sands and clayey sands.Figures 5.1, 5.2 and 5.3 show horizontal and vertical profiles across the site. Thesefigures also indicate a large pocket of clay at the north end of the site from the ground

SCAPS Investigation Report Popile Superfund SiteNovember 1997 El Dorado, AR

6

surface to about seven feet below ground surface. There also appears to be a nearsurface silty clay layer just north of the two holding cells (along the G and Hgridlines). This may be a result of the earth moving that took place when the cellswere created. The blue coloring at the tops of the probes in Figure 5.2 indicate thatmany of the penetrations encountered a thin clay layer near the surface.

The SCAPS Field Sampling Plan indicates that, based on a RemedialInvestigation/Feasibility Study performed in 1992, there is a silty clay layer, believedto be continuous, whose top is between 38 and 57 feet below ground surface. Figures4 and 5 of the SCAPS Field Sampling Plan show the elevation of the top of this layer ataround an elevation of 150 feet. Several pushes made by the SCAPS reached depthsbelow elevation 150 feet (OB, OC, -1C, -2C, 2D, OD, -ID, -2D, OE, OG, AND OH), butthe CPT did not indicate any notable change to silty clay or clay either in the raw dataor in the figures.

Figures 5.4, 5.5 and 5.6 present spatial visualizations of the fluorescence intensitymeasured at the site. The isosuriaces shown are 400 counts and 1000 counts. Asshown in Figure 5.4 the SCAPS encountered two distinct plumes north of the debrisholding cells. Grid line E appears to mark the separation between the plumes. Thereare other smaller plumes as shown on Figure 5.4, one located southeast of theholding cells that shows intensity counts over 1000.

Figure 5.7 shows the isosurface of 1000 counts fluorescence intensity superimposedon the soil stratigraphy data visualization.

No effort has been made to correlate peak fluorescence intensity nor the wavelengthsat which it occurs to actual contaminant type or contaminant level. However, prior todemobilization from the site, the SCAPS did take several soil samples to analyze thetypes of contaminants that existed where high fluorescence intensity had beenencountered. Six samples were taken at various depths at grid points OG, OK and ID.The samples were shipped to Pace Analytical Services, Inc. in St. Rose Louisianawhere they were analyzed for SVOCs using method SW8270 and TPH as diesel usingmethod SW8015. The chains of custody and data for these analyses are included inAppendix B, and Table 5.1 summarizes the data in a single table.

As shown on Table 5.1 grid point OG was sampled at a depth of 9 feet and showselevated levels of every SVOC analyzed. The peak fluorescence intensity of thissample was measured twice and was between 1000 and 1200 counts (Figure 5.8).The peak intensity during the actual push at this location was greater than 2000counts.

Grid point OG was also sampled at a depth of 2 feet where the peak SCAPSfluorescence intensity during the push was around 400. Figure 5.8 shows thesample's peak fluorescence intensity to be between 100 and 300 counts. No SVOCsor diesel was detected during analysis.

Grid point OK was sampled at depths of 5 feet and 9 feet with the objective ofquantifying the large intensity peaks seen during the push. This corresponds to thearea of high intensity shown on Figure 5.4 south of the holding cells. Sampleanalysis failed to confirm the presence of SVOCs there, but did detect TPH at 362

SCAPS Investigation Report Popile Superfund SiteNovember 1997 El Dorado, AR

7

ppm and 2,670 ppm at depths of 5 and 9 feet respectively. The peak fluorescenceintensities of the samples, all less than 600 counts, were significantly lower than thepeak of 4000 counts seen during the push. See Figure 5.9.

Grid point ID was sampled at depths of 6 andl6 feet. The ID-6 analysis was done toquantify contaminants corresponding to a peak of 1800 counts of fluorescenceintensity encountered during the push. The only SVOC hit at this sample was 2-methylnaphthalene at 3,510 ppm. The concentration ofTPH in this sample was2,790 ppm. The peak fluorescence intensity of the sample is shown in Figure 5.10and was measured between 1100 and 2100 counts.

The ID-16 sample was taken at a location where the push indicated an intensitycount of around 100. This sample successfully confirmed that there is no SVOC ordiesel contamination when the count is at this level, and its peak intensity countswere below 200.

6.0 Conclusion

The SCAPS investigation at the Popile Superfund Site met the objective of collectingadditional hydrogeologic and analytical site data. The SCAPS pushed an average of37 feet deep to an average elevation of 157 feet which penetrated well into the aquifermaterial. CPT data obtained for 49 holes provide an insight into the aquifercharacteristics and will be used by the TERC contractor for groundwater modeling.The graphical visualizations provided in this report will enhance the conceptual modelfor the site. Additional visualizations may be obtained through Ricky Goodson atWaterways Experiment Station at 601-634-2469.

The LIF data provided an indication of where the contamination plumes are likely toexist as well as their relative magnitude. Verification samples confirmed at least onelocation of SVOC contamination and three locations ofTPH. Correlation of theintensity counts to contaminant level was beyond the scope of this report, however thedata provided on the zip disk may enable this as part of the modeling effort.

Critical project requirements of rapid execution, minimal aquifer disturbance andwaste minimization were fully met using direct push technology provided by theSCAPS. Time and cost savings using this method over conventional drilling have notbeen quantified but are significant.

SCAPS Investigation Report Popile Superfund SiteNovember 1997 El Dorado, AR

8

Figure 5.1 View of Soil Claulflcation Cutting Plane at Elevation 177 ft.

SCAPS Investigation Report Poplle Superftmd SiteNovember 1997 El Dorado, AR

9

Figure 5.2 View of Soil Cl&uiflcation Cutting Pl&nec from the Northe»«t.

x-plane: Bl 106632y-plane: N1500659z-pl&ne: elevation 177.4 ft

SCAPS Investigation Report Popile Superfund SiteNovember 1997 El Dorado, AR

10

Figure 5.3 View of Soil Classification Cutting Plane* from the Northwest.

x-pl&ne: El 106632

y-plane: N1500559

SCAPS Investigation Report Poplle Superfund SiteNovember 1997 El Dorado, AR

11

aoooo1000 00

\ ,, \

/ / ^^ /

,/\

\ \„/.

/' // •'/••

Figure 5.4 View of fluorescence intenxity at i»o«urface» of 400 and 1000 counfrom the ground surface.

Figure 5.5 View of Fluorescence Intensity at Isosurfaces of 400 and 1000Counts from the Northwest.

SCAPS Investigation ReportNovember 1997

Popile Superfund SiteEl Dorado, AR

13

Figure 5.6 View of Fluorescence Intensity at Isosurfaces of 400 and 1000Counts from the Northeast.

SCAPS Investigation ReportNovember 1997

Popile Superfund SiteEl Dorado, AR

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Figure 5.7 View of Soil Classification Cutting Planes from the Northeast withfluorescence isosurface at 400 Counts Embedded in It.

x-plane: El 106632y-plane: N1500559

SCAPS Investigation Report Popile Super-fund SiteNovember 1997 El Dorado, AR

15

Figure 5.8 LIP Shots on Soil Samples at OG

750

500

450 500 550 600 050 700 750

Wavelength

Figure 5.9 LIF Shots on Soil Samples at OK.

SCAPS Investigation ReportNovember 1997

Popile Superfund SiteEl Dorado, AR

16

500 550 600

Wiveleaftb

Figure 5.10 LIF Shots on Soil Samples at ID

Table 5.1 Results of Laboratory Analysis of Soil Samples

Grid Point Location OG-2 OG-9 OK-5 OK-9 ID-6Compound (ug/Kg)Acenaphthene <386 <393 <1960 <2050Anthracene <386 <393 <1960 <2050Benzo(a)anthracene <386 <393 <1960 <2050

<386 <393 <1960 <2050Benzo(k)fluoranthene <386 <393 <1960 <2050Benzo (a) pyrene <386 <393 <1960 <2050Chiysene <386 <393 <1960 <2050Dibenzofuran <386 <393 <1960 <2050Fluoranthene <386 <393 <1960 <2050

2 - Methylnaphthalene <386 <393 <1960Naphthalene <386 <393 <1960 <2050Phenanthrene <386 <393 <1960 <2050Pyrene <386 <393 <1960 <2050

nig/Kg

TPH-Diesel Range <11.6

SCAPS Investigation ReportNovember 1997

Popile Superfund SiteEl Dorado, AR

17

APPENDIX A

SCAPS LIF PLOTS

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

in in01 01c. c.3 3

0)>10

13

Cone ResistanceQc (tons/ft2)

1 10010 | l00<

Sleeve Friction

f, (tons/ft')

X x•rt -rt2 3:

in in in in-»-' >• •u •o 'o 'o10 ID '-1 c. c. c01 •-' •" ID 10 IDa u en ui 01 u)

0 1 2 3 4 5i.-i.-i.-i..

Fluartscence IntensityHor» Countt - Mei BKGMD

0 500 1000 1SOO 2000

X:4Ja0)a

Fluorescence Intensity

Nor*. Counts - No WSMa

100 1000010 i 1000

• •", • "A '. —. • •••350

Wavelength

at Peak (nm)

400 450 500 550-I.. •I

CPT: OASTATE COORDINATES:

EASTING ( f t . )

0

Project: Popile

NORTHING ( f t . )

0

ELEVATION

0

( f t . )

CPT based SOILCLASSIFICATION

Cone Resistance

QC (tons/ft21

1 10010

-i-ffl

Sleeve Friction

f, (tons/ft')

0 Z 4 6 B 10

••-i •i-i tOs z

in in in in4-1 >• 4-1 •O T3 'O10 10 «-< C C C01 1-1 •i-i 10 ID 10a u <n in 01 in

0 1 2 3 4 5

Fluorescence IntensityNor« Counts - No BKGMO0 500 1000 1500 2000

Fluorescence IntensityNorn. Counf - No BKGNO

10 | 1000• I " , ' '"I ! •". • •!•

330

Wavelength

at Peak (nin)400 450

^L500

.L

Project: PopileSTATE COORDINATES:

EASTING ( f t . )0

NORTHING ( f t . )0

ELEVATION0

( f t . )

CPT based SOILCLASSIFICATION

U)1—1

in rn n*

CPT based SOILCLASSIFICATION

in«—i

CPT based SGII).CLASSIFICATION

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

r

CPT based SOILCLASSIFICATION

in in01 0)L L3 3

Cone Resistance

Qc (tons/ft')

1 10010 | 100

i JWl Z '•• Z JU

z zSleeve Frictionf, (tons/ft*)

2 4 6 8 10

in in in in4-1 >• •u 'o 'o '0m n) •-i c c cQJ 1—1 .f-« (0 (0 IDQ. u 01 in (n in

0 1 2 3 4 5

Fluorescence IntensityMor« Counf - tuto BKGM)

Mavelengtnat Peek (nm)

350 400 <50 500 550

Project: PopileSTATE COORDINATES:

EASTING ( f t . )

0

NORTHING ( f t . )0

ELEVATION ( f t . )0

rCPT based SOILCLASSIFICATION

Cone ResistanceQc (tons/ft')1 100

10 |HWUM

m in0) 0)t- L3 3JJ JJx x

•»-* •»-<z z

ca

Sleeve Friction

f, (tons/ft')} 5 4 6 8 10

in cn in in4-1 >• -i-i •o •o •o10 <o •-« c c ca) •-< "< 10 ID 10a. u en in 01 w

0 1 2 3 4 5..'••••I-

Fluoreactnce Int«nsityNoi-r. Counts - No BKGMO

0 500 1000 1500 2000

Fluoriscenc* IntensityNorii. Counts - No BK6NO

HBvelengtnat Peak (nm)400 450 500 550

• ' • • • • ' • • • • I 0

PopileSTATE COORDINATES:

EASTING ( f t . )

0

NORTHING ( f t . )

0

ELEVATION

0

( f t . )

CPT based SOILCLASSIFICATION

tft

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

<n in0) 01C. L3 3

Cone ResistanceQc (tons/ft2I

1 10010 | 1000

JEM f tl

Sleeve Friction

f, (tons/ft ')

) 5 10 15 SO 25• 1 . . . 1 . . . 1 .

••-> ••-> t3Z Z

in in in in4J >• .U •D T3 1310 10 rt C C C0) —" "< 10 ro IDo. u w w m in

0 1 3 3 4 5..I....!

Fluorescence IntensityNOPK. Count! - No BKGNO

0 SOO 1000 1500 SOW

Fluor»sc»nc« lnt«n»tt»Horn Count! - No BKGNO

1 100 10000

Wavelengthat Peak (nm)

350 JOO 450 SOO 550

-1—4-0

CPT: 3 E Project: Popile

CPT based SOILCLASSIFICATION

01 U101 01I- t-3 3

Cone Resistance

q<; (tons/ft2)

1 10010 I 1000

"•'I'

us

Project: Popile

Wavelengthat Peak (nml<00 ••SO 500 550^L

<

STATE COORDINATES:

EASTING ( f t . )

0

NORTHING ( f t . ) ELEVATION ( f t . )

0 0

CPT based SOILCLASSIFICATION

Cone Resistance

He (tons/ft '1)

1 10010 J1 4t»j ; tn|

in in 01w w >L L ID

JJ JJ 0X X

-1-1 -i-i iff•K. Z

w m in inJ-l >. 4J •O •O •O10 TO «-i c c cQ) 1—1 -i-* n> *o *oo. t-> in in in v)

0 1 2 3 4 5

luorBSCBHc* IntensitNarr. Counts - No BKGNC

1 100 lot10 | 1000

• •••> • •••I • •", • •••

I • 1 1 • ••

y1

-0 ^

•

Wavelength

at Peak (nm)

50 Wa 450 500 55

r^

i

1 " ' " | |'

CPT based SOILCLASSIFICATION

one Resistanc^ ( tons/f t 2

1 10010 | 10

; JIM 1 <M ; «M

1

' ' "| ' ' "| ' ' "

e

00 0

-

•

Sleeve Friction

f, ( tons / f t ' )

2 4 6 B 1

\

\

" ' ' ' '

0

•

-

•

in in a)0) 0) >L. C- 103 3 C-4-14-1 0X X. .„ iaz z

in in in in4-1 >• 4-1 •O •O •OID ID 1-1 C C CQJ •—* -^ ID fD 10o. u vi tf) (n v)

0 1 2 3 4 E

^

""'""""""""""""

Fft

5 o

• •

• -

• •

uorescence Intensit>Jorc. Count • • No eKCNO

500 1000 1SOO 20

t

' ' '

Fluorescence IntensityNor'iw. Counts - No BKGNO

Have lengthat Peak (nm|

350 400 450 500 550

CPT based SOILCLASSIFICATION

m m ai0) 0) >c- c. <o3 3 C.4-1 -H 0

Cone Resistance .2 .2 caq^ (tons/^1

0-

•

•U0)0)»»-

"' 5-i-•Ua.«"Q

10-

10010 1 10

; <«« 2 JUJ i <W

1

' " •1 • " 1 ' " '

)

z z(n in in in

00 0

• •

- -

• •

• •

Sleeve Friction

f, ( tons/ft ' )Z 4 6 8 1

\

\

1 1 1 1

0

U >. •t-1 •O •0 010 10 "-< C C Ca) <-i —I (o n} IDa u (n (n in in

0 1 3 3 4 S

?S

f1

'""""'" " "••••""

FNc

5 c

luortsccnce Intent itDrill. ClHints - Auto BKEN

D 500 1000 1500 201. . . > . . . i . . . i . . .

. i i

F

y Nc0

00

luorescence Infnsitarm. Count! - «uto WW

100 1010 I 1000

• •••• • •"I • •••I • •"

1 ( 1

ya

000 y

Havelengtn

at PeaK (nm)

50 400 450 500 S

l • i l

50

-0

'4JUW^

-5 '"c.4-1Q.0)0

- 10

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

in in ww w >C. C. 103 3 t-•i-i-i-i 0

Cone Resistance -S .S iaq, (tons/ft2) m u, 3: 2 a, m

'w 0-0) :»*-

JC :

S 1 0 -o a

1 10010 | 10

; JM| ? «B(j i JM

7-. , . . , . . . . , . , , .

I00 I: :

: :

'

Sleeve Friction

f. (tons/ft')

5 10 15 SO 2...i...i...i...i...

)

" i • • • i • i ' • "

5

4J >. 4J •O T3 •O10 10 •-i C C CQ) r-1 .r1 ID ID 10

a u w in in (/)0 1 2 3 4 E

....!....1....1....1....1....

""'""'"""""""'"""

F

5 c

luorescenct Intensit•Urm Count! - N0 gKGNO

500 1000 )»0 SO,.^,,,,,,

i i i

F

y

00

luortsctnct IntensitNOPr Counts - -1 BKGNO

100 10010 1 1000

""" ^ "

l i l

y

v"> 35

Mavelengtn

at Peak (nm)

50 JOO 450 500 5!

1 1 1

50 —

- 0 1u0)^-

: c

1 - 1 0 g

CPT: 2.£ Project: Popile

CPT based SOILCLASSIFICATION

C

q

l

0-

4JOJ0)

*fc-

^ 5-c•Ua

a

1 0 -

one Besistanc

c (tons/ft')

100

10 | 10; •W Z JMI Z <M

?1

' •"| • "•| ' •"

e

00 0

• •

- -

• •

Sleeve Friction

f, (tons/ft')

5 4 6 8 1

)

•"l"'l"'l"'l' "

0

-

m m ID0) 0) >L. I. 103 3 C-J-> JJ 0x x•ii ••- usz z

in in OT in•u >. *J •o 'o •oID 10 •-• C C CQ) 1-1 -n 10 10 IDQ. u in in in in

0 1 2 3 4 5

(

I

..... 1 ,.,

F

' 0

'

\

uoresctnce Inttnsitnor". Counts - No WWO

500 1000 1300 ZOt

\

' ' '

luorescence IntensitNw. Counts - Ho BKGNC

1 100 lOt10 l 1000

! '", • •••1 • "!, ! •••

}

• 1 1

y

000 „

Wavelength

at Peak (nm)

50 400 450 500 S

l l l

50

-0

<->0)01

M-

-5 "

C4-1Q.

5

- 10

CPT based SOILCLASSIFICATION

Cone Resistance

Qc (tons/ft2)

1 1001000

vi ui0) 01C- 1.3 3JJ 4-1X X

•»•» ••-*

z zSleeve Friction

f, (tons/ft1)

* 6 B 10

W I

in 01 in u)4J >. *> T3 •0 •O10 10 rt C C C0) rt rt 10 10 10o. u in (n ui in

0 1 2 3 4 5

FluorescBncB IntensityHarm. Counti - No DKGMO

) 100 1000010 l 1000

! !!!l ! ;;« i ,!;l i !!;

Wavelength

at Peak Inin)

3SO 400 <50 500 550

CPT based SOILCLASSIFICATION

»

CPT based SOILCLASSIFICATION

m

CPT based SOILCLASSIFICATION

ffl

CPT based SOILCLASSIFICATION

Cone Resistance1.2 '

Sleeve Friction

f, (tons/ft')

0 5 10 15 50 25

m m 01as as >t- t- ID3 3 L.

J-> •k> 0x x. .rt la3E Z

in in in in•u >. *> •o •o •oID ID rt C C CID 1—1 •1^ (0 ID f0a u ui (n ui ui

0 ) 3 3 4 5

Fluorescence IntensityNorn. Count! - No BKGND

0 500 )000 ISOO 3000

Fluorescence IntensityNor». Counts - No BKGNO

Wavelengthat Peak (nuil

10 '" 1000 "T" 350 <00 00 500 550

CPT: 2F Project: Popile

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

in

Cone Resistance

Qc (tons/ft")

1 10010

i 4M i• • "I •

Sleeve Friction

f, (tons/ft')

3 5 10 15 20 £5• ' • • • ' • • • ' • • • I -

in inV 0)c. c-

0)>ID

13

tS

3 3J-> 4Jx x•*1 •l-l

3: SU) in in in4-' >« •" •o 'O •O10 10 <-» C C C(I) •— •— 10 10 10a u in (n (n (n

0 1 2 3 4 5

Fluofscinct IntensityMorn. Counts - No BKGMD0 500 1000 1500 2000

Fluorescence Intensitynorm. Counts - No BK6K1I KM 10000

10 i 1000! !!!l ! ;;n ! t!;l ! i

Wavelengtnat Peak (nm)

350 400 450 500 550

CPT: OF Project: Popile

CPT based SOILCLASSIFICATION

Cone ResistanceQc (tons/ft2)

1 1001000

Sleeve Friction

f, (tons/ft'14 6 8 10

in ui0) 0)t- c.3 3

4-1 4-1X X

in in m m•U >. •U •O n Q10 (0 «-f C C Cd) ^ ,1 (0 t0 10Q- (-> w in in v»

0 1 2 3 4 5

Fluorescence IntensityHorn Caunf - No BKGNO

Q.0)a

Wavelengthat Peak (rim)400 450 500 550

CPT: OFSTATE COORDINATES:

EASTING ( f t . )

0

Project: Popile

NORTHING ( f t . )

0

ELEVATION

0

( f t . )

CPT based SOILCLASSIFICATION

Cone Resistance

Qc (tons/ft2)

1 10010 | 1000

Sleeve Friction

», (tons/ft ')

0 5 10 15 20 25

in in 010) 0) >C- (- 103 3 LJJ JJ 0

X X•i-i •ii tS3: X

m m m m•'-' >• •u •o •o •oID 10 «-< c -c cM •-'••-' 10 10 10Q. (-> in oi oi (/)

0 1 2 3 4 5

Fluorescence IntensityNOT-. CBuntS - NO BKCNO

0 500 1000 1500 2000

Fluorescence IntensityNorr. CountI - No BKGNO

1 100 100001000 3S<110 | 1000

• •H. 1 •••I • ; • • • • •

Have lengthat Peak (nm)400 450 500 550

-i—4-O

•i""i""r

CPT: 46 Project: Popile

CPT based SOILCLASSIFICATION

m

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

Cone Resistance

qc (tons/ft2)

1 10010

Sleeve Friction

f, (tons/ft')

•) 5 10 15 SO 35

in in01 <uL c-3 a•i-i -i-iX X

0)>ID

t3

t3•X. Z

m m m m•K >« 4-1 •o 'O •o10 10 -< c c cQJ r-* •r^ (Q (0 10a u in w (D in

0 1 2 3 4 5

Fluortscenct IntensityNQr«. Counts - No BKGNO

Fluorescence IntensityNOTM. Count! - Ho BKGNO

100 10000350

Wavelength

at Peak (nm)

<00 <50 500 550

CPT: 1G Project: Popile

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

Fluoriscencc Intensity

Norn. Counts - No BKGHO

1 100 1000010 | 10000 | 1000

• •••I • •". • •••

Wavelengthat Peak (nm)wo <50 soo aso

CPT: 5HSTATE COORDINATES:

EASTING ( f t . )

0

Project: Popile

NORTHING ( f t . )

0

ELEVATION

0

( f t . )

CPT based SOILCLASSIFICATION

Cone ResistanceQc ( tons / f t 2 )

l loo10 | 1000

f •W I fW» 1 4M|_i—mJ—i i ill—i * 1 1 |

JC-1-1a.uQ

Sleeve Frictionf, (tons/ft')

} 2 4 6 B 10

in inw 0)L L3 34-' -Ux x

t3•S. •S.

m m m m•u >. *» •o •o •o10 ID '-l C C C0) ^ rt 10 (0 naa. u w w in ui

0 1 2 3 4 5

FluorRSCBncR XntRnsityHorm. Counts - No WGNO

0 SOO 1000 1500 2000

luorescence Intenaitnorii Count* - No BKEND

| 100 10010 l 1000

• •". ! •••I • •". • •••;

y

00 35

Wavelengthat Peak Inm)

50 400 450 SOO 5S

CPT: 4H

STATE COORDINATES:EASTING ( f t . )

0

Project: Popile

NORTHING ( f t . )

0

ELEVATION

0

( f t . )

CPT based SOILCLASSIFICATION

Fluorescence IntensityNorr Counti - No BKGNO

Mavelength

at Peak (nm)

10 J

! :!!l ! !!«350 400 4SO 500

J-

Project: PopileSTATE COORDINATES:

EASTING ( f t . )

0

NORTHING ( f t . )0

ELEVATION

0( f t . )

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

in OT01 01L c-3 3

Cone Resistance

Qc (tons/ft2)

1 1001000

•rt "< iaz z

in in m m.i-> >• 4-1 •o T3 •o10 10 rt c C C(u 1-1 •i-i in (D 10Q. (J (n io i/) en

0 1 2 3 4 5

ELEVATION ( f t . )

0

NORTHING ( f t . )

0

--• 7V - T'llii i 1 1 1 1 i 1 1 1 -

STATE COORDINATES

EASTING ( f t . )

0

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

VI

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

m m (u0) 0) >C- t- ID3 3 C.•u •u o

Cone Resistance x S ,.•»•< -rt ^3

Qc (tons/ft ') in in 2 z in in

1

0-

t; 10 -0)**-

n '•4->S 20-ua :

30-

100

10 | 102 4(11 ; fS» t JM

<?1/jij^^' ' " i ' ' " i ' ' "

00 a

:

J

^

'

', '.

Sleeve Friction

f, (tons/ft*)

5 10 15 20 2

\?

s•

,. ,,,..,...,. .,,...

5

•i-' >•••-' 'O '0 '010 10 '-' C C CCD •-• —i io m loa. u in 01 in in

0 1 2 3 * E

5s3

^s^^i

5^-E>,

..,.,. .... , .... ., .

FlM

3 0

: :

J

•

^"

- —

;

•

uorescence Intent itUrm. Counts - No BK6NO

300 iooo 1500 ro

1

' ' '

F1

100

luorctcence IntensitMorn. count! - No BKGNO

100 10C10 l 1000

• •!h • ••d • •". ! •"

i . .

y

OO 3.

Navelengtri

at Peak (nm)

50 100 J50 500 5;

l i l

50

-0

- 1 0 ^OJ**-

C.•U

- 20 Q

0): Q

-30

CPT: 01 Project: Popile

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

inr-<

4

CPT based SOILCLASSIFICATION

inf—i

in in ID0) 0) >c- t- <o3 3 t-

4-1 J-> 0

Cone Resistance .2 .S 13q<: ( tons/ft2) u, in x z in in

Sleeve Friction ^ S'^ ? ? ? Fluorcscenti intensity Wavelength1 lou f , ( tons/f t1) £ ^ - ro ro TO •-iuor.,c.nc« int.nsuy H»-. <^nt, - N. «K6No at Peak (nm)

10 I 1000 a u (n u) in (o ' '"'•"• counn - NO wens „„ igoin, °>• •—"- "'°"; .^|; ...I . ...i 0 5 i0 15 20 35 0 1 S 3 4 5 » m im ,w> wo , , ..j°. .,J "M ,.i 'f ^JSLT

40- i • i i [ i ...i i • • i - 1"-r"i"-r- ' r" l 1n»i....i...„„„„„„„..[ 1 • • • i • • • i • • • • • • • 1 ^——i • • • • i • •••i——t- 4—l""i""i—4-40

CPT based SOILCLASSIFICATION

m m w0) 01 >c- c- 103 3 t-•u -u o

Cone Resistance .2 .2 ia

q,. (tons/ft8) OT in 2 z m in

1

Cl-

lO-

'S<u '.0)**-" 20-c.•LIa. '•01

a :30-

40-

10010 | 10

I JHI f <«« » <«.1 1 1 1 1 1 1 1 1 1 I 1 1 1

^

^\

^

^

\

^

^

^^

' ^^•

^

<^

• • • • I • • • • I • • • •

00 C

'

; ;

\ \

\ \

Sleeve Friction

f, (tons/ft')3 5 10 15 20 3... 1 . . . 1 . . . 1 . . . 1 . . .

S

?11>

»>?

1 1 1 • !

5

.U >. 4J T3 T3 •0ID ID •-i C C C0) ^ •x 10 10 10a u in (n ui in

0 1 2 3 4 ;

—s=^

^'^

>f''?

^ ,^^^^^™^*^ ^^

..... , ........ ... .

F

N

0

•

;

- -:

•

;

- -•

;.

•

- -;. ',

uortscence Intensit»r*. Counts - No BKGMO

900 1000 1500 201.

. . .

F

y

00

luorescence Infc«nslt

Harm. Counts - Ha BKGNO

100 10010 l 1000

; •"l • •" • • " 1 • •"

I • 1

y

w0 3S

:

^•

Wavelength

at Peak (nin)

50 WO 4SO 500 5S

J

1 1 " "1 "

SO

-0

- 10

•hi01

QJ•*-

-20 ~c.4-1

: a<u

; Q

-30

-40

CPT: OJ Project: Popile

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

in

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

CPT based SOILCLASSIFICATION

in

APPENDIX B

CHAINS OF CUSTODY

and

RAW DATA

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corps of EngineersTuba District

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corps of EngineersTuba District

-^r^c^LL& L5>t^Lab# Chest/Temp.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corps of EngineersTulsa District

Pn

Sai

Pn

CONTAINERS

fi

^PARAMETERS SAMPLED

«

^

^

oiect: Popile. Inc. (^.-^S-^

mnie ID: 0 K 5^ Date: /(e Sent 1997 Time: <9

€5-0^^

oiect POC:/?tcBEK AlAfig^ Phone:662-2706 Due Date: ^

ilass Plastic Vials Chest # Custody Seal #

1 —— —— -•7° ^^7

Semi-Volatile Organics

'-T^H-T). / F^AC.r/0^.»'

.r

^^sVOA

^^^

Chest Sam^Br# halnals

8270A

60/s'

1S^

.u^k.s

v ^1 '

^

>

* Containers: () = 1 L Amber Glass [ ] = 1 L Plastic { } = 40 mL Vials

CUSTODY RECORD

-d—•V

Jlelmquifhed Byymw^ Received By Date Time"e—~~^——————- ^//fl/77 IS 00

—————————————————————— 1 / f O f i l ' s'

D Bus Bill n Shipping Bill o Other No.

Lab# Chest/Temp.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corps of EngineersTuba District

Project: Popile. Inc. , r{c\.0-{0.6

Sample ID: d i< ?_______ ^ate: Zfl Scot 1997 Time: 08o0

Project POC:'i?ii&Piu X^6g^ Phone: gp^-afcZ'2708 Due Date: Z, 10^

CONTAINERS

filass Plastic Yials Chest # Custody Seal #

J_ -=. _T ^0 f/^

VOA Chest Sampler ^

PARAMETERS SAMPLED

l^

1

Semi-Volatile Organics

^-TP^-bic^ -P^c-ro^

8270A

SOISm -H-^

* Containers: ( ) = 1 L Amber Glass [ ] = 1 L Plastic { } = 40 mL Vials

CUSTODY RECORD

nm'^'^rf

tffiiqhi(dByW^

(J

Received By /Date- y/fi/?7

TimefS-00

D Bus Bill o Shipping Bill a Other No.

Lab# Chest/Temp.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corps of EngineersTulsa District

Project: Popile. Inc.(2.^-3.5')

Sample ID: (T^ 6"2-_______ Date: t6 Sept 1997 Time: 1010

Project POC: Ri<fif^ MAger Phone: ^2-T-7Qg Due Date: "2 ^J^ ^

CONTAINERS

Glass Plastic Vials Chest # Custody Seal #

_L —— ^_ M1--JO ^7

•s^VOA Chest Sampler^--^ ^ # _ hiit*d£

_.^^c.PARAMETERS SAMPLED

y Semi-Volatile Organics

^ ^ . /' ff^ *

T?/4 — D/cse/ n<? AC,T/O/J.•ir,

8270A

eo/s'^\i

1 3

* Containers: () = 1 L Amber Glass [ ] = 1 L Plastic { } = 40 mL Vials

CUSTODY RECORD

/i .Rcimquished ByftSSf-^^y.

~

Received By Date Time';=——————————— ^//«^7 /S-OO

a Bus Bill a Shipping Bill n Other No.

Lab# Chest/Temp.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corps of EngineersTulsa District

Protect: Popile. Inc.

Date: /&Sept 1997Sample ID: Time: /02^

yo</Project PQCi^ftg <U ^<6 w' Phone: fi62-'Z'70R Due Date: 2. ^/Cy

CONTAINERS

Glass Plastic Yials Chest # Custody Seal #

^L ^- ° ^/6Y

PARAMETERS SAMPLED

«^

<•

^Semi-Volatile Organics'

TPH'2>ieSe/ P^c-r/aA}r,

8270A

8-0/5'w s

^(-yo,) J

* Containers: () = 1 L Amber Glass [ ] = 1 L Plastic { } = 40 mL Vials

CUSTODY RECORD

r%

~

o Bus Bill

quishod By%€y

D Shipping Bill

Received By

a Other No.

Date

Y^-iTime

/6"2 ->

INVOICE

Pace Analytical S«rvic»», inc.HW 8922, P.O. BOX 1450

Minneapolis, Minn«»ota 55485-8922New orleani Phone (504) 469-0333

Bill To;DISBURSING CENTERU.S. Amy Corpa of Engin»T«,M.O.POBt Office BOX 60267N«V OrleaM, LA 70160-0267

Invoice N o . :Invoice Date:Lab Pro) Mo . tLab Acct H e . :Ternf:

2252009/26/97524520385126Net upon Receipt

Project:Sif:PO No.:

CALL #0013

DACW-29-95-A-0010

Suronarv by Sairpr

Lab ID Client IP

JAP-001 'OG2JAP-002 'OG9JAP-003 'OK5JAP-004 'OK9JAP-005 1D6JAP-006 1D16

6 Smplw

=£l2£ Collected Received

SoilSoilSoilSoilSoilSoil

09/1809/1809/1809/1809/1809/18

09/1909/1909/1909/1909/1909/19

TotalPrice

9295 00295 00295 00295 00295 00295. 00

$1,770.00

summary bv Product

fity Peecrtption

6 SeiDivoletile Organic* by SW 82706 Moiature by CLP sow6 Fee for disposing of aamplea6 TPH a« Diecel by SW 8015

6 saoplee - Totel Amount Due

UnitPrice

TotalPrice

$240.00 $1,440.00.00 • .00

5.00 30.0050.00 300.00

$1,770.00

Pleace eubmit a copy of this invoice with payment

Pana AnalyticalPtCtAfttlyticlServtet.lnc.

161 JtmnDrivWMt Suit* 100______ft, (tot. LA 70087

TB): 804^694383FUC504-48B-0555

Reuben MabryU.S. Army Corps of Engirteert,N.O,Poit Office Box 60267New Orleans, LA 70160.0267

Project: CAUL il0013Site:Episode: JAP

To: Reuben Mabry

Enclosed please find the analytical remits for sample(s) received byPace Analytical Sendees, Inc. • New Orlean&i

This report contains a summary of the quality control data associatedwith the analyses as well as copies of the chain-of-custody documents.

You may direct any inquires concerning this report to your ProjectManager, or any one of the Project Managers listed below:

Ms. Karen H. Brown, Manager, Ext. 325Mr. Craig McCollum, Ext. 326Ms. Cindy Olavesen, Ext. 327

Sincerely,

v-^^g^Project Manager

Enclosures

Pice Analytical Service!, lac. -New OrleansSimple Crou Reference Summazy

Episode:

Project;

Site:

Lab ID

JAP-001JAP-002JAP-003JAP-004JAP-005JAP.006

JAP <

CALL*0013

Client ID

•OG2•OG9'OK5•OK91D61D16

Client: U.S. AnnyCorptol

DeccriptioB

(iy-3^(9ff-WS)(5.'-6.5')(9Jtr-io )(6 .75')(iss'nff)

rEagiaeenJf.O.

MatrixScfflSoilSoilSoilSoilSoil

Collected09/18/9709/18/9709/18/9709/18/9709/18/9709/18/97

Received09/19/9709/19/9709/19/9709/19/9709/19/9709/19/97

Report of Laboratory AnalysisPace Analytical Service, Inc. • N«w Orieani

Sinfl* Sampli • Protocol

Client ID: yqi

ProJtt: CALLI>M13

LabID: JAP.M1

D«Kr(ptlon: UJL2 1

Method! t^ San SW »»fl Semtvol.tll. Organic!

ni.nf U.S. AttMV CORPS OF ENCWmS.N.O.

Site: None

Epiiode: JAP Sample Qu:

Matrix:' Sofl % Moliture: U

Batch: p637 Untf; 11102

r«p Factor!

CASNamb«r

i3.32-9201-96-1120.12.7S6-fS-3205.M.220741496».tf-0191-24.250.324100-51.6101.5S.3IS.66'7106474111.91.1U14M10140.1S9.S0.791.M-7<S-S7.»7005.72.}211-01.9S3.70.1132-6«.914.7A.2»$.50-1541.73.1106-46-791.94.112043-21446.21 OS-67.9131.11.3S34.S2-1fl.2(.S

•••

B«B»o(».h,l)pciylenB

2,4.Diehlorephenol

2.4.Dimcihylp)ienol

4.6.[>iphn>-2-me>hylphBnol (4,6.Dinliro«<tnol)

1.00 Laad»«l;nA

P«nm«ur

Aeenaphlhcn*AaenaphthyliiHAnthnecwB«nio(i)uithnc«T(eBcnu(b)nuonnihenoB«nxo(k)fluoH»thmiB«BUleKid

Bcnxo(«)pyreBcB«niyl alcohola.Bpomophcnyl phuiyl «h»Butylbcnzylptutuliie4.Chlorouiline (p^hloroinlline)bli<2-Ckloroeihoty)m«thu«bi*(2^Hore«hyl)tlh«rM»(2-ChlBroitOpropyl) •thw4-Chloro.3-iMthylph«no) (p-Chloro-m-crewl)2^'hlorenaphlhal«n«2<hloreph«nol (o-Chlorophenol)4^hl«iophn>yl phcnyl etherCtuyoncDibcni(»,ti)«Jiihn<KntDitemofufMDi^rbutylphtlultM1 •Djchlorobenz«m (o-Diehlorebenxene)l.J.Dichlorobcnxnc (ni-DiehlwobtRitn*)1,4^iehloreb«u«n* (p-Dichlorebenzenc)SJ'-Diohlorobenzidine

Dilhylphlkitaf

Dimcthylphitctiic

2,4-Dimliephenol ND

Pr»par»d: msa

Dttailin RMult

ND

ND

ND

NDNDNDNDNDNDND

NDNDNDNDNDNDNDND

NDNDNDND

NDNDNDNDNDNDNDNDNDNDND

hT

Qu

.

Analy

R

,

i

•d: 2,L&

ipoRincLimit

316316316316316316966316316316316316316316386316316316386386316316316316316316316774316316316316966966

dd2Z 1«!06JA

Rf.Limit

MBfMBHM D———JI WftwActflMMJ MBWIl

OT—MlMulMrMfririuMi iwmprMuri•—nks Lhrti h •n««« fer MB Il «tth IMllM •MQI in 4MMtarbJ»i«k wtMWn m «<<lM4n«lH •

fMiturtrcMh—lilt—lit to.ft^——fUUM Iffl i BhL

rruunfn.

Report of Laboratory AnalysisPace Analytical Service!, Inc. • New Orl«an«

Slogte Sunpl* • Protocol

CtlmtID; •aSal

Project; ^Lif*0""

LabID: JAP-MI .

Dwcrlption: 12^=2^1

Mrthnri. Law Son 8W ITO S«Tilvol.tU. QManto

Client: SLfii-ABMXJ

Prop Factor: Lnehod: n/a

Site: Hflnt

Epbodc; JAP

Matrix: Sea

Batch: 22fi2Z

Pripandi ,Q.SW^

Sample Qu:

%Motetun: 11

XJnSU! n«/i«

Aiialyxod! 22&Be2Z IfcfifiJA

CAS Number

121-14.3

606-20-3

11744411741.7206-44-016.73.7

Ht-74-1

1748-3T7.17.A(T.72.1

19}.39-S

TS-59-1

91.57*9M1.7

10M4-591-20.311-74-4

9949«2100-01<6

91>9S-3(1-7S.S100-02-7

16-304

621.64-7

1746'SIS-01410f-9i-2129^0-0120-i2'l95.95-4

(146-2

FTBIHIT

2«4>D»iaoioluciM2 'Dinltrotoluenc

Di-n-oeiylphihilucbi*(3.Eibylhwyl hih«l«ie

PluonnlhcncFlwicaeH«x*chlofob«nun»

HuMhlombuudl«m

ItarehloroeyelopmudifHcrehlorMdnn*Indffio(lJ.2<d)pyicne

Isophoron*2.Mnhy)M(»hlhxlcnc2-Melhylphcnol (o-Cmol)

4>M«hylph«nol (p-Cmal)Niphihalcn*

2-NlireuiiliB* (o-Nlirouiilinc)

l-Ntmullint (m-Nltiwnllloc)4.Nitro»)l)iiK (p-Nitrotniline)

Nilrobenacnc2'Niirophenol (o-Niirophcnol)

4-Niuophenol (p-Niirophtnol)

N'NitroMdip)»nylinlM (DiplHnytemiM)

N.NiUB»o-di.B.pn»pyl«niM^ntaehloiophenolPherunliirenePhtnol?ywncl ,«.Trieh)orob«ni*n*

2,4 -TriehloTOphOTot

2,4,6-Triehlofoph«nol

DUudon Rnult

ND

NONDNO

ND

NDND

NDND

ND

ND

NO

ND

NDNDND

ND

ND

NDND

ND

NDNDNO

ND

NDNOND

ND

ND

ND

Qu

AIO

RiponiDfLimit

316316

316316316

316316

386

316316

316

316

316

116386

316966

966966

316

316966

316

316966

316316316

316

966

. 316

Ret.Limit

NB «•«• MM IMUMI M •r •k>f IM •«|«M npMitai taH.UUUUUHllHllMnStHH* n<»»^»——»———Ufcr«l

OBku^^Mtan. »>ini iiitrniiiiiniiirri iritirmi

Report of Laboratory AnalycisPace Analytical Service!, Inc. - New Orleans

Sinite Sample • Protocol

Client ID:

Project: f^

Lab ID: JA

Oe*cripUon:

Method: U

Prep Factor:

CASNumbf

•3-32.920t.96-<120.12.7

S6-55.3

205-99-2

207414965-15-0191.34-3

50.324100-51-6

101.55.3IS41.7

106-4741 1 1 - 9 1 - 1111-U.4

10(40.159.S0.7

91.58.795.574

7005-72-3211-01-953.70.3

132444K-74-295.S0.1Ml.73.1IAJL.A&^T100^0^7

91.94.1

12043-2•446-310547.9

1 3 1 . 1 1 . 3534-52.151-2».S

m(to»Kirt>tfriiiN»nf«te-il>TrlMlrtrirnlnftrtkr4R—MMl—rM»*rMi«L TI>cPpwF——f'——Uhriwrr—(l»Ufl<ril&«WMUMU>l>k«WT«MI

rwitew—k.——

aLLLOOflia

P-001

ft'-Mtff')w Son SW MTO S.mlvol«t0» Omnlci

1.00 L«aeh«di n/a

hmnlir

ABn hiiMMA««Mphthyl«n«

ARthncnrB€nzo(i)unhrec*ntBen2o(b)fluonnih*ne

B«2o(k)fluennih«n«

B«aoie«eidB«iao(f.h.i)p«ryt«neB«ao(«)pyt»rx

Bmyt alcohol

4'BromoplMnyl ph*nyl tirr&uiylb«nzylphihiliu

4-ChloroinlliM (p-ChlorMnlline)bii(2-Chloreethoky)meihui«

UK2-Chlofa«hyl)«h«r

bit(2<hl(Wt>itopn>pyl) ethtt4<hloro.3^n*ihylphcnol (pChlore-nxmol)

l hlorenaphtlulcn*

2-Chlorophoiol (o-Chloropbinol)4^hlon»phwyl ph«pyl •ih»r

ChrytcncOJben2(a.h)uithneeneDib«nxofunn

Di-n-buiylphtkaliic1,2'Diehlorobenxcne (o-DichlorebeniMie)l -Diehlorobiixeiic (m-Dlehloiobenzeac)

l.4.Diehlorob«n2cne (p-Diehlorebauue)

3J'.Dichlorebenzidine

2.4-Dichloiophmot

Dieihylphtlalite2,4.Dimahylphenol ,Dimeihylpbltalne4.6.Diniiro-2-meihylphcnol (4.$-Dinitro-«<iMol)

2,4-Diniirephenel

1 If •——!• •I L •lUBltoft —•1 f^f——fl IfABBUMkk

Wf • • —if — i— r •c — Ryww

aii51

SplMK

Matr

BaU

Pnpin

Dilution

500100

100

100

100

100

100100

100100

100

100

100100100

100

100

100

100100

100100$00

100100

100

100

100100

100

100

100100100

"t: VA.Jt«: l)j[ffM

l«l JAP

Ix: M!h: 23637

id: Itt-Sm

RMldt

145000

NO234000

164000

5660046200

mNO

50400mND

NO

ND

Nt>ND

ND

ND

ND

ND

ND149000

ND632000

NDND

ND

ND

NDNOND

NDND

NDND

iBiCLCfiBB

Samp

%Mo

"97 Ani

Qu

P2D1

P2DI

KDl

P2D1

P2D1P2D1

P2D1P2D1P2D1P2D1MDl

P2D1

P2D1

P2D1

P2D1

P2D1P2D1

P2D1

P201

P2D1

P2D1P2D1P2D1P2D1P2D1

P2D1

P2D1P2D1

P2D1

P201

P2D1P2D1P3D1P2D1

SOFENGINEERS.N.O.

ilcQn:

totun: 24 • •

Unito: ue/kg

dyMd:lfcSlfc22 IfilfilJA

Rixntrt Rn.Umtt Limll

2200004400044000

44000

44000

44000

110000

4400044000

44000

44000

440004400044000

44000

44000

44000

44000

44000440004400044000

22000044000

4400044000

44000

81000

4400044000-

44000

44000110000

110000

MW 12«J1

Report of Laboratory AnalysisPace Analytical Servlcel, Inc. - New Orleans

Sine)* Sunpli • Protocol

Client ID: 1

Project: £

LabID:

Deicription: f?

Mttbod: Li

Prep Factor:

C\SNumb»r

12M4-2(06-30.2117.144|l7-»l-7206-44416-73-71 It-74.1»7-68.377-47.4

(7.72.1193.39.571.S9.191.57495-4C.7106-44-591.20-3M.74-49949-2100414M.95-3M-75.S10042.716.304(2144.7

I7.»6-i1541.810».9$.;12940412042.195-9S.4»46.2

41——FMrflUrq

B2ALL 00013

^myw}sw SoH SW »270 S»mlvolitllt Oreinlf

1.00 Leiehfd: n/a

PanmMcr

2,4-Dinimioluenc2,6-DiniiroioluMitOi-fl-octylphihalaicbi«(2-Ethylh«xyl)phlh«taieFluoruithm*PluorencHexKhlorebcnuneHixuhlorobuudicmH«xkchloracyclopentidi«n«Hex»chloTO*ih*neInd«no(1.2.3<d)pyttncInphorone2.M«thyln»phih«lcnc2'Mthylphcnot (o-Cmol)4-Mclhylphcnol (p-ClCtOl)Naphlhalene2-NiimanlIine (o.NnrenUine)3-Nitroaniline (m-NiireaniHne)4-Nitnailin* (p-Nitretnilin*)Nilrebcnuiw2-Niirephfnol (o-NnrophcnoI)4.Niirophenol (p-Niwphcnol)N.Nitro*odiphBi»yl«mlnc (Dipkenylnninc)N-Nitroto-di-n-propyltminePenuehlorophtnolPhcMnihnn*PhtnolPyfBe1,2,4-TriehlBfobeniene2,4,5-TrichlorBphenol2,4.6.Trichlorophenol

•Hrt

Clh

S

Cpbo

M«ti

Bat

Pnpir

inhnlon

100100100100500

- 500100100100100100100500100100

2000100100100100100100100100100

2000100500100100100

nt; VrS^If: Non»

dc: JAP

•IX; SQfl

eh: 23637

edi 2ibSa

Rwull

NONDNDND

994000735000

NDNDNDNDNDND

756000NDND

2900000NDNDNDNDNDNDNDNDND

2460000ND

691000NDNDND

AMY COUP

Samp

%Mo

:22 Ani

Q"

P2D1P2DIP2D1P2D1P2D1P2D1P2D1P2D1P2D1P2D1P2D1P2D1P2D1P2D1P2D1P2D)P2D1P2D1P2D1P2D1P2D1P2D1P2DIA10P2D1P2D1P2D1P2D1P2D1P2D)P2D1P2D1

S OF ENGINEERS N.O.

lie QU!

fature: 21

UniU: ue/kg

dyxed; 24-S«-97 13 ^

RqwHiiiy Rf.Limit Limtl

44000440004400044000

220000220000440004400044000440004400044000

2200004400044000

1790001100001100001100004400044000

1)00004400044000

110000(7900044000

22000044000

11000044000

m ••MC N« Biu«rf ii w •»»>« •< *«)•««« npMitti miiftr ««•«)<• Mllllur—ft nuwL •nM^vri—r •€••«• hr i•^•A—i UBK • MflMMB fcT MBI— •—• HMU— ••• BWIUfr W

Qihii —An lrrilk4«Ukn«i*«—MlMttc««r—f«ftf ••taw ftMkL —l J—IM iwMl ti n fvuJ fcf Biriilw i

Report of Laboratory AnalysisPace Analytical Service^ Inc. - New Orleam

SiD{l» Simple • Protocol

CUmti U.S. ARMY COBPS Or ENCINEERS.N.O.Client ID: ;flK£

ProJ«ct: CA,LLffOO»

Lab ID: JAP.M3

DMcripllon: Sa^&£l

Method: Ifflw Son SW »n0 SMnivolrtite Or«nk,

Site: Non«

Epbode: JAP Sample Qu:

Matrix: Sou %Mol»ture: If

Batch! 33637 Unite Bidse

Prep Factor:

CA9 Number

»3-32-<

201-96-8

120-12.716.S5.3

205.99-2a07.08.09

if •(5-01 9 1 •34.3

SO-32-8

100-51-6

101.SS.315-68-7

106-474

1 1 1 . 9 1 - 1

111 -44 - *

101-60-1S9.S0.791.SS.79S.$7.»

700S-72.3

211-01-9S3-70-3112-64-9K-74.2

9f-$0-l

$«1.7}-1106^6-7

91.9*.!120-13-214-66-3

10547-9

1 3 1 . 1 1 . 3

534-53.1

51 •21-5

ND A——lM KM MMArt

UF «—n piruM ru*IWHiwUikJik—niqiUM«Minm. l «•—— ^LJ« B^ hL •tfTV* •WO<W ^——•^ ^W

1.00 L««ch«d: H/I

PttiiMltr

Aeen«phlh«n«

AecBiphlhylm*

AnthneeneBcnxo(l)intlnMene

Biuo(b)flua(wi(hcncBanxo(k)fluor«nthene

Benxoic Kid

Benw(|J),i)payleM

BmsoOpynne

Benzyl alcohol

4.Bremoph»nyl phinyl *ihtr

Bulylb«nzylphthsl»it4-Chloromlllnt (p<hloreanilinc)UK2<hlon»«hoxy)methnc

bii(2-Ckloieelhyl)eiher

bi*(2-Chloi«i(oprepyl) ihcr

4<:hlDro4-BMihylph*nol (p'Chloro.ni-ciwI)2<hloroniphih*lcnc2^hloropheno1 (o-Chlorophenel)

4 :klorophenyl phenyl ethtr

ChxycneDibenx(i,h)utthru«n«

DibtflxofunnDi-n-butylphlhilnc

1 i2*Dicli)orobcnsene (o-Oichlorobenzenc)1,3-Dichlorobeiizene (m-Diehloro benzene)

1,4-Dichloreb«n2«ne (p'Diehtoreb«nxene)

3 '-Diehlorob(nzidia«3.4-DlchlorophcnoIDieihylphlhilue

2.4'Dimcthylphtnot

Dimnhylphihilu*4,6-DiBiuo-2-m»lhylphenol (4,6-Dinitro«mol)

2,4.DiBiireph«nol

uf(«Mui. TkhwyiiwriMiMiliriMi'r—dM—yh—LiMfcr •iwk ill*. 4U«ilw •rt ••liun—IMI If •rftaMe.ft Mino"' i" «m»n 11 i»i •n irfti nfin

Prepared: 2JkSfilh

Dilution Itwult

—•- —

ND

NO

ND

ND

NDNDND

ND

ND

ND

NDNDNDND

ND

NDND

NDND

ND

ND

ND

NDND

ND

NDNDND •NDND

ND

NDNO

NO

«4&ri IM-SI

XL Anal

Qu

M2

M2

M2

M2

M2M2M2

M2

M2

M2

M2M2M2M2M2

M2M2M2

M2M2

M2

M2M2

M2M2

M2M2M2M2M2

M2

M2

M2

M2

lyxed: 2&&

ReportingLimit

393

393

393

193

393393983393

393

393

393393393

393393

393393

393393

393393

393

393

393393

393

393717

393

393393393

983

983

S&22 UifZJA

Rt.Ltnill

Report of Laboratory AnalysisPace Analytical Service*, Inc. - New Orleans

Single Sample • Protocol

CItantID: aKS

Project: ffALlf*?9"

LabID: iIAE fil

Description: i& dL

Method: p.w San SW »70 S .hml.tlte Oro.nlcc

Ql«.t; y^ ABMYCQftPSOFSNGINEEBS.N.O.

Site: KfljOS

Epbode: JAP .SampkQu:

Matrix: SflB % Motetar*: If

Batch: 23622 Unit*! yg^g

Prep Factor:

CAS humbir

131.14.3tOt-20-2

IIW-0117.11.7206-44-0

16.73.7111.74.1

17.6S.377.47-467.72.1193-39-S71.S9-191.S7.69S-4».7

106<44.591 •20-3U.744

99.09.2100-014

91-95-3M.7S.S10042-7

16-104(21.64.7»7-»&-5

1S41-B10g.9i-2129-00-0120-82.1

95-9S.4

((•06-2

tar-. 1.00 Leached: n/»

umbir Pinmeur

-3 2,4'Din<uo(ol.u«Mi-2 2,6.Dlniirotoli»M-0 D^n-octylphilulnc•7 bll(2.Elhylhciyl)phth«l»M

\-0 Fluoruikcne

7 Fluonm^1 H«xKhlofobauECfle3 Htxachlorobuudiene

4 HexKhloroeyclopenudien*1 Hcuchloroethinei.S Indent 1 3<d)pyi«Mt liophorone6 2-Mcihylnaphdulcm7 2>M«bylphmol (o-Crwol).5 4.M«hylp)wnel (p-Crfol)3 N«phl>«lenc4 2'NftroaniliM (o-Ni(reuiiUM)

2 3-Nitreuiilin«(m-NiinnniUiu)4 4'N)(roaalliM(p-NinDaUiM)3 Niuobenz«MS 2-Ninopb«nol (o-Niwphenol)1.7 4-NltrephcBol (p-NiUBphMBi)6 N'NinosodiphenyliffluM (DiphOTylBBBw)(.7 N-Niuow'drn'prepylttnin*5 Puuehloropbenol& Phm»thi«n«

i-2 nMHOl

)-0 Pynnt1.1 1 .4.TrichlorebCTi»nt4 2,4 -Trieh}orop)Mnol

2 2,<.6.Trich)orophenol

Prapared: 21bSfiB

Dilution RwuU

NDNDND

NDNDN0

NDND

NONDNDNDNDNDNDNDNDND

1 ND1 ND

1 ND1 ND

NDNDNDNDNDNONDNO

ND

=22 An

Qu

M2M2M2M2M2M2

M2

M2M2M2M2M2M2M2M2M2M2M2

M2M2

M2M2M2A10M2M2

M2M2M2M2M2

M2

alyzad: m

ItoportincLimit

393393393393393393393

393

393393393393393

393393393913983983393

393913393393983393393393393913

393

ap-S

•

22 ILfliA

R,.UmK

•

HO fw H« RIMM* 11 w •tonik* rtl—MJ nrwPf <•«• M.OM VMM f MMO. T**n«tFMwr1fMlk| UBM b •rmid (kr ••»)• A*, ikitel—Qil—4iiUbn. (-dlh<1MhnMt«««Mluf«*(U*mp«n.

hr i MHWUM——k ilu.

•likur hr ••imi* —4 MI J«ir MI rtUakW.

VUlfJ 1145:11

Report of Laboratory AnalysisPace Analytical Servicel, Inc. - New Orleans

Single Sample • Protocol

atoHti U.S. AKMV CORPS OF ENGINEERS.N.O.Client ID; «OK»

Project: CALL<IM13

Lab ID: ilAEdlfli

Description: ^B'•10•S^

Method: Law Sell SW PTO ScmivolitHe Org.nlci

Site: MBDC

Episode: JAP Simple Qu:

Matrix: Sell % Moltturt: H

Batch: 23637 VnlU: XfZkfi

p Faeior:

CAS Niinbtr

13-32-920S.96.1130.12.7

56.55.3205.99.;207.0g.09-

6S-IS.O191-24.2

50.33.1

100-51 •<

IOI-fS.31541-7

106-<7-»1 1 1 . 9 1 - 1

111-44-<

IOi-60'119.S0.7

91.SI-7»5-574

700S.72.3211-01<9

53.70.313244.9

»4-TA-295.SO.I

541-73.1

106-16.791.94.1

120-11.2

1446.2105-67.91 3 1 - 1 1 . 3

534-52-151-2(.S

I-M L.ach«d: 1^1

rttnmfr

Aceniphthm*

AccMphlhylene

AaihiweneBcnzo(<)uithncen«

Ben»{b)nuonniheneB«no(k}nuonnlhene

BcMeicKidBCT20(».k,i)peiyt»nt

DcMO(ft)pyiBM

Benyl aleohol

4-BToniophenyl phenyl «h«rButylbenzylphtlulau

4-Ch)orBuil1int (p-Chlorouilini)bji(2<hIoro«lhoKy)(n«ituncbit(2<l»loreeihyl) ether

blt(2-CW<w>l»opn»py))eiher4<;hloro-3-mclhylphcnol (p-Chlorc-nxntol)2-Chlarofliphihaltn*

2^h]orophmiol (o^hlorophcnol)

4<hloroph«nyl ph«nyl •thcr

ChryicneDibnn(«.h)uiihr*eene

Dibcnxofunn

Di rbutylphthaltM

IJ-Diehlorobenxut (o.Dichlorobaame)I,3.Dichlorobcn2Ui (m.Dichlorobcnzcnc)1.4.Dichlorob«nz»n* (p.Oichlorol>*nMn«)3.3'-Dichlorob6nzitlinc

2,4-Diehlorophenol

Oi«ihylphihalti«2,4.Diinnhylph«nol

Dinnthylpluhaliic4.6-Dlnino-2-mcihy1phenol(4.6-Dinitnx-ciciol}2,4-Dinilrophcnol ND

Prepared: ySkSSt

Dilation Ruuli

ND

NO

NO

ND

ND

ND

NO

ND

NDND

ND

ND

ND

ND

NDND

ND

NDNDNDNDND

ND

ND

ND

ND

ND

ND

ND

ND

NDND

ND

6fiZ A

Qu

D2

D2D2

02

D2D202

02

D2

D20202

02

02

020202D202

0202

02

02

D2

02

02

03D2D2

02

02 .02D2

02

Jialyzed: Ifci

iteponiniLimit

1960

I960

1960

1960

1960

19604910

1960

1960

1960

196019601960

1960

19601960

19601960

1960

19601960

1960

1960

1960

1960

1960

19603940

19601960

1960I9604910

4910

>CB-!12 14:11JA

RI.Limit

NO *m« 4) D|WIM« M •'«br« ikf i«iMf« rwwilq M»li.bFimUiMillMPMUffninA. TW rrw r MM———*)•'• M.mllMiu*»ltilK.•« nlf Ulk k—T——4 fcr ——ptellM.«UlU— 11 ••bun •Mr trnfllllfcQ* nu vMMifk (p«l( 4«Mlm •r* «*11«<« M iftf •J (fikf npMt.

Report of Laboratory AnalysisPace Analytical Services, Inc. • New Orleans

Single Sample • Protocol

Client ID: '0X9

ProJtCt: CALLOQ013

Lab ID: JAP.B04

Description: {«JLJfi£l

Mthod: Lour Soil SW «270 S^mtvolatll. Or»ank»

Prep Factor! Leached: n/aJM.

Site: None

Epiiodc: JAP

Matrix: Soil

Batch: 22fi2

Rnparad: ISbSiB Z

Client: U.S. ARMY CORPS OF ENGINEERS NO

Sunpk Qu:

% Moiiture: If

Unitt: Hg e

Analyzad: 24.SMi.07 IUIJA

121-14.3

606-20-2117.14411741 .7

206444

16-73.71H-74-1

17-61-3

77.47.467.72.1

193.39.S

71-59.191-S7-6

95-41-7

10644-S

91.20.311.74.4

9949.2100014

91-9$-3M-75-510043.7

16.30462144-7

17.16.SM-01-*

108-9S-2

129404

120.12.195-95^

1146-2

«——»WM

r«niM(T

2,4.Diniiroialucn«a.6>DiniumeIuene

Di-n-«etylphihilue

biK2.Eihylhexyl)phih^ue

Fluonnthene

FluercneHftiLftehtoAbGiiXftueHexiehlorobuUdiene

H«XKhloroeyclopentidi«n«

Hcxuhlorocihuit

tod«no(l «l)pyr<m

liophorone2-Methylnapktlrlcnc2-Meihylphcnol (o-Cmol)4-Mcthylphenol (p-Crwol)

Niph(hal«n«

3-Nitrouiline (o.NltrouillM)

3.Nluunilin« (m-Nluoiailim)

4-Niuouiltoc (p.Niiroanillne)

Nilrobcnxmi2-NiiropkenoI (o-Niirophcnol)4-Niirephenol (p.Niirephenol)

N-Niirecadiphnylinim (DiphmyluniM)N.Nluoto-<li-B ropyl«mlBe

{'•nuchlorephcnol

PheMBtluencPhenol

Pywr1.2,4.Trichlorobentenc2.4J.Tnehloroph*nol

2,4.6-Trichlorophtnol

DUutlop RM«II

ND

ND

NDND

ND

NDND

ND

NDND

ND

ND4380

ND

ND

ND

ND

ND

NDND

ND

NDND

NDNDND

NDND

ND

ND

ND

Q«

D2D2

D2

D2

D2D2

D2

D2

D2

D2

D2D2

D2D2

D2

02

D2

D2

D2

D2D2

D2D2A10

D2

D2

D2

D2

D2

D2D2

D2

R^ortliK• Umk

1960

19601960

1960

1960

19601960

19601960I960

1960

1960

1960

1960

1960

I960

49104910

49101960

I960

49101960

196049101960

19601960

1960

4910

1960

R«frUmh

Nb «••«•!•« DM«I« 11 •r Urn* ue •JJiMf HpMitat IILM «M«H» BUMI— VMM sl linn, IWPrwFMuriMMMiftram-fiUiMM—pbilM.

r«ffcw»r»ln.»«> run nrMhaN •in* «<>»«• ••linn MIMI '

VWn 124fJI

Report of Laboratory AnalysisPace Analytical Service!, Inc. • New Orleani

Single Sample - Protocol

Clitllt: U.S. AHMY CORPS OF ENGINEEHS.N.O.

Site: None

Epiiede: JAE Simple Qu:

Matrixi Sell . % Motetun: 12

Batchi M63? Unite av^se

Client ID; Ififi

ProJ«ct: CALLfmi

LJbID: ^P.005

D-cription: fg.ft'.T 'l

Method: Law Sofl SW «270 S.mtvolatll. OrgMito

ip Factor:

CAS Number

13-32-9201-964120-12-756-5S-3205.99.2207.01.09<5-<5.C191-24-250-32-tIOO.S14lOI.Si.31541.7106^74111-91.1111-«4-4IOi.60.159-50-791-S(-79S.S7.»7005.72.321ft41.953.70.3132-*<-9•4-74-295-SO.I541.73.110fr46-791-94-1130.13.21446.2Ktt.67.9131-11-3534-S2-15i.a»-5

1.00 Leichtd: n/i

PTimter

AceiuphtbcncAcenaphlhyleneAnihmceneBeno(t)MilhncencBomc<b)fluoTWihcncBeMe(k)fluomiheneBenxoicaeidBcnto((.h.l)petylcncBemoOpyicneBenzyl •leoholi-Bmnophenyl ph»nyl etherButylbenxylphthiluci^hloronilinc (p-ChlonwIline)bi«(2<h1ort)«hexy)meih«ntbiK2<hlof«ethyl) Th«rbl((2<:hloroliopropyl) (ih*r4-Chloro-3-mcthylphcnol (p-Ckloro-m-c(«(ol)2-Chlorontphthilene2<hloreph«ne) (B-Chlorophwiol)4-ChIerophMyl ph«nyl «lhfCluycrnDibc(a(iJi)uihmc«rDibeniofUwiDi-o-buiylphthxiatet^-Diehlorobenxni (B-Diehlorobcnzene)l^-Dichlorebrnzcne (m'Diehlorebenxene)1,4'Dlchlorebenien* (p-Diehlorobtnzent)^•-DichlcTObcniidine i2,4.Diehlon»phenolDithylphlhiluc2^.Dlmuhylph«nolDimeihylphihilM*4.6.Diniiro-2.mnhylphcnol (4,6.Dinitroo<rttol) i2,4-DinlirBphcnoI

BBlklll fgffg^

PnpBnd: JO'Sfl;

INIoiion Rmll

iiJ

<

j

j

1

1

1

j

5 NDjj;iijj4

1

;

1

j

1

S NDS Mnpiu5 ND

J

J

1

5 ND

f ND

; ND! ND! ND! NDi NDi ND-; ND( ND! ND! ND

8 NDS VDi NDS NDf ND5 NDi NDi ND5 ND! ND? ND! NDi ND

i ND! ND! ND1 ND

> ND

S22 An

0"

D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D2D202D2

UUlfl JUf

alyzMi: 24.

R^MHineLimh

205020502050205020502050S120205020SO205020SO20SO20SO205020502050205020SO20SO2050205020502050205020SO20SO2050410020502050'205020SO51205120

?w?.1 l±fi^

KtfrLimll

wn9n

o»"fwi

M Nt) BM«M< M ir •to^ U( •JJ—M mwilM tollkM D—WR rUBW W Ml ML I— r9Vf^ V9WUt ——MUlBI wH' • ——^MflBt NIfM NR&I LMlk It fTVlUt ff ——yll Itak 4llfl4— •W —llttrt •Mfl tf l pM^Mc*[ •W^^k • JIb •MJU^ R • J ^B J — • kJ •f •— •M^—L|—W^ < ^ W ^—————m • ————^^ 1 •W ••• I •Wi —pw^

, *fM>ff IliUill

Report of Laboratory AnalysisPace Analytical Servicci, Inc. • New Orleans

Single Sample • Protocol

Client ID: U2fi

ProJtCti CALL«OB13

Lab ID: JAP-OQS

DMeriptlon: .fl'-T.g't

Mrthad! Low Sofl SW M70 S^mlvol.HI. Organic.

CMmt! U.S. ARMY CORPS Or ENCP1EEHSJV.O.

Site: Hflnfi

Epiiode: JAf SunpltQu:

Matrix! gsfl % Mol»tur»; IS

Batch: 23637 Unite: UgZltf

Prep Factor: Leached: n/e Prepared; IfeSeeaZ Analysed: •Se^?? laiaIcA

CAS Number PBraiMCr

121-14-2 2.4-Diniireioloene

60i-20-2 2,6-Dinhnxoluene

1 1 744.0 Ditcoeiylphitulne11741.7 biK3-Elhylhexyl)phihil*ie

X)6-444 Fluomubene

16.73.7 Fluoror

I It'74-1 Hexichlorebenzene

17-66-3 HuwhtorebuudieneT7-47-4 H«whloreeyelop«nudi«ne

(7.72.1 HcxKhloRMlhttuIM-S9.5 lBdwo(l ^<4)pyi«ne

71.S9-1 liophoronc

91-574 2-M«ihylM»hlhalen«

95-*»-7 2'Mthylphcaol (o-Cmol)(Oi.44-5 4-Melhylphenol (p-Creiol)

9) .20.3 Naphtlrlene

li'74-4 2.NitreiiiliM(o.Niiro*nilint)

99-09.3 3.Niiro»ntliM(m.Niin»»nilin»)

100-01 •6 4-Nilioanilln* (p-NiiroiniliM)

91-9S-3 NitrobcnunoM-7S-5 2-Niirophfnol (o-NiirophtBol)10042-7 4-Nitrophenol (p-Nllrophenol)16-30-6 N-Nio«*adlph«nylunuc (Diphuylunine)

621 •64-7 N-Nitiofo-di-n-prepylunm*

17.16-S PcnuchlorophcnolIf •414 PhciunlhimcIOS-95-2 Phenol129-00-0 Pyrttit

13042-1 1 ,4-Triehlorobmxm*

95.95-4 2.4.5-Trtehlorophcnot

Sl-06-2 2.4.6-Triehlorop)»nol

M—»MMl()n«wu«

lUlBtiOl

l

J

1

1

<

1

1

1

1

j

<

1

1

1

j

1

1

1

1

<

1

J

ne) !1

ii

i

ii

<

<

i RwuK

» ND

i NDi ND

S ND? ND

i ND

i ND

i ND

S NDS NDi ND

i ND! 3S10

i ND! ND

S ND

S ND

i ND

i NO

S ND

5 NDS NDi ND

S NDS ND

? NDS ND

S ND

S ND

S ND

5 ND

Qu

D2

D2

D2

D2

D2

D2D2

D2

D2D2

D2

D2D2

D2D2D2

D2

D2

D2

D2D2D202AIOD2D2

D2

D2

D2D2

D2

D2

R«portl«|Unit

20102030

2050

20SO

2050

20SO

30)0

30)03050

3050

20502050

305020503050

3050

51205120

5120

2050205051303050

3050

5120

2050

20SO20SO2050

5120

2050

RH-Limit

•

KB taWIM Mri IIMMI—M «lhn< lk« •<|MH< IWHk| MRlkDF——MOItaU—FKkffMfV. 1W fnr FMfr MinMi fcr i MKMidM—|k il»&B f tef U—li k —^•^ fay u—J> ilaa. AttMtoB —J —taB— —l rt If •—llMktai.0«lUlfJlkr«i «ylHi M»II«»»«W <lllM« II WnMUlVtnflH.TV •itii»n r—ln •m «mr rain fc m 11 in^ f»r •«linn n* nfi <min •n in»«Mi

Report of Laboratory AnalysisPace Analytical Service!, Inc. - New Orieam

Single Sample • Protocol

Client ID: U^

Project: niTiLffffrP

Lib ID; ^At flflfl

Dncriptlon: flS.SM7.01

Method; Low San SW 8270 S.mtvol.tU. Organic*

Client: U.8. ARMY CORPS OF ENOINEEHSJV.O.

Site: BJJUU

Episode: ^AP Sample Qu:

Matrix: San % Mohture: 2fi

Batch: ^07 Unit*; usM

Prep Factor!

CAS Nuiber

•3-32-930146.1120.12.75fr-55-320S.W.23074849(S-15-0191.24.250.3M100.51-6IOI.S5-3»4g>7106-«7.»1 1 1 4 1 . 111I-<4-«101-60-15M0.191.S».79S.S7-»7005-72-3211-01-9Sl-70-311244-9«<.74.295-SO-l541.73.1106^6.791-94.112043-21446.210547.91 3 1 . 1 1 . 1534-i2.151.21.5

1.00 Leached: n/a

r Panimter

AemiphtbutAe«Mph(hylnrAndiwMB«n2o(*)anthcMentBenu(b)fluoruih«»B«nn(li)fluanuilhcn«BenzoiewidBenio(»A,i)peiylefltBcnzo(a)pymcBenzyl kleohol4-BrornophnyI ptwnyl «lhcrBuiylbcnzylphthalir4-ChJoreuillin* (p.Chloroinilinc)bi»(3-Chl<»n>clhoxy)inciti«ncbi»<2-Chlon>clhyl) elherbit(2-Chloroiioprepy1) ihn4<:hlon>-3-nrihylph»nol (p<h]ore-m<mol)Z-Chlofoniphilulcnc2-Chlorophuiol (o^hlorophcnol)4-Chlorophcnyl phcnyl elherChiyciicDib«nz(L.h)«ilhme«n«Dib«nsoflinnDi-n-buiylphthtlatc1.2-Dichloiobenune (o-Diehlorebenzene)1 •DiehlorebnzMM (m'OHhlofl)b«nz«nc)1.4-Dich)orob«nz«fli (p-Diehlontenzmc)3J'-Dichlorob«nzidint2.4.DielilorophcnolDie(hylphlkil«lc2,4.DimelhylphtnolDimcihylphlhilne4.6.Diniiro.2-mtlhylphcnol(4,6-DinHro-o<rc»ol)2.4-DinHrophenol

Prepared: 2ffi^l

MutloB R««ult

ND

—

ND

NDNDND

NDNDNDNDNDNDNDNDNDNDNDNDNONDNONDNONDNDNONDNDNDNDNDNDNONDNO

IP-?? A

Oil

'

Jialyzad: »•»

RiponinfLimit

443443443443443443

11)0443443443443443443443443443443443443443443443443443443443443S17443443443443

11101110

W-J?7 1212SIA

R«Limit

NB JiMKi K« Bmm* M *f IIM* u* •J)—i—Np«lk( MiHiW MIWM MlBlh* f*CMr *r •lum. TW (f Fia*r M—HI hf «iwr—llM —»l*J*frb^Klq U«M k m—«< br —yk ita. tteUr UJ ••Cm •utal iripfUi lt.«l«Mi—iinffc n 1*11 <M«n«rnf«o<im »n»« •oriMNpin.Iwtam r«lu. — «WM«» nHU 1(—i •mcrt lir •whr—n4 •« 4iM«» M«—plhrtlft

Report of Laboratory AnalysisPace Analytical Servim, Inc. - New Orleani

Single Sunpl* • Protocol

ClitntID: lEtlfi

Projtct: r i.n^

Lab ID: JAP-006

DMCriptton: nSJS'.lW

Method: Law SoB SW WQ SMnlvaktIk Qrp.nki

Clleat: VS. ABMyCOnPSOFENCaNEERS.N.O.

Site! NDM

Epiwde: JAP SimpliQu:

Mitrix: SeB % Mobture: 25

Batch: 23637 Unite: M/hg

Prep Factor: JiSfi. Luch«d: n Prepared: UhSeo ; Aoalyxed: ya^SOSI 12d2lA

CAS Numb«r Panmfr

121-14-2 2 -Diniln>ioluenc

M'26-2 2.6-Dinhiotolucnc117.14-0 Di-o-ociylphilulucI17.«1.7 bii(2-Elhylhexyl)phlhduc

20M44 FluonnihcBc

16.73.7 Fluorenc

111-74-1 H«x«chb?obcnxcnc

r-61'3 HcxKhlorobuudicnc77^7-A HcxKhlorocyclopenudiene(7-72-1 Hcrchloroethue

193-39-5 lndo»B(l <d)pyrene

71-59-1 luphorenc91-$7.6 2-McthylMphlkalene

t5-*«-7 l-Mfthylphmol (»<:nol)

106^4-f 4.M«lhylphmol (p-CreMi)

9) •20-3 NaphthitaMS«.74.4 2-Niuoulhrr (o-Niuoullini)

9949.2 3.Nitmni]ine(m-Nilr«wllinc)

100-01 -6 4-Nltiowdline (p-Nilroanilinc)

9145.3 Nhmteizm*M-7S.S 2-Nitrephmol (o.Nhrephenol)

100-02.7 «.Nitropbcnol (p-Nluophcool)16-304 N-Nitiofodiphenylmiine (Diphcnylinunc)

621 •64-7 N-Niuowdi'n-prepylimine

1746-5 Pcnuehlorephmol(S-01.8 Ph*n«nihmi«

IOt'95.2 Phenol12940-0 Pylcne

iaO'82-1 1,2,4-Trichlorebentent

95-9S-4 2,4 -Triehlorophenol

11-06-2 2.«4*Trichlorophcnol

DUutiftn

-

Rwull

NO

NDND

ND

ND

ND

ND

ND

NDND

ND

ND

NDNDND

ND

ND

ND

NOND

ND

ND

ND

NDNDND

ND

ND

ND

NDND

Qu

AlO

ReportingLimit

443

443443

443443

443

•43

443

443

443

443443

443

443443

443

1 1 1 01 1 1 01 1 1 0

443443

1 1 1 0

443

4431 1 1 0

443

443443443

1 1 1 0443

•

RnLimit

^

KB MMM MM OUMI M •r tftM* Ift* «DlU« HyHkq ••IL6r«M—DIMUuFUMr*(Kimi. TlMrntFMiM—MMiftri*M>milM—|kili«.

Qll •I f—N^ki •f—M JMNNfft •Hi —MMf M —— M Wf HIMrtiPf ——[— f—lk. —l J—tel MMk •i —i iv—lfJ 9vp mhuift —41 ata tf - ~

Report of Laboratory AnalysisPace Analytical Services, Inc. - New Orleani

Single Simple • Protocol

CllcniID: fil CIlMiti U.S. AttMY CORPS OF ENGINEERS Jf.O.

Project: gAV,l»0013 Site: Non«

Lab ro: JAP-MI Eptwdt: iAE Simple Qu:

Oeurtptlon: tt.O'.A.sn Matrix: Soff % Mol*tur«: 14

Method: Low Son SW gQISM TPH DlM.1 fang* Oro.nki Batch? 222& Unitt: mfi

fClP-OO

Prep Fietor; 1.00 Leached: fl Prepared: 12dSlB=22 Analyzed: 2S.8ro.97 li43 t£K

ItopTlinX R«|.CAS Number r*nm««r Dilution RMUII Qu Limit Limit

n/a TPH • Dinil Rang* Orpnici I ND 11.6

I WillBftUBflllf tPMC

ro I IMII KM DIUI M w •ftim «• BJ)wli4 n»«111« ••ILDr««MinDltwfa«Fl«lwrBlrML Tfce Nwp F——f t—ii* >f I —i •—iHr —ipHriae.• i uUBM I. BA* Ik ——^rt^ •i ^^klft •&^ J «tek •a^ ••kU—— •i l«w IfA ftB^BBJ*•i pB^Mf u—— • wr^d— ^^ •Mi — •ft • •n M —— ——wr« ^—^ n •fy—miQ«teil«MlllRh lrrtlkwllll*H*nJrfk—fc««ruifrfM«rwMluif«i«clii>——MiMn—liliMi«wi—diw»Uwirin«iwmM<»HMabic.

tOft^) II:i6;l<

Report of Laboratory AnalysisPace Analytical Service!, Inc. • New Orleani

Single Simple • Protocol

CIlMitID: 'OG9 Cli.nt! vs. Asasv CORPS OF ENGiNms.N.o.

Project:

Lib ID:

Description:

Mithod:

Prep Factor:

CA» Numb

CALL 00013

JAP-002

(M'-lM'lLow Soil SWU(CU.C14)

1.00

•r P«ram«(«r

ISM TPH DterI R»nec Orui

Leached: a/*

Site: KflHt

Ephode: JAP

Matrix: Sofi

liSL Batch: 23216

Prepared; 19.Sep.97

Dilution Ruult Qu

Sample Qu:

% Moltturt:

Ualti:

Analyzed:

R(p»nln{ R«c.Uoill Limit

•

21mg/ka

2&SfiB^2 2i32 LSK

n/i TPH • DieccI Rui{e Oi-pnic*

I —rMk«» nynil

50 13600 Dl 660

N6 *•«» MM Bm(M« •I «r thw* (IM •4«uJ n|Mlhw l—h.OrJ—MBUiillcFutWfHinei. TtemyrMurcwiibrrw-midM—fitM.• inl«|l lall li •ii rH fir ni|li ila rtniiln •nl •ilnin •in iri|i|llrili^1 PMC miN k" •pMiRC lMiMHWCMi—l N W— —I—' —H

M6<rf 1241; 11

Report of Laboratory AnalysisPace Analytical Service*, Inc. • New Orleans

Single Sample • Protocol

Client ID; :flK£ CHarti U.8. ARMY CORPS OP ENGMCElISJf.Q.

ProJect: CALL»0013 Site: None

Lab ID: JAP-003 Epiiode: J P. Simple Qu:

Dwerlptioo: (j.'- . Matrix: SoU . % Moilture; IS

Mrthod: Low Soil SW WISM TPH DIM.) R«B« Or«anl« Batch: 21Z16 Unto: nuQsa(ClO^M)

Prep Factor: 1.00 Lfched: ofi Prapandi 1M«>.97 Analysed; 2&See5Z iifiS LSK

•Iteponinx RJ|.CASNimbtr Parwifr DUuiion Rwuh Qu LInll Limll

n/« TPH-Dic*elR«ngeOrpnic» 1 362 G4 1 1 . 1

) ••r—lKlnpiriri

IW •IWM H« DWW « •r tbw «M •4«Mri Hrwdil UBil.»F4MMlMMlMrMIM*fMUML 1W fnr P-Ur •nn—hr * MMMlhH—»k ihfc&pMk| LhBh h«>TC«rt ftr——pk Ibh AMiM MM IMUllMIMMII iriffltaMt.Of—WtflfliK I—Mi —Uftntn «•«••« like* •fttriwrt.r«f»litTTr»iriii,«M4«m<»m>rtll»«rrTMM<»flK>r««»<w»«iiiir«»>«»»U^

Report of Laboratory AnalysisPace Analytical Service!, Inc. - New Orleani

Singk Sample • Protocol

Client ID: ;flK2 Client! U.8. ARMY CORPS OF ENGINEEM.N.Q.

Projtct; CALLM013 Site: BfiBfi

Lab ID: JAP.004 Epiiodc: ,tAE Sample Qu:

Oetcrlptlon: ^ '-lO.S^ Matrix: SoB %Mobture: Ifi

Method: Law Soil 8W M1SM TPH DiMri Raage Org.nl« Batch: 222tf UniU: 1010(2{£lfc£211

Prep Factor: 1.00 Leached: J^ Prepared: !Mep.»? Analyzed: 2fc5fib22 AlSfi LSK

CAS Number Paramerr

A/a TPH • D«Ml Ruf Or(Mic(1——fMJWMfMlri

R*p«nlne R«(.Dilution Ruult QN Umh LImh

5 2670 Dl 59.0

W <«»im Mniihii tuHM N gmn. 'nirnpFM«WMniiMifcriin-twUM—pl>ii«i•ipHtaf Unll b •HMri fcr—»-•IM. JUMlw |*J ••Ilin——M If •rWMkQitaC—lMm. lMriftlwlUinin«HlMl«lll«««*r«rr«M«.fir —hutfi nxM. •ii ••—• (—h k •i •HXM* fcr • H«n •H Ut «•— ni »»lh»fcl>.

Report of Laboratory AnalysisPace Analytical Servicw, Inc. - New Orleani

Single Sample • Protocol

CllrotID: Ififi Client: V.S. ARMY CORPS OF ENG1NEERS.N.O.

ProJKt: £AU.W913 Site: Kflnt

LabIDi JAP.OOS Ephodc: JAP SampltQu;

D-cription: fft-O'-?^') . Matrix: Sofi % Mobtuni IS

Mthod: faw Sa« SW S01SM TPH DImI Range Oremici Batch: UJtf UnlU; JniOtt

lO^W

Prtp Factor: 1.00 L«uh«d: Q^ Prepxnd: 19.Sgn.y7 Analysed: 2&Sfi|b2Z &12 LSK

CAS Numb«r P«r«mM«r

n/a TPH • Diesel Rinfe Oriuict

Rcponlni R«.DUuiiffl Rnult Qu Umit Uml(

5 2790 Dl 61.3

KD «MUI NM ftKMrt • •r ilww Ui* kilnu4 iWMlta* llBiLOr 4W MI—tear ul*r*(n««a. Tte Pr«r F——r *———U l*r •——ft«UM—pit lln.••w<lML—kli«unw«ter—»)»ilu.«feitlMM«BrtMM«—rllri aertk.0,kU«ulUhn. (prilh««BAn*nWlMtfllk«|rt«r«k«»«w«.

Report of Laboratory AnalysisPace Analytical Services, Inc. • New Orleani

Single Sample • Protocol

Client ID: IDIi Clienti U.S. ARMY COUPS OF ENGINEEM.N.O.

Project: CALL 00013 Site: Vast

Lab ID: ^AP-006 Epl»ode: JAP Simple Qu:

Detcrlptlon: flS.S'»17.0^ Matrix: SojB % Moiiture; 2f

Method! Low Sen SW M1SM TPH DIeMi RMM Orifntee Batchi 22^46 Unltai ffi lsfi

l£Hb£2fi2

Prep Factor! 1.00 Leached: all Prepared: 12Alt22 Analyied: 2&SfiXb2Z xlli LSIC

Reportial Rec.CAS Number Peremeier Dilution R«uh Qu Limit Lloili

ND 13.3rvi TPH • D«c*cl R«n(c Oriwici

1 ••r»»ll» Mrrcl

MD J<WM NM ftMMM M U «km ft* *«|<HM r«M*« llBk.Or iolo BOidw FMM> •r«fU««. Tbt Itw FMIW M——U fcr i MITMdK — It Utt.

» fcu viMm. HuMi mIKWn T« NO>N na* •« •ft r»«n.

Pace Analytical Services, Inc. -New OrleansLaboratory Quality Control Definitions

Our laboratory employs quality control (QC) measures to cncuro the quality of our analyticaldata by defining if accuracy and precision. Presentation of the QC data with the reportallowx the data user the opportunity to evaluate these reculu aad to gauge the methodperformance. la order to assist the understanding of these data, routine components of bur QCprogram are defined below.

BATCH • A batch is a group of 20 samples or less of a givea matrix and analysis by a specificprotocol or analytical method.

B1ANK • A method blank k a'dean'laboratory sample carried through the entire analytical.process. One or more method blanks arc prepared with each batch.of samples. The analysis ofmethod blanks demonstrates thai method interferences caused by contaminants, reagents andglassware are known and minimized. A method blank should not contain any analytes of interestabove the reporting limit. There are method allowances for common laboratory artifacts such asmethylene chloride, acetone and bis-2-ethylhexyt phthalate.

LABORATORY CONTROL SPIKE • A laboratory control spike (LCS or blank spike) Is a blankwhich hu been spiked with known concentrations of target analytes. The LCS is carried throughthe entire analytical process. One or more LCS are prepared with each batch of samples. Thepercent recovery of the spiked analyies provides a measure of the accuracy of the analyticalprocess in the absence of matrix eITeeis.

MATRIX SPIKE • A matrix spike (MS) is a client sample which is spiked with known concentrationsof largel analytes. The MS is carried through the entire analytical process. One or morematrix spikes are prepared with every batch of samples. For organic methods, a matrix spikeduplicate (MSD) is also prepared. The percent recovery of the spiked analytes provides ameasure of the method accuracy in the selected sample and matrix.

DUPLICATE-A duplicate is a sample for which replicate aUquouts are carried through (heeotire analytical process. Comparison of the original results to those of the duplicateresults provides a measure of the method precision in the sample and matrix By convention,precision is measured for inorganic analyses using a sample and a sample duplicate, whereas fororganics analyses, an MS/MSD are used.

SURROGATE • A surrogate is a noo-target analyte which is added to all samples and QC samplesprior to extraction or aaalysis. The percent recovery of the surrogate providec a measure ofthe method accuracy in each sample tested. Surrogates arc used for organics methods only.

QC LIMITS • QC limits specify the expected percent recovery range for a spiked compound. QClimits may be set by method criteria or calculated from laboratory generated data. For manymethods, these limits are advisory and do-not require corrective action if exceeded.

Report of Quality ControlPace Analytical Services, Inc. - New Orieani

Organic Protocol • Single Bitch

Mthod: .w Soil CC/MS Semlvol.tne Or«niM

PTIMCr NBHM

AecMphlhUfAccniphihytaMAnthnccn*B«nie(a)uilhnecMB<Mo(b)nuoiuih*mB«ize(k)fluomih*ntBCMPOIC Uld

B«uo(f.h.i)pciylcncB«n»(i)pymcBtnxyl ikohol4-Bromophaiyl pkcnyl elherBulylbcnzylphlhxl*le4-Chknainlline (p-CMonuniline)bi((2-Chlofeahoky)mcthuiebif(2-Chlorodhyl)cihcrbit(!-ChlereitBpiopyl) eth*r4-Chloni-3-mcihylphcnol (p-Chlore-m<iitol)2-Chloron»phih»lcnc2-Cli|orophciiol(o-Ct>lorophenol)1-Chlorpphcnyl phcnyl etherChryieneDibfnKa.htanihKCtMDIbcnzofUruDi-n-buiylplilluliH1.2-Dichlorobmune (o-Dichlorebwiiwc)1,3-Dichlorobcnxcnc (m-Dichlorebenzcnc)1,4-Oicklorobcnzene (p-Dicklorobeuene)IJ'.Dichlorobeiaidinc2.4-OiehlorephenolDilhylphihilau2.4-DlmclhyIph«nolDimethylpbdulale4.6-Diaiire-2-iMihylphenol (4,6-Dtnilro-<xpw2,1-Diniirophtnol2,4-Oinitrololuenc2.6'Dinlireiolucn*Di'H-eciylphlhalllebn(2-Elhylhexyl)phlh«liltFluonnlkcneFluemicHcxaehlorobentencHei*cklorobuudi«M

LCStplk*

166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660

LCS LCSD%R« %R«c

109190«4

101(47249<«10S375477472687S10777878587811777170S981847578715989789573 -88837611

Epbode:

Bitch:

MSSpUw %RM

166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660166016601660

2A£a'3g37

MS

7278168195

10}164789707584386667656874777082537173677065517474716949217470

12179

101797575

MID%X*c

565858617275

1-20037625255672550474552545356604052534948474356584SSS7

1-200 1-2005654936459585157

Dup .%RTO LCS MS/MSD

25* 28.137 31.1372939 1-200 1.20021 1-200 1-20028 1-200 1-20031 1-200 1-200

24 1.20036 1-20030 1-200 -20031 1-20023 1-20041 1.20028 1-20035 1*20036 1-200 1.20027 28-103 26-1033137 28-102 25-10222 1-200 1-20031 1-200 1-20028 1-200 1-20031 1-200 1-20032 1-200 1-20031 1-200 1-20037 1-200 1.20032' 28-104 28-10417 1-200 1-20028 1-200 1-2002439 1-200 1-20021 1-200 1-200

150*

28 28-89 28-8926 1-200 1.200362152"313127

Vnlu: JiadU

QC Limits

.200 1-200

-200 1-200

-200 1.200

1-200 1-200

-200 1-200t200 1-200-200 1.200.200 1-200-200 1-200.200 1-200

-200-200-200

.200-200-200.200-200

•

RPD QuMax

195050SO505050 Q1505050505050SO5030335030505050505050502750505050SOSO QlSO Ql4750SO50SO505050

• ——• nantf —U»rOC toll.Mf •Ihi •MMrul—i in •M «Mn«rf Rr •tluiim

WSVfl IWM

Report of Quality ControlPace Analytical Services, Inc. - New Orleani

Orfnic Protocol - Single Batch

Method: Low Soil GC/MS SenJ I B . I - . • • —————•

himmlw Nanr

HcuehloreeyetopmudinicHexiehlorecthanelndcM(1.2.3<d)pymuItophorene2-MRhylniphlhllcne2-Methylphmol (o-Cr»»oI)4-Mcthylphenol (p-CrwI)Ntphlhileoe2'NiUBUiiline (o-NhmtnIIln*)3-Niuouillih* (m.Niiro»niliir)4.NiireaniliM (p.Nhre»nilin»)NitfobcMMW2-Nlmphmol (o-Niirophmol)4-Niireph«nol (p-Niirophenol}

' N-NiirofodiphcDylMiine (Diphcnyliniine)N-Niiro*o^i-ft-piopyl»roiBcPeauchlorapkenolPhciBnihiencPhenolPyrtn*I^,«-Thchlorobcflunt3^^'Triehlofgphmol2^.6-Triehlorophmol

«——pM**>)n^MU4

itvo^PeQ

LCS•pik*

1MO166016«016601660166016601660166016601660166016601660166016601660166016601660166016601660

''""»"

LCS U%R*e %

uw615$

1 1 1777»

7<77

77

61126110758671

66867411711013

Epiftx

Bati

:SD MSiHM Spikt

1660i W»V

\w>166016601660166016601660166016601660166016601660166016601660166016601660166016601660

Ie: iA£

fh: 2363

MS%RM

296352

10477757472

66$7726271698467SS917299726875

2 -MSD%RK

1546427956535454514562524145

635010*575265535253

DW%RPD

64*312127323431292624151139422929

138"463241 •30-2734

UDit

QCILCS M

1-2001.2001-2001-2001-2001-2001-2001-2001-2001-2001-2001-3001-200

21-1141-200

21.12617-1091-200264035-14238.1071-2001-200

X: Ug/1^

JmlteIS/MSD

1-2001-2001-2001-2001-2001.2001-2001-2001-2001-2001-2001-2001-200

11-1141-200

41.12617-1091-20026-90

35-14238-1071.2001.200

RK> QuMix

50 Ql505050SO505050505050505050503847 Ql503536235050

Ml wlk* •wi—mllMi «n MI •Mi«md f» ••him* •MIIMI •( IW wIM wk.WM1 \'tMM

Report of Batch Surrogate RecoveryPace Analytical Service!, Inc. • New Orleans

Organic Protocol. Single Bitch

Method: l s

Lab ID

23637B1

23637B223637B321637MS

23637MSD23637S11WP-001

IWM02IWT.001

1WT-002

1WT-003

IZC-001

JAP-001JAP-002

JAP-002DLJAP-002DL2 0 D

JAP-003

JAP-003REJAP-004

JAP-005JAP'006

QCUmlu:

SurliSur2:SuritSur4!

^tIGC/MSSemiveltl

Surl%R«c

717267

65

517143

6873

7S

!«

68

630 D

0 D

SO49

736267

23-120

SS NlirobenunfrdSWl-FlirroblplunyiSST«rpk«Ayl-dl4SSPhenoMS

lie Ornnici

8ur2%Itoe

7566

7472

521241

74

7559

61

71

69

0 D

0 D

0 D

54

55887t

74

3 0 - 1 1 5

Sur6:

Rur3%R«c

IS77

9392

73

93

6116

9313

12

11

19

0 D0 D

O D90

92931094

11 • 137

Epbo

Bat

Sur«%R*«

75

7568

75

54

1253

7367

58

6871

630

0

0S1

5074

62

71

24.113 2S.U1

Surd

de; JAP

ch; 23637

SurS%ftK

70

72

6273

507648

66

5855

62

6761

D 0 D

D 0 D

D 0 D

49

46

795968

SS 2-FluorephnolSS2,4,6-Trlbramoph(Mil

SwrC%RM

1 173

70

7951

1)

4372

6254

73

6S60

O D0 D

O D71

73

10989

II

19-122

Sir 7%Rw

Surl%R*c

1^ h •M k •rQC a«hi ••• u impta «lkU*«. ii h 1*1 cuiMmo u MwnlMi.* Lib ID MMlMb| •ri MMk MINT 1U l • rffll b l •KM kMkA l«» ia •Mittel •fi k«u* uBtar •a* • • Mini 11 • LCLA Lik 10 •Ml * Ml Ulflb It I •Urti fite.« U» ID •ltt « MSB-lib b I •Mri* wDu &>pU«u-

Report of Method BlankPace Analytical Service!, Inc. - New Orleans

Orfnie Protocol • Single Batch

Lab ID: 23637B1

Deteriptlon: Law Soil Method Blank

Method: Law Sftll PC/MS Scmtvolatik QMMitt

Prep Factor! 1 Leachtdi .J |

Epiiodt: ^AE

Batch: 23637

Prepared: Qg-Sro'0?

•/•Moisture: n/a

Unite ysQsi

Analyzed: ll.Sep.97 22iaii[&

ItepoitlirLimitDilution QuCAS Numb«r Panmeur

M.32.9

201-964

120-12-7i(-SS-3205-99-2207-01-09

65-IS.O

191-24.2

(0-32.8100-S1-6101-SS-311-68-7

106-47.1

111.91.1

111-44-4lOg.60.1

Sfl.50-7

91-51.7

9S.S74

7005.73.3

2114)4$1-70.3132.A4.9

14-74-295-S0.1

S41.73.110&-46.7

91-94-1

120-13-2

1446-2105^7.9

131.11.3

S34-12.1S1.28.5121.14.3

606.20-2117.144

1 1 7 . 1 1 . 7

206^4.0

NO 4iM<M NM DMKU* N •r itaf lk* M»*Rb| UiBll.BF —MMI DUldMl fMUf,

AemapblhcncAe«n«phlhylene

AnthnctncB«n20(i)uiih]*cenc

B«nzo(b)fluai*nthene

Bmzo(k)nuonnihene

Bcraoic •eid

Biao(|JJ)pnylene

Bcnxo{i)pyicne

Bcnxyl alcohol

4'Bromophenyl ph*nyl •ih*rBu(ylbcnzylphth*l*r

4<hloroanilin« (p<:hloro«nilinc)

bi(0-Chloreethoxy)m«th»)c

b<i(2^hlero«thyt)Mh«rbuO-ChloroitopropyI) ether4.CMoro.34n«(hylpticnel (p.Chlore-ra<l«»ol)

3fhloroMphihilene2-Chlorophenol (o-Chlorophenol)

4-Chlorophenyl phrnyl ether

ChflrfntDib«iz(lJi)uihAcen«

DibenxofuruDi.n^utylpHtlul*ie

1.2'Dichlorobenune (o-Dichlorobinunc)

IJ-Diehlorobenzene (in'Dichlorobenzene)l.4.Diehtorobcnzene (p-Dichlorobenzent)

3.3'-DichlorobeMidine

2,4-Dichtofophenol

Diethylphihalu*2,4-DimnhylphmolDirneihrlphihiliic

4.ft-0inilr&-2-meihylph»nol (4,6.Dinliro«i»K)l)

2.4-Dinitrophenol

2.4-Dinllrotaluene2,6-Diniirotoluene

DJ4i«eiylpht)ulaicbi»(2.Elhylhcxyl)phthil«le

Fluonuithent

NO

ND

NO

ND

ND

ND

ND

NO

NDND

ND

ND

ND

ND

ND

ND

ND

ND

ND

ND

ND

NDNO

ND

NDND

ND

ND

ND

ND

NDND •

ND

ND

ND

NDND

ND

ND

333

333

333

333

333

333

133

333

333

333

333

333

333

333

333

333

333

333

333

333

333333

333333

333

333

333667

333

333

333333

133

133

333

333333

333

333

•IKWn •n Mteci M iki M« fikc N|MTvum n-AiM

Report of Method BlankPace Analytical Servicci, Inc. • New Orleans

Organic Protocol - Single Batch

Lab mi 2S

Method: L

Prep Factor: 1

CAS Number

8(-73.7

lll-M-l

17-61-377-47-4

67.72.1

193.39.5

7g.S9.1

91-57.6

9S-4».7

106-44-f

91 •30-38S-74-4

9949-a100414

98.95.3

g»-7S.5

10042.7

16.30-i62144-7

1746.5

15414

101-9S.2

12940-012042.19S-9i-4

•146.2

ifi2Bl«w Soil Method Blink EDl«od«: IA? % M

ow Soil GC/MS S«nivolatile OrMnici Batch: 13637

L«aeh«d: n/l Prepared: 09-Sep-97 An

PTimiT Dilutten Rmilt Qu

FIUOf»B«

HoKhlorebcMeene

HuKhlorcbutadiene

Htxwhiorocyclopcnudien*

HnKhloroeihue

lni)c«»o(l J-ed)pym»»

Iwphorene

2-Meihy1n«phth*lene

2'Mdhylphmol (frCntol)

4.McOiyIph*nol (p<i«fol)

Ntphihilene

2-Nitroiniiin* (o-Niirouiilinc)

3-Nitroanilinc (m-Niironilinc)

4-Niireinllinc tp-NHroinilinc)

Nlirobmun*2-Niirophtnol (o.Niirophenol)4*Nitrophcnel(p'NiirophcnoI) ND

N-NiireKxiiphinyluniBC (Diphenyltmin*)N-NnrotO-di-B-propyltmine ND

Penuchlorophenol

Phcnanlhrene

Phenol

Pyr«n«lA4.Triehlon)bcnzcnc2,*.5-Trichlorophcnol

2,4.6-TrichlBrepheno!

ND

ND

ND

ND

ND

ND

ND

ND

ND

ND

ND

ND

NO

ND

ND

ND

ND AIO

ND

ND

ND

ND

NDND

ND

oteture: n/»

unitt: asOsilalyxed: ll-Sm-o? 22:37 JA

KtponineLimit

333

333

333333

333

333

333

333

333

333333

133

133

833

333

333

833

333

333

133

333

333

333333

833

333

m4»iMlOil

iKMl untilM'—ttUttwnlltelL.iFMHr.

ifafMitefLtek.(««k (wMltan uc •(OMd « Uf •« •f Uc Mrwh

Report of Quality ControlPace Analytical Service!, Inc. - New Orleans

Organic Protocol • Single Batch

Epdodc

Method! Low Sell GC Eitrattable TPH ______Batch; J^________Unite: SttOSS.

PmmfrNimt LCB LCS LCSD MS MS MSD Dup QCLtadu RPD QuSplk* %R<e %Rw Spflr %RM %Itee %UD LCS MSMSD Mu

TPH.DI—IRanfOrfMici 50.0 92 50,0 B4 18 7 50.150 50.150 50

(••n**()npiruJ

•«—uinwmMUMclOCBaUfcMt «lk« igMnmibM m M< iMmwl ter ••l«w* (Mium •ru* irlkrt—|k.

Report of Batch Surrogate RecoveryPace Analytical Services, Inc. • New Orleans

Organic Protocol • Single Batch

Epiiodc: JA£

Method: LowSBUGCExfa^ttbleTPH Bitch: 25246

Lab 10 Surl Sue? Sur3 Sur4 SorS Surfi Sur7 SurB%R«c %Rcc %R*c %R«t %RM %K*c %R«e %Rw

23746BI23746B2U746S1JAP-001JAP-OOIMSJAMOIMSDJAP-002JAP.003JAP-004JAP-005JAP.006JBO-021JBO-022JBO-033JBC-024JBC-025JBC-026JBC427JBO-021

1011031051141091007710412S11210412710312268114120103119

QCUmUii SO •ISO

Sur 1: 55 n-PcnueedM

«*»rociD iair •ITI»» |—»«) h wWi «fOC ••to *« X ••>1* Oath*, irf b «« •»»MCTd M nainto*.« IJ* m——hlte( •f* kMA •—far •Uk • • •lh h I ••*•« ktekA U» 0 •u*U« 1 • kM •—Nr •kk « f •flii k » LCt.« Uft ID •la i Ml nflU h • •ufk—Ik*.4 Lik IR •tek f Mt6 llffil b • •Mrb wHu JMfltau.

Report of Method BlankPace Analytical Sarvket, Inc." New Orleans

Organic Protocol • Single Bitch

Lflb ID: 2374ml

DMcripHon; Low Son Method Blank

Method: Low SoH GC E»r«ct»blc TPH

Prep Factor: 1 L—ch«di fl a

Epiiode: JAP

Batch: 23716

Prepared: 19-S«p-97

•/oMohture: n/a

Unit*: fflgZlU

Analyzad: lS.Sae-97 ffiil2 LSX

R—orilniLbniiDUutianCAS Numbtr P«tm*l*r Rwit Qu

TPH • DIccel Rince Olfniet 10.0 NDn/»

I IMIpWMHI'

ND <(•—> N- D—cu* M M ib t ik* n^ntuf H»k,W ••MC MliUM fMi«r.M, ——I- MBph •wnki| Ltak.QllbUfMtefc (——k««dlll«fWlMtwJuik«i4«f«lKi«pri.

Report Qualifier!Pace Analytical Servicii, Inc. - New Orleair

• SiBfIc Epteode

Epiiode: JAP

Qualifier Qualifier Dicriptim

A 10 N-Nlmxodiphcnybuiune if npomd u dipheaylamlnt.

Dl The «Mly*i( wu pufemud « a dilution du» u lh« hlfb walyle eoneenuxion.

D2 The vrlyili wu pnfonncd •t • dilution du« to th« prnmcc ofnutrix infttwnei,

. 04 Oil ttnfe orpnici pmeni in the umpte nry contribute * U(h biu u the dicwl ru|C orfknict vilu* npemd.

M2 The nmplf required icoulytii du« to fainnal itindtfd reipenr ouuidc ih» QC limit*. RMiulyilt yielded (imilir rewht. indicttin( i nmpitmatrix «IT«ct. The twulu reporud ire from (he orifinil «n*ly»ii.

P2 The Mmpic •xinci could not b« coMotnted «o the method tpteilkd fin*l volume. The reponiol limli if •Icvaud •ceordm|ly.

Q I The murix fpike rccoveriec art poor. Acceptable method perfonrumce for thil analyte hu be«o d*moniBU«d by th« laboBtofy control umplencovery.

WMW \w-»

Chesi/Temp.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corpt ofEngiB—nTul» District

Project: Poplle. Inc.

Pate- /eSentl997

5^

Sample ID: ^S 61. Time: /O/O

^ ,y 5^Project POC;. KuSKt} ^W fbone:JS^Z3£&—— Pue Date;_2^JLs

CONTAINERS

filass Plastic Yiflls Cheat #_ Custody SeaLg

_ »= r_ ^J-io ?/fl7

PARAMETERS SAMPLED

•'' Semi-Volatile Organics

T?^ -3^tf.S&/ ^ACT/OfJ

^noA^\

eo/sr^

—l?•' ^7

1 '

* Containers: () " 1 L Amber Glass [ ] " 1 L Plastic { } - 40 mL Vials

CUSTODY RECORD

/\ J&®AinM»hed By Received By Date Time..£B^^y ———•——^-^fez ISJBB.^ ^ i^D^^A y/y^7 ^3:0r T

Q Bus Bill a Shipping Bill a Other No.

L«b#

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corpi ofEBgiB«enTulsa Diftriet

ProtoPopile.Ipc. (3.0'- fO.r')

Sample ID: 0^ ?______ Date: /& Sept 1997 Tune: lOS^

S'o^ProieetPOC^ftgtJ ^V< Phene: fl62.- I^Oft Due Date: 2. ^k f

CONTAINERS

glass £laai£ Ylsh Chest# Cugtedv Seal #

J. ___ 0 g?^^

PARAMETERS SAMPLED

•

^

Semi-Volatile Organics

TPH-''3>i^Se/ P^C.TfOfJ

8270A

So/fi s

^-^,) J

•

* Containers: () - 1 L Amber G l a s s [ ] - I L P l a s t i c { } " 40 mL Vials

CUSTODY RECORD / <.

wsw^K^ e^/^

,

n Bus Bill D Shipping Bill

Received By

o Other No.

Date

- ^ , -? /m47f^e^s-' »

^7 ^yW?7— / ——i"—-r-

Time/$-27^

e.?pa-o

L«bN Cheit/Temp.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Anay Carpi of EaxineertTubi Dliiriet

Pr PopHc. Inc. 6-<-&.ff')

Sample ID: €p^S' Date:/«Sept 1997

Cs-o^Time: PiS^

Project POC;. Etf/^Aflgy Phone: 6^2" 27 Og DueDate: Z>tJ_fe/

CONTAINERS

Glasa plastic Vials Chert # CttStedYSeti*

_L Z=- =- u1^ ^^7

^PARAMETERS SAMPLED

^1 Semi-Volatile Organics 8270A |^/ Yo^

* Containers: () - 1 L Amber G l a s s [ ] - ILP las t ic { } " 40 mL Vials

CUSTODY RECORD

Received By DateV/6^7

Time/SOP

e^a.

a Bus Bill 0 Shippine Bill D Other No.

Lab« Chest/Teap.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corp* ofEaciBtnTolu Dbtriet

Project: Popile. Inc. , /(9^-/o.&

Sample ID; <yi<?_______ ^Sate: W Seat 1997 Time: S^SOSL

ProjectPOC:^»^c«i ^ft^ phone: Ce^-ftfcl»g70g Due D>te:_JLafe^

CONTAINERS

Glass Plastic Vials Chest # Custody Seal»

-L -^ 11 ^fl7VOA Chest Simpler -^

PARAMETERS SAMPLED

l

•

» Containers: () - 1 L Amber Glass [] •B 1 LPlaslic {

Semi-Volatile Organics

T?H^wJ ^KM-rOJ

8270A

eois'm.

- 40 mL Vial

r-H'3

s

Received By Time/g-oo

a Bus Bill DShippmeBill o Other No.

Llb# Chert/Temp.

Soil SAMPLESCHAIN OP CUSTODY

U.S. Army Corpi ofED|iBecnTuba District

Project; Popilt,to._ ^6.0'-7,5-^

Sample ID: i T^ ______ Date: ASfiBLlS21

Project POC:luJ86&2-J ±--- Phone:. gVg2-7.70fi Due Date:_^_M^

CONTAINERS

Glass Plastic Vials Chest # guitodv Seal #

_1 __^ J=: ••70 ?/87

PARAMETERS SAMPLED

^

^r

' cmi-Volatile Ortanies

rPf4 -Dr^e/ ffAWGAJ

8270A

e^y^^>fyo

1 l

n, A^Upq"18*1®'1 sy

%</ ^c

-

A

Received By

J>^^

/ Dye

y/ff/^r^^ r ^/»y^p

Time/?&<»

^ya-c>•

o Bus Bill D Shipping Bill o Other No.

Cbeit/Temp.

Soil SAMPLESCHAIN OF CUSTODY

U.S. Army Corpi of Engineer*Tuba District

Projectiffflllt. faC. (/S.S-'-P.o')

Sample ID: J 2)/^______ Date: 2£LSSELlS22———— Time: 35"

Project PQg-?LtBg^ ^AggY Phone: 'gfe2'2708 Due Date: Z^m^L

CONTAINERS

filas Stasis. Yifila chest # Cu^vSgrf^

J_ rL ^^^ ^fg7

PARAMETERS SAMPLED

^>

&•

"Semi* Volatile Organics

'TPH-'Df&se.f

8270A

80/5-^-

^,1 ^y ' ^

• Containers: () - 1 L Arobcr Glass [ ] - 1 L Plastic { } - 40 mL Vials

CUSTODY RECORD ./ ,.(^•^/^

Received By Time^£7 JLSSs?

'^er ^V^ . ^g=^

a Bus Bill o Shipping Bill a Other No.