# 347944- RECEIVED OPPT CBIC



## 2012**H~'?** 

## 16**t\t~** 

## 10: 35

August 15, 2012

VIA FEDERAL EXPRESS

TSCA Document Processing Center (7407M) EPA East- Room 6428 U.S. Environmental Protection Agency 1201 Constitution Avenue, NW Washington, D.C. 20004-3302 Phone: 202-564-8940

Attn: EPA Docket ID Number OPPT-2003-0012

Re: Supplement to Document ID Number OPPT-2003-0012-1294Andrea V. Malinowski Corporate Counsel

DuPont Legal Wilmington Office Buildings 1007 Market Street Wilmington, DE 19898 302-774-6443 Tel 302-774-4812 Fax andrea.v.malinowski@usa.dupont.com E-mail

Final Report- Pascagoula, MS Follow-Up Study re Monitoring of Perfluorinated Chemicals in Environmental Media and Biota

Dear Sir/Madam:

Please find attached, for inclusion in EPA Docket ID Number OPPT-2003-0012, and any other applicable docket, a copy of the above-identified final report.

This submission supplements information previously submitted to the above-identified docket and referenced by Document ID OPPT-2003-0012-1294. The documents provided with this submission have also been submitted under separate cover to the TSCA 8(e)/FYI Office.

Please contact me directly if you have any questions or require further clarification.

Very truly yours,

Andrea V. Malinowski

Enclosures



### • 

## • Letter from First Chemical Corporation to Mississippi DEQ- (2 pages) Pascagoula Follow Up Study- Final Report- (31 pages)



# AUG 23 2012

CONTAINS NO CBI

E.l. du Pont de Nemours and Company1001 Industrial Road Pascagoula MS 39581-3237 USA

PO. Box 7005 Pascagoula. MS 39568-7005 USA

228 762-0870 Fax: 228 769-5355 

# ©, First 

# Chemical Corporation

A DuPont Company

August 13,2012

CERTIFIED MAIL No. 7008 3230 0002 0880 9314 

### RETURN RECEIPT 

### REQUESTED

Ms Carla Brown, P E. Chemical Branch Manager Environmental Permits Division Office ofPollution Control Mississippi Department of Environmental Quality P 0. Box 2261 Jackson, MS 39225

Re: Results of monitoting for perfluorinated chemicals in environmental media and biota
at First Chemical Cotporation, Pascagoula MS

Dear Ms Brown,

A multi-yeat monitoiing program for petfluoiinated chemicals in environmental media and biota was recently completed by the Gulf Coast Research Laboratory on behalf ofthe First Chemical Corpmation (FCC), a DuPont Company.. The program was designed to evaluate concentrations ofpedluorooctanoic acid (PFOA) and perfluotohexanoic acid (PFHxA) in environmental media and biota at several time points: in 2006 (representing environmental background concentrations prior to start-up of a new fluorotelomer alcohol pmification unit) and in 2008 and 2010 (two and four years after start-up}. A copy of the report is included for yo ill' reference.

Monitoting within the boundruies of the FCC site included storm water runoff; groundwater and effluent and sludge from the on-site wastewater treatment plant. Offsite surface water srunples were collected from the rivers, bayous, and bays adjacent to FCC facility as well as from local inigation water and industrial water.. Marine biota sampled included two fish species (hardhead catfish and speckled trout) and one invertebrate species (blue crab).

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1- l IPFOA and PFHxA were detected in all three on-site monitming wells (MW17, MW28 and MW 6.3) with variable concentration trends exhibited dming the 2006-2010 period of sampling. Tluee additional on-site sampling locations (i e. water and sludge from the
wastewater treatment plant and storm water mnoff) showed downward concentration trends over the four years of sampling. The nondetectable-to-low initial background concentrations ofPFOA and PFHxA in environmental waters and biota did not show any discernible temporal changes in concentration

..
Overall, the results of this monitming program indicate that the nmmal opetation ofthe FCC facility results in low, but detectable concentrations ofPFOA and PFHxA in storm water runoff and surficial groundwater immediately beneath the plant. Based on the data fi'om this monitoring progtam, there is little or no impact of the FCC operations on background concentrations in the surface waters or biota in the environment surrounding the plant.

I o control off-site movement of groundwater impacted by othet chemicals beneath the plant site, FCC is cunently operating its groundwater recovery trench system which establishes a groundwater captme zone which extends under the plant boundaries. This system will also serve to capture and remove PFOA and PFHxA from groundwater, effectively reducing the concenttations which are eventually discharged into actjacent surface water bodies

Periodic on-site monitming ofPFOA and PFHxA are planned to help evaluate ongoing effmts to improve process operations and to demonstrate approptiate envimnmental stewardship.

Sincerely,

Whit Griffin Plant Manager First Chemical Corporation Pascagoula, MS

Enc: Pascagoula Follow-Up Study: Final Repmt June 10, 2012

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# Pascagoula Follow Up Study Final Report

Prepared For First Chemical Corporation Pascagoula, Mississippi By Kevin Dillon, PhD University of Southern Mississippi Gulf Coast Research Laboratory June 10, 2012

## TABLE OF CONTENTS

INTRODUCTION Purpose of environmental monitoring studies 3 WATER SAMPLING SITES AND METHODS 4 Surface waters: Rivers, Bayous, Grand Bay, and Mississippi Sound 4 Effluent samples 4 Irrigation water samples 5 Industrial water sampling 5 Storm water samples 6 Groundwater sampling 6 POTW sludge Sampling 7 BIOTA SAMPLING SITES AND METHODS Fish sampling sites and methods 7 Invertebrate sampling sites and methods 8 WATER, SLUDGE, AND BIOTA ANALYTICAL METHODOLOGIES 9 WATER RESULTS Surface waters: Rivers, Bayous, Grand Bay, and Mississippi Sound 10 Effluent samples 11 Irrigation water samples 11 Industrial water sampling 11 Storm water samples 12 Groundwater sampling 12 POTW sludge Sampling 13 BIOTA RESULTS Fish samples (hardhead catfish and speckled trout) 13 Invertebrate samples (blue crab) 14 DISCUSSION AND CONCLUSION 14 LITERATURE CITED 18 TABLES Table 1. 2008 surface water sampling locations, date, times, and tidal stages 22 Table 2. 2010 surface water sampling locations, date, times, and tidal stages 23 Table 3. Water quality parameter results measured for each station. 24 Table 4. PFOA and PFHxA concentrations from water sampling sites. 25 Table 5. Biota sample names, numbers, and lengths for 2006 and 2008 26 Table 6. PFOA concentrations for fish samples collected in 2006 and 2008. PFHxA concentrations for fish collected in 2008 27 Table 7. PFOA concentrations for invertebrate samples collected in 2006 and 2008. PFHxA concentrations for blue crabs collected in 2008 28

FIGURES Figure 1. 

### Follow Up study sampling locations. 29 Figure 2. Ground water sampling locations at First Chemical Corp. 30 Figure 3. PFOA concentrations vs. salinity for all surface water samples. 31

2INTRODUCTION PFOA was first manufactured in the late 1940's and has been used in manufactured products that have a variety of applications ranging from providing water and oil repellency for a multitude of surfaces (clothing, furniture, floor waxes, etc) to its

use in aircraft production, electronics, and other items such as personal care products. The manufacturing of fluoropolymers uses PFOA (generally as the ammonium salt

- APFO) as a processing aid and has resulted in the largest historical source ofPFOA in the environment, corresponding to**~85%** of all emissions (Prevedouros et al., 2006). Emissions associated with the production ofPFOA and degradation of various precursors correspond**to~** 12% and**~3%** ofhistorical emissions, respectively (Prevedouros et al, 2006). An additional potential source ofPFOA is the biodegradation ofprecursors in
wastewater treatment plants (Sinclair et al., 2006) although increases in effluent concentrations are not always observed (Schultz et al., 2006). Several industrial processes involving polyfluorinated chemicals exist at First Chemical Corporation (FCC): a process to purify fluorotelomer alcohols and processes to manufacture surfactants and ingredients for fire-fighting foam. Local environmental detections ofPFOA in sludge, water and biota can potentially result from industrial emissions of one or more ofthese processes to air, water or soil.

Purpose of environmental monitoring studies The purpose ofthe original First Chemical Corporation (FCC) Pascagoula Baseline Study performed in 2006 was to conduct one sampling event to analyze for perfluorooctanoic acid (PFOA), and to provide a "snapshot" ofthe environment in various media (water, sludge, biota) prior to the startup of a new fluorotelomer alcohol purification operation at the First Chemical site in Pascagoula. The study measured environmental concentrations of both PFOA and perfluorooctanesulfonate (PFOS). PFOS was included in the Baseline study to indicate background levels ofperfluorinated compounds not associated with FCC Pascagoula. The purpose ofthis follow-up study is to monitor for the presence ofPFOA to evaluate whether there have been changes in PFOA concentrations over time in local
waters and biota. Because the manufacturing of 8-2 fluorotelomer alcohol (FTOH) and other chain length alcohols (both longer and shorter) is currently being phased out and being replaced by a process that exclusively produces 6-2 FTOH, analysis of perfluorohexanoic acid (PFHxA) was added to the follow-up study. PFHxA is both a potential low level impurity and degradation product of 6-2 FTOH. We have developed and implemented a 3-year plan to generate scientifically sound data to identity and monitor changes in environmental concentrations ofPFOA and PFHxA consistent with the original FCC Baseline Study. Water and sludge samples were collected in 2008 and 2010. Biota samples (fish and crabs) were collected in 2008. All sample types are collected at the same locations as the Pascagoula Baseline Study conducted in 2006 so direct comparisons can be made. The results presented in this report are from water and sludge samples collected during the years 1 and 3 of the study period (July to August in both 2008 and 2010) as well as biota samples collected during 2008. The PFOA results will be compared to those from the Baseline study conducted in 2006 as well as to the results of similar studies conducted at other locations to put our results in a more global context. As described above, water and sludge samples collected

3in 2008 and 2010 were also analyzed for PFHxA to provide background concentrations of this perfluorinated compound prior to replacement of 8-2 FTOH (containing longer and shorter chain lengths) with 6-2 FTOH in the First Chemical telomer-based products.



### WATER SAMPLING SITES AND METHODS All sample bottles used for sample collection were prepared by the contract laboratory, sealed to ensure cleanliness and shipped to GCRL. Sample bottles were not cleaned or reused in the field. To ensure against cross-contamination between surface
water sampling locations, the individual collecting the surface water samples wore clean, disposable latex and/or nitrile gloves and avoided direct contact with the sample water.



### Samples from Rivers, Bayous, Grand Bay, and Mississippi Sound Surface water samples were taken from the Pascagoula and Escatawpa Rivers, Bayou Cassotte, Grand Bay and the Mississippi Sound. Figure 1 shows the sampling locations and Tables 1 and 2 provides each sampling location's geographic location (latitude and longitude) and the time and date of each sampling event. Samples were taken during flood and ebb tides at each location. Sample bottles were prepared by the contracted laboratory, sealed to ensure cleanliness and shipped to the University of Southern Mississippi's Gulf Coast Research Lab (GCRL). Sample bottles were not cleaned or reused in the field. To ensure against cross-contamination between surface
water sampling locations, the individual collecting the surface water samples wore clean, disposable nitrile gloves and avoided direct contact with the sample water. Surface water samples were collected as grab samples at approximately mid-stream and mid-depth using a pre-cleaned acrylic horizontal Beta water sampler (Wildco part number 1940-064). Before the 2008 sampling campaign began, the new Beta sampler

was soaked in a recirculating seawater tank for 1 week to leach out possible contaminants. The Beta sampler was then cleaned with "Neutrad®" laboratory soap, rinsed three times with deionized water and then rinsed with ethanol (per the protocols used in the 2006 study) prior to sample collection. Water depth and basic water quality parameters (temperature, pH, oxidation-reduction potential [ORP], turbidity, dissolved oxygen [DO], and salinity) were measured at each station for 2008 and 2010. While collecting water, the open sampler was lowered to the desired depth and then held there for several minutes before being closed to insure that the sample was representative of the desired water depth. After collection with the Beta sampler, a water sample was transferred into a 500 ml pre-cleaned and pre-labeled Nalgene bottle and stored on ice in

a cooler. The chain of custody (COC) form was then completed, and entries were made in the field log indicating the time of sample collection. Water samples from 2008 were shipped to MPI Research for analysis ofPFOA and were also sent to Axys Analytical Services, Ltd. (AXYS, in Sidney BC Canada) for PFOA and PFHxA analysis as described below. Samples from 2010 were shipped only to AXYS for PFOA and PFHxA analysis as described below.



### Effluent samples Samples were taken from the Pascagoula POTW effluent discharging to the Pascagoula River (Figure 1). The samples were taken at a point before the effluent mixing with the water of the Pascagoula River on August 18, 2008 (08:01 to 8:49am)

4and on August 21, 2010 (10:20 am). To ensure against cross-contamination between effluent water sampling locations, the individual collecting the surface water samples

wore clean, disposable nitrile gloves and avoided direct contact with the effluent sample
water. Sample bottles were prepared by the contracted laboratory, sealed to ensure cleanliness and shipped to GCRL. Sample bottles were not cleaned or reused in the field. This sample was a single, discrete grab sample and was collected by submerging the sample bottle below the water surface and unscrewing the bottle cap. The bottle was then filled by turning the bottle parallel to the water surface and slowly rotating so that the mouth of the bottle is up right. This procedure ensures that a representative sample ofthe surface water, excluding water from the surface microlayer, will be pulled into the sample bottle. The bottle was then recapped while under water then stored on ice. The COC form was then completed, and entries were made in the field log indicating the time of sample collection. Another effluent sample was taken at the FCC Pascagoula site from water discharged from the site to the POTW. This sample was a composited sample taken from
water collected from the effluent stream over a 24-hour period. Due to limited access of GCRL staff to the FCC site, the composite sample was provided to the GCRL field technicians by First Chemical Corporation as a valid QA/QC split from the weekly monitoring composite sample FCC #1-7176. Effluent water samples were stored on ice after collection. GCRL technicians picked up the samples on August 13, 2008 at 17:20 and on August 12,2010 at 10:05. The COC forms were then completed, and entries were made in the field log indicating the time of sample collection. Effluent water samples from 2008 were shipped to MPI Research for analysis of PFOA and were also sent to AXYS for PFOA and PFHxA analysis as described below. Samples from 2010 were shipped only to AXYS for PFOA and PFHxA analysis as described below.

Samples from Irrigation Water Samples of irrigation water were taken from the West Jackson County Landfarm. The water derived for irrigation originates from the effluent of the Ocean Springs Wastewater Treatment Plant and is not associated with or connected to the Pascagoula
water supply or the Pascagoula POTW. The 2008 sample was taken directly from a water faucet at the Landfarm on July 31,2008 between 13:20 and 13:50. The 2010 sample was collected on September 1, 2010 at 10:22 from a water holding pond as the faucet used in 2008 was not available. Both samples were stored on ice immediately after collection. The COC forms were then completed, and entries were made in the field log indicating the times of sample collection. Water samples from 2008 were shipped to MPI Research for analysis ofPFOA and were also sent to AXYS for PFOA and PFHxA analysis as described below. Samples from 2010 were shipped only to AXYS for PFOA and PFHxA analysis as described below

Samples from Industrial Water Water samples of industrial water supplied by the Jackson County Port Authority

were collected directly from water taps into pre-cleaned and labeled sampled bottles on July 31, 2008 (11 :02 to 11: 17) and on August 12, 2010 (1 0:22) then stored on ice. The COC form was then completed, and entries were made in the field log indicating the time of sample collection. Industrial water samples from 2008 were shipped to MPI Research

5for analysis ofPFOA and were also sent to AXYS for PFOA and PFHxA analysis as described below. Samples from 2010 were shipped only to AXYS for PFOA and PFH:xA analysis as described below.

Samples from Storm-Water Storm-water samples were taken during the discharge of storm water from a stormwater trough at FCC Pascagoula before the stormwater drained to the Mississippi Phosphate drainage channel on August 11,2008 between 15:08 and 15:22 and on August 12 at 9:29. Samples were collected by submerging the sample bottles below the water surface and unscrewing the bottle caps. The bottles were then filled by turning the bottle parallel to the water surface and slowly rotating so that the mouth of the bottle is up right. This procedure ensures that a representative sample of the surface water, excluding water from the surface microlayer, will be pulled into the sample bottles. The bottles were then recapped while under water then stored on ice. The COC form was then completed, and entries were made in the field log indicating the time of sample collection. Storm water samples from 2008 were shipped to MPI Research for analysis of PFOA and were also
sent to AXYS for PFOA and PFH:xA analysis as described below. Samples from 2010

were shipped only to AXYS for PFOA and PFHxA analysis as described below.

Groundwater sampling On-site groundwater was sampled from the first groundwater-bearing unit in the vicinity ofthe new chemical process unit on July 30, 2008 and August 12, 2010. Chosen sample locations included monitor wells MW-17, MW-28, and MW-63. Figure 2 shows the locations of the pre-existing monitor wells used for the Follow Up Study. Sampling

was conducted at monitor wells MW -17 and MW -63 because of their proximity to the

new chemical process unit. Sampling was conducted at monitor well MW-28 because it is down gradient of the new chemical process unit. Prior to sampling, monitoring wells

were purged of three well volumes using a peristaltic pump with aged and pre-cleaned Tygon tubing prior to monitoring field parameters for stabilization. Total well depths
necessary to calculate the required purging volume were tabulated and accompanied the sampling team in the field. During well purging, pH, specific conductance, turbidity, dissolved oxygen, salinity, oxidation/reduction potential, color, odor, and temperature

was measured at regular intervals until stabilization was reached, which was always achieved prior to the purging of three well volumes. Stabilization was considered achieved when three consecutive readings of each indicator parameter, taken at three to five minute intervals are within the following limits:

• pH(+/- 0.1 units)

• specific conductance (within 3%)

• turbidity (10% for values greater than 5 NTUs)

• temperature (within 3%) These parameters were measured with a YSI model 600XLM sonde which was calibrated daily before use. None of the wells sampled were pumped dry during the purging and sampling. Once purging was complete, the well was sampled through the discharge tubing of the pump by directly filling the laboratory-supplied pre-labeled sample containers. Sample containers were filled to at least the container shoulder. Sampling times for wells MW-17, MW-28, and MW-63 on July 30,2008 were 13:21, 13:40, and

612:52, respectively. The same wells were sampled on August 12, 2010 at 09:19, 09:45, and 08:50, respectively. After the sample containers were filled, they were sealed and immediately stored on ice. The COC form was then completed, and entries were made in the field log indicating the time of sample collection. Ground water samples from 2008

were shipped to MPI Research for analysis ofPFOA and were also sent to AXYS for PFOA and PFHxA analysis as described below. Samples from 2010 were shipped only to AXYS for PFOA and PFHxA analysis as described below.

POTW Sludge Sampling The objective of the testing is to determine concentrations ofPFOA and PFHxA in the sludge two and four years after the start up of a new process to purify 6-2 fluorotelomer alcohol at FCC. The general location of the sludge sample is shown in Figure 1. Samples were collected from the sludge on August 18,2008 (08:15) and August 21, 2010 (10:35). Appropriate personal protection equipment such a nitrile or latex gloves

were worn at all times samples were handled to avoid contamination of the samples during collection and during preparation for shipping to the laboratory for processing and analysis. In addition, sampling equipment was pre-cleaned and decontaminated between sample collections with 10% hydrochloric acid and deionized water to avoid contamination. Sample collection activities were documented in the field with notes in a logbook. Composite samples of sludge were obtained from the top 12 inches at the sample location. The composite samples were placed in a clean aluminum mixing bowl and homogenized in the field. The required volumes were then placed in the sample bottles and prepared for shipping to the laboratory using standard soil sample protocols. The samples were shipped to AXYS for processing of PFOA and PFHxA analysis as described in the following section.

FISH SAMPLING SITES AND METHODS During the baseline study conducted in the summer of 2006, hardhead catfish and speckled trout were collected at both study sites. These target species can usually be found at the two sample sites (Mississippi Sound and Grand Bay). Hardhead catfish are bottom feeders that prey on crabs, fish, shrimp and detritus along the bottom of the bays and bayous where they live. Speckled trout are a recreationally important fin fish in the northern Gulf ofMexico and associated estuaries and is pivotal to the coastal economy of this region. They are important secondary consumers in the coastal ecosystem that show

a high degree of spatial and temporal flexibility in their diet (Roese and Moore 1977). Descriptive data suggest that speckled trout (C. 

### nebulosus) utilize benthic and pelagic trophic pathways but that the relative importance of these two pathways is highly variable both seasonally (Scharf and Schlicht 2000) and spatially (Overstreet and Heard 1978, Llanso et al. 1998, Scharf and Schlicht 2000). To determine the PFOA concentrations in the tissues of local biota, large and small specimens ofhardhead catfish 

### (Ariasfelis) and speckled trout 

### (Cynoscion nebulosus) were collected and analyzed. These species provide targets that should be readily found at most times in these two sites and tissue data in hardhead catfish can be compared across time to results of the 2006 baseline study.

7Fish were collected with gill nets that were placed in the water and left for 2 hours. Target fish were removed from nets as carefully as possible and placed in a holding vessel (ice chest, bucket, etc.,) on the boat. By-catch species or fish not meeting the minimum size objective were returned to the water as soon as possible to avoid injury. Once collected and determined to be an acceptable sample for retention, fish were euthanized with MS222. Selected whole fish samples placed in ZiplocTM bags, labeled, and place on ice until tissues were processed (filleted). Once tissues were isolated into the appropriate samples they were placed in zip lock bags, frozen on dry ice, and shipped overnight to the receiving laboratory under proper chain-of-custody. Sampling was complete when the target number of fish had been collected. Fish sampling was conducted in Mississippi Sound and at the Grand Bay National Estuarine Research Reserve (NERR) for the presence ofPFOA and PFOS in fish to compare with results of the baseline study conducted in July 2006. Fish samples were taken in Mississippi Sound as close as possible to 0.5 miles beyond the mouth of the Pascagoula River and within 1000 feet ofthe position of the sampling conducted during the PBS. The coordinates of the Mississippi Sound fish sampling reported in the baseline study report were 30.32751N and 88.56678W and the coordinates ofthe 2008 sampling location was 30.32769N, 88.56668W. These two locations are within 25m of one another. Fish samples were also taken in the Grand Bay NERR at a location agreed with NERR staff. The fish sampling in the Grand Bay NERR in the earlier baseline study was conducted at coordinates 30.35722N and 88.418056W and the 2008 sampling was conducted at the coordinates 30.35761N, 88.41774W. The two sampling locations are within 55m of one another. Existing fish and invertebrate collection permits at the University of Southern Mississippi's GCRL were used for this study. The primary objective of the fish-sampling program was to determine any concentration of PFOA and PFOS in fish tissue. To fulfill this objective, replication of tissue samples were collected. Six samples of the selected fish species (catfish and speckled trout) were collected. Three samples of each species were of smaller fish (approximately 9" to 14" total length) and three samples will be oflarger fish (approximately 14" and 17'' total length). In addition to fillets, the viscera, skin and remaining carcass were also combined from each fish, and analyzed for the presence of PFOA. Samples less than 10 grams in mass were not analyzed and fillets, combined viscera, skin and carcass samples were not composited. Fillets do not include skin. Skin

was included as part of the combined viscera and carcass samples. Analyzing the fillets, the combined viscera, skin and carcass separately provides an indication of where PFOA and PFOS partition in vivo, ifPFOA and PFOS were present in fish at all. In summary, two tissue types were analyzed for PFOA from each fish sample: fillets and carcass (including viscera, liver, and skin). The fillets samples and combined viscera, skin and

carcass samples from each fish were collected and then frozen. The COC forms were then completed, and entries were made in the field log indicating the times of sample collection. Fish samples were shipped on dry ice to AXYS for PFOA and PFHxA analysis as described below.

INVERTEBRATE SAMPLING SITES AND METHODS The blue crab 

### (Callinectes sapidus) was sampled in Mississippi Sound and Grand Bay NERR for the presence of PFOA in an invertebrate species in the areas around First

8Chemical Corporation. To fulfill this objective, six samples ofthe target invertebrate species (blue crabs) representing a range of sizes were collected at the sample location. Samples were taken in the Mississippi Sound as close as possible to within 0.5 miles beyond the mouth of the Pascagoula River. Every effort was made to conduct the sampling within 1000 feet of the proposed sampling location. Invertebrate samples were also taken in the Grand Bay NERR at a location agreed with NERR staff. The blue crab (Callinectes sapidus) was used as the target species as it is an inhabitant of the proposed sites and was successfully collected from these sites during the baseline study. Blue crabs have been harvested in Mississippi for hundreds of years and spend a portion of their lives in brackish-water areas of the Mississippi Sound. Blue crabs are omnivorous and feed on both plants and animals, including marine worms, snails, fish, seaweed, and marsh grasses. Blue crabs represent important seafood for recreational fisherman and
must be five inches or larger as measured from the tip of one lateral spine across the back ofthe shell to the tip of the opposite lateral spine to be harvested legally according to Mississippi law. Blue crabs were collected with a crab trap baited with raw chicken that was deployed over a tidal cycle. Crabs were assessed for proper sample size and if acceptable placed directly on wet ice in chest on the boat after collection. By-catch and crabs not meeting the minimum size objective were returned to the water as soon as possible to avoid injury. Following separation of soft tissues samples were placed in ZiplocTM bags, labeled, frozen on dry ice, and shipped overnight to the AXYS analytical laboratory under proper chain-of-custody. Samples were maintained on ice and transferred using overnight courier to the analytical laboratory under proper chain-of-custody.

WATER, SLUDGE, AND BIOTA ANALYTICAL METHODOLOGIES The PFOA and APFO analytical methods used for the first analysis in 2008 is a validated liquid chromatography-tandem mass spectrometry (LC/MS/MS) aqueous method developed by Exygen Research of State College, Pennsylvania (OPPT-2003- 0012-0040). Analysis was conducted by MPI Research in State College, Pennsylvania. The method used initially had a limit ofquantitation (LOQ) of0.012 ng/mL and a limit of detection (LOD) of 0.0023 ng/mL in water. Water samples for 2008 were also analyzed at AXYS for PFOA and PFHxA analysis with an improved analytical method with lower detection limits. Water samples for PFOA and PFHxA from 2010 were run only analyzed at AXYS. The LOD and LOQ for both PFOA and PFHxA with the more sensitive method ranged from 0.99 to 1.9 ng/L for PFOA and 1.0 to 1.4 ng/L for PFHxA. Sample preparation, instrumental analysis and analyte quantification procedures were in accordance with AXYS Method MU-060 ''Analytical Procedure for the Analysis of Perjluorinated Organics Compounds in Aqueous Samples by LC/MS-MS". Accurately weighed sample (approximately 500 g) was spiked with Be-labelled quantification standards, extracted and cleaned up using SPE cartridges. Target analytes were collected in basic methanol. After spiked with labeled recovery (internal) standards, the extract was analyzed using HPLC-MSIMS. The final
extract volume was 4 mL. Analyte concentrations were determined by isotope dilution/internal standard method, comparing the area of the quantification ion to that of the 13-labelled quantification standard and correcting for response factors. Quadratic

9quantification equations with 11X weighting fit were determined from a multi-point calibration series prepared alongside with the sample in an identical manner. PFOA Samples analyzed by each method gave nearly identical results when compared (slope=l.01, n=0.9961) therefore both sets ofPFOA measurements are presented here. Sludge sample preparation, instrumental analysis and analyte quantification procedures were in accordance with AXYS Method MLA-041: Analytical Procedure for the Analysis of Perfluorinated Organic Compounds in Solid Samples by LC-MSIMS. Accurately weighed sample (approximately 59g dry) was spiked with 13 C-labelled quantification standards and extracted in acetic acid and basic methanol. The extract was cleaned up using SPE cartridges and carbon. After spiked with labeled recovery (internal) standards, the extract was analyzed using HPLC-MS/MS. The final extract volume was 4 mL. Analyte concentrations were determined by isotope dilution/internal standard method, comparing the area of the quantification ion to that of the 13 C-labelled quantification standard and correcting for response factors. The analytical methods used for PFOA were validated LC/MS/MS tissue methods. The target LOQ for the analytical methods will be 5 ng/g for fish samples. The actual LOD for this study was 1.9 to 2.5 ng/g. Biota samples were also analyzed for PFHxA, using a validated method involving LC/MS/MS.

WATER RESULTS

Samples from Rivers, Bayous, Grand Bay and Mississippi Sound Physical data for all surface water stations for 2008 and 2010 are presented in Table 3. Salinities ranged from near fresh (0.4) to near marine values (31.4) and were highest at each station during flood tide. Values for 

### pH ranged from 6.55 to 8.32 with the lowest values measured in fresh water stations and the highest in more marine waters. This variation in pH is common for estuarine systems; similar values have been obtained in the Grand Bay National Estuarine Reserve, just to the east of Pascagoula (Dillon and Walters, 2008). Water temperatures were between 25.1 and 32.8 

## oc during the 2008 sample collection surveys. Higher temperatures were recorded during the 2010 sampling
surveys and ranged from 30.87 to 33.72° C, Lower water temperatures were typically observed at each station during the flood (high tide) samplings conducted during the evening or early morning hours. Turbidity values for surface water sites ranged from 2 to 33.4 nominal turbidity units (NTUs). The lowest turbidity values were found at the river stations, which are more sheltered from the wind by tree cover. The higher values were at the more open stations near and in the Mississippi Sound, where turbidity is wind driven (Dillon and Walters, 2008). Dissolved oxygen (DO) concentrations ranged from hypoxic (1.73-1.92 mg/L) at the river stations during flood tide to near saturation (7.06 mg/L) at Bayou Cassette during the ebb tide sampling. With the exception of the Grand Bay NERR sample site, all stations had higher DO concentrations during the flood sampling due to the time at which the samples were collected. Sampling at flood tide was conducted at night or in the early morning when respiration dominated the oxygen pool and phytoplankton were not producing oxygen. Such diel fluctuations in DO concentrations are common in aquatic systems. All surface water samples from the Pascagoula River, Escatawpa River, Bayou Cassette, Grand Bay, and the Mississippi Sound were below the PFOA LOD (2.3 ng/L)

10with the initial analytical technique in 2008. Upon further analysis at AXYS, surface
water samples were found to range from 1.2 to 3.0 ng/L with the highest concentrations observed at low to intermediate salinities (0 to 24) while the lowest concentrations were observed at highest salinities (Figure 3). Above a salinity of 24, there was a negative correlation between PFOA concentration and salinity (r2=0.60), which is most likely due
to the dilution ofPFOA with seawater of lower PFOA concentrations. PFHxA concentrations were very low in all surface water samples (<1.0 to 3.8 ng/L.) and concentrations that were detectable decreased from 2008 to 2010. During 2008, three of the twelve surface water stations were below the LOD while in 2010, eight of the twelve were lower than the LOD. All four surface water stations that had detectable concentrations of PFHxA during 2010 were slightly lower than that measured previously.

Samples from Effluent The effluent samples taken at the FCC Pascagoula site which discharges from the site to the POTW had an average PFOA concentration of43 ± 1 ng/L in 2008. The errors shown are the deviation from the mean between laboratory duplicate samples that were split from the original sample during analysis. A field duplicate sample was also collected from the FCC effluent and had a similar PFOA concentration of 49 ng/L. The average PFOA concentration ofboth field samples from the FCC effluent was 46 

### ± 3 ng/L. The

errors shown are the deviation from the mean between the two duplicates field samples collected simultaneously. The AXYS analytical method for the 2008 sampling effort showed a slightly lower but comparable PFOA concentration (38 ng/L). PFOA concentrations in the FCC effluent during the 2010 sampling dropped to 13 ng/L, similar
to that measured in 2006. PFHxA concentrations in the FCC effluent decreased from 590 in 2008 to 310 ng/L during 2010. The POTW effluent PFOA concentrations dropped from 33 to 17

- 21 ng/L from 2006 to 2008 and then increased to 33 ng/L in 2010. This suggests that the changes observed may be within the "normal" variability of PFOA concentrations in these different effluents.

Irrigation water samples The Ocean Springs WWTP effluent water used for irrigation at the Jackson County Landfarm (POTW-IR-1) were collected from the same location in 2006 and had lower PFOA concentrations (11 ng/L) than observed in 2008 (43- 48 ng/L); however during 2010, PFOA concentrations had dropped to an average concentration of 16 ng/L. PFHxA concentrations in this irrigation water dropped from a concentration of 22 ng/L in 2008 to an average concentration of 8 ng/L during 2010. As stated previously, the irrigation water originates as effluent from the Ocean Springs wastewater treatment system and is not directly associated or connected to the Pascagoula water supply or the Pascagoula POTW.

Samples from Industrial Water The PFOA concentrations for samples of industrial water supplied by the Jackson County Port Authority (IND-H20-1 and D-1) were some of the lowest observed in the study; are similar to those observed for surface waters for 2008 and 2010 (<2.8 ng/L;

11Table 4). PFHxA concentrations were also very low during the study period (ND to 1.6 ng/L; Table 4) and are similar to those observed in surface waters.

Samples from Storm-Water The composite stormwater sample (FCC-SW-1) collected after a rain event from the stormwater trough at FCC Pascagoula had a temperature of 26.4 °C, a turbidity of 77 NTUs, and a pH of 5.38 (Table 3). Rainfall can have a pH as low as 4.5 so the observed
stormwater pH is not surprising and may be representative of stormwater from highly developed (i.e. hardened) catchments in this region as the FCC plant has a high proportion ofhardened surfaced at its Pascagoula facility. The salinity of the stormwater

was low (0.38) and the DO concentration was high (7.16 mg/L). DO concentrations are high in rainwater since it is at equilibrium with atmospheric oxygen concentrations. Stormwater oxygen concentrations can drop rapidly if the temperature is elevated as stormwater flows over hot surfaces however the observed value is near saturation for fresh water at the recorded temperature. The PFOA concentration of the stormwater sample collected in 2008 was 600 ± 100 ng/L. The error shown are the deviation from the mean between the two duplicates field samples collected one after another from the stormwater trough. Since these were composite samples collected over a 24-hour period, it is likely that differences in rainfall
rates throughout the sampling period could result in rapid variations in dilution and flow
rates across different surfaces, which could easily be reflected in two composite samples collected alongside one another. The more sensitive analytical technique utilized in 2008 reflected almost the same concentration as the first field sample (530 ng/L). Stormwater samples collected during 2010 had much lower PFOA concentrations (85 ng/L). The PFHxA concentration in stormwater fell from 590 ng/L during 2008 to 140 ng/L during 2010.

Groundwater samples Groundwater from monitor well MW-17 (Figure 2) contained the highest PFOA concentration (1000 ng/L) found in all water samples collected in this Follow Up Study with excellent agreement between analytical methods used (Table 4). Groundwater from MW-63 had a relatively lower PFOA concentration (260 ± 10 ng/L), which was slightly higher when reanalyzed with the more sensitive analytical technique (2008b column: 290 ng/L). Groundwater collected down gradient of the new chemical processing unit at monitor well MW-28 had a still lower PFOA concentration (93 ± 2) relative to the other groundwater samples and showed a slightly lower concentration of 82 ng/L when reanalyzed. The highest level ofPFOA observed in all of the 2008 water samples was from MW -17 (1 000 ng/L) which was much higher than water collected from the same well in 2006 (44 ng/L). Smaller increases in the groundwater PFOA concentrations between the Basline Study and the 2008 sampling were evident at the other wells (MW-28 and MW63) but were not as drastic. Well MW-28 increased at least twelve fold from< 7.8 to 93 ng/L while MW-63 (the well down gradient from processing) increased approximately four fold from 79 to 260

- 290 ng/L. From 2008 to 2010, The PFOA concentration in MW-17 decreased from 1000 to 280 ng/L while MW-28 and MW-63 both increased over this time period. Average PFOA

12concentrations in MW-28 rose from 88 to 250 ng/L while the average PFOA concentration at MW-63 increased from 280 to 950 ng/L. PFHxA concentrations in MW -17 fell from 790 ng/L to 520 ng/L from 2008 to 2010. The other two monitoring wells followed the same trend as the PFOA concentrations, increasing from 2008 to 2010. MW-28 increased slightly during this period from 210 to 360 ng/L while MW-63 rose dramatically from an average concentration of 950ng/L to an average concentration of 3000 ng/L, the highest concentration observed in any water sample during the study.

Sludge sample The POTW sludge samples from 2008 and 2010 were similar (32 and 33 ug/kg, respectively) and were of lower concentrations than was measured during the 2006 Baseline Study (68 ug/kg) suggesting that FCC activities have had no impact on the POTW sludge. PFHxA concentrations in the sludge decreased from 6.6 ug/kg in 2008 to 2.5 ug/kg in 2010.

BIOTA RESULTS

Fish samples Large catfish collected for this study from Mississippi Sound ranged from 14 to 17 inches in length during 2006 and 2008 while small specimens collected in Mississippi Sound ranged from 9.5 to 14.5 inches. Smaller specimens were collected in 2008 relative
to 2006 for both size classes therefore there is some overlap in the reported ranges. Large catfish sampled from Grand Bay ranged from 13.1 to 15.5 inches during the study period and again, the large catfish that were collected in 2008 were smaller than those collected in 2006. Small catfish sizes from Grand Bay ranged from 9 to 9.75 inches and were similar between 2006 and 2008 samplings. PFOA concentrations in all catfish samples were low. During 2006, carcass catfish samples from Mississippi Sound ranged from 1.4 to 2.2 ng/g. PFOA concentrations in the catfish filets were slightly but significantly lower than the carcass concentrations and ranged from 0.77 to 1.7ng/g. There was no statistical difference between catfish PFOA concentrations in either tissue type between the large and small size classes. Catfish carcass samples collected during 2006 from Grand Bay ranged from 1.5 to 1.7 ng/g. PFOA concentrations in catfish filet samples from Grand Bay were slightly but significantly lower than the carcass samples (1.4 to 1.6 ng/g). There was no statistical difference for either tissue type between size classes. PFOA concentrations from all catfish carcass and filet samples were not detectable (<1.9- 2.5 ng/g) during 2008. There was also no statistical difference in PFOA concentration within tissue types between Mississippi Sound and Grand Bay Speckled trout samples were collected from Mississippi Sound during 2006 and 2008 and from Grand Bay during 2008. Results from speckled trout were similar to those obtained for hardhead catfish. Carcass tissues from 2006 (Mississippi Sound) had PFOA concentrations ranging from 1.3 to 1.8 ng/g with an average concentration of 1.5 

### ± 0.2 ng/g. Filets from the same samples had slightly but not significantly lower PFOA concentration (1.5 

### ± 0.1 ng/g). All speckled trout samples from 2008 from both Mississippi Sound and Grand Bay that were sampled were below detection (<2.3

- 2.5

13ng/g). The detection limits between sampling years both both fish species were slightly different for the two sampling periods however the results do show that PFOA concentrations were low in all fish samples and are comparable to results from similar studies in Europe and North America (see discussion section).

Invertebrate samples Blue crabs were sampled from Mississippi Sound and Grand Bay during 2006 and 2008. Crabs from Mississippi Sound ranged from 5.5 to 9.4 inches carapace width during 2006 and from 5.6 to 6.8 inches during 2008. PFOA was below detection (ND < 0.0043 mg/g) in two of the six crab samples from Mississippi Sound during 2006, three had concentrations that were not quantifiable (between LOD and LOQ), while one had a measurable PFOA concentration of 0.065 ng/g. All blue crabs from Grand Bay during 2006 were above detection, ranging from 0.058 to 0.13 ng/g (average= 0.100 ± 0.036 ng/g). These PFOA concentrations are within five times the concentration measured in matrix blank controls. All blue crab samples collected during 2008 from both Mississippi Sound and Grand Bay had PFOA concentrations that were not detectable (<2.3- 2.5 ng/g) with the analytical detection limits determined for the 2008 samples, which was again higher than the limit of detection during the 2006 sampling campaign. Oysters were only sampled during the Pascagoula Baseline Study in 2006 and all had PFOA concentrations that were not detectable (<0.023 ng/g). Oysters were not sampled during the Pascagoula Follow Up Study.

DISCUSSION AND CONCLUSION Surface water PFOA concentrations in the Pascagoula River, Bayou Cassotte, Mississippi Sound and Grand Bay were all low from 2006 to 2010. It is difficult to discern whether there has been a change in PFOA concentrations in local surface waters between the time of the Pascagoula Baseline Study and this Follow Up Study (summer 2008 and 201 0) due to analytical differences between the two study periods. In 2006, the LOD was 1.6ng/L and the LOQ was 13 ng/L. All surface waters sampled had PFOA concentrations at or below these thresholds thus quantification was not possible. In 2008, the LOD and the LOQ with initial analytical technique used were 2.3 and 12 ng/L, respectively and all surface water samples were below the LOD. The more sensitive analytical technique used in 2008 showed low concentrations (1.2 to 3.0 ng/L) that would
not have been quantifiable in the 2006 study or with the initial technique used in 2008. PFOA concentrations in 2010 were all above the LOD and were similar to the 2008 results (1.5- 3.0 ng/L). These concentrations are comparable to those observed in other coastal waters while open ocean concentrations are typically 1 to 2 orders of magnitude lower (Yamashita et al., 2005). PFOA concentrations in coastal and open ocean samples from the Atlantic and Pacific ocean range from 0.045 to 15.3 ng/L with higher values (1.8
to 192 ng/L) being found in Tokyo Bay (Yamashita et al., 2005). Aside from these high values around Japan, PFOA concentrations were typically higher in the Atlantic ocean (0.1 to 0.5 ng/L) than concentrations measured in the Pacific (<0.14 ng/L). The lowest values found in this survey were in the central to eastern Pacific Ocean in surface waters (0.015 to 0.062 ng/L) and below 4000m depth (0.045 to 0.056 ng/L; Yamashita et al., 2005).

14PFHxA concentrations were examined to investigate the background concentrations of this perfluorinated compound prior to the replacement ofprocesses using 8-2 FTOH containing fluorotelomer alcohols with primarily 6-2 FTOH in First Chemical's Telomer based products. Concentrations in all surface water samples were low in 2008 (< 2.9ng/L) with 25% of the samples being below the LOD. Surface water samples that were above the LOQ from 2010 were lower(< 1.4 ng/L) with 75% of the samples below the LOD. These results indicate that the 6-2 FTOH processing being conducted at the FCC have not caused a measurable increase in surface water PFHxA concentrations in the Pascagoula River, Mississippi Sound, or Grand Bay sites. FCC Effluent which discharges to the Pascagoula River had higher concentrations ofPFOA than the surface water samples and ranged from 11 to 38 ng/L during the 2006 to 2010 samplings with the highest concentrations being measured in 2008 and lower concentrations during 2006 and 2010 (11 and 13 ng/L). Effluent from the POTW ranged from 17 to 33 ng/L during the 2006 to 2010 sampling efforts and were lower than the FCC effluent concentrations during 2006 and 2008. Water from the Ocean Springs wastewater treatment plant used to irrigate the Jackson County landfarm had similar concentrations (11- 48 ng/L). The 3M Company measured PFOA in six US cities
wastewater effluent and found a wide range of concentrations (40 to 2420 ng/L; 3M Environmental Laboratory, 2001) that were higher than that measured in the POTW of this study. PFHxA concentrations in the FCC effluent were much higher than PFOA concentrations: 590 ng/L in 2008 and 310 ng/L in 2010. The POTW effluent had PFHxA concentrations (22 and 14 ng/L in 2008 and 2010, respectively) similar to the few surface
water samples that were above the LOD. While no studies ofPFHxA concentrations could be found for wastewater treatment plants in North America, Guo et al. (2010) measured similar PFHxA concentrations of <0.5 to 16.1 ng/L in nineteen different
wastewater treatment plants in Korea. Industrial and drinking water from the FCC plant had PFOA concentrations that

were low, similar to the surface water samples, and ranged from below the LOD to 2.8 ng/L. Initially, it was believed that the industrial water and the drinking water sampled in 2008 were from different sources; however, in 2010, it was realized that these two samples both originated from the same drinking water source. This is confirmed with the nearly identical sample results between the industrial water and the drinking water obtained in 2008 for both PFOA and PFHxa. Therefore in 2010, water was only collected from one tap rather than the two sampled previously. PFOA concentrations in drinking
water in six US cities (Decatur, AL; Mobile, AL Colombus, GA; Pensacola, FL; Cleveland, TN and Port St. Lucie, FL), was measured by from 1999-2000 by the 3M Company and found that it was only detectable in Columbus where concentrations up to 27 ng/L were found (LOQ of25 ng/L; 3M Environmental Laboratory, 2001). Samples from the other five cities were below the LOD (7.5 ng/L) of that study. Drinking water concentration in New Jersey were comparable (<39 ng/L) to our study (Post et al., 2009). Japan and other Asian countries had drinking water concentrations of <0.1 to 41 ng/L (Saito et al., 2004; Tanaka et al., 2006) with the highest concentrations being found in the Osaka region. Sporadic concentrations at other Asian drinking water sites were as high as 456 ng/L (So et al, 2007). The current EPA advisory limit for drinking water is 400 ng/L (EPA, 2009).

15Several studies in the Great Lakes region have shown that surface water concentrations range from <2 to 59 ng/L (Sinclair et al., 2004). European studies have shown that PFOA concentrations in fresh waters of several countries including Germany, Italy, Sweden, and Norway range from below detection to as high as 57 ng/L with 75% of the concentrations ranging from less than the LOD to 8 ng/L (Tanaka et al, 2006; Loos et al., 2007; Skutlarek et al., 2006; Kallenbom et al, 2004; deVoogt et al., 2006a, 2006b, Weremiuk et al., 2006). Two contaminated rivers from Germany and the Netherlands

were reported to have values of3640 and 33900 ng/L. Stormwater samples from the FCC facility had similar PFOA concentrations from 2006 and 2008 (460 and 560 ng/L) however PFOA concentrations in stormwater were considerably lower in 2010 (85 ng/L). Stormwater from the Twin Cities metropolitan

area had an average PFOA concentration of9.3 ng/L (Xiao and Gulliver, 2011). Stormwater in an urbanized region of Singapore had PFOA concentrations of 5-31 ng/L (Nguyen et al, 2011). Stormwater runoff in Tokyo has been shown to have PFOA concentrations ranging from 15 to approximately 105 ng/L (Murakami et al., 2009a). The high concentrations for the FCC stormwater are much higher th an those found in these other studies and is also much higher than the FCC effluent. This suggests that some

source of PFOA exists from the FCC facility such as a leak within the facility or dry deposition from the FCC plant was depositing residual PFOA aerosols or particulates to the hardened structures on site which could then be entrained by rainwater and/or
stormwater into the holding areas that were sampled in this study. Stormwater PFHxA concentrations in 2008 (530 ng/L) were similar to that ofPFOA and also decreased significantly from 2008 to 2010. The decrease in levels of both perfluoinated compounds in 2010 may indicate lower production within the facility or an improvement/repair was made to lower the unknown source. PFOA and PFHxA levels in the monitoring wells at the FCC facility rivaled or exceeded stormwater concentrations and provided the highest values ofboth PFOA and PFHxA measured in this study. During the pilot study in 2006, PFOA concentrations (<7.8 to 79 ng/L) were lower than measured from 2008 to 2010 (93-1000 ng/L). PFHxA concentrations in the wells were 210 to 3100 niL and levels increased significantly in well MW-63 from 2008 to 2010. Increases in these perfluorinated compounds in these shallow wells can be attributed to FCC activities. While this aquifer is not used for drinking water, it should be noted that the high PFOA concentration at well MW-17 (1000 ng/L) during 2008 and well MW-63 during 2010 (945 ng/L) are above the EPA's provisional health advisory of400 ng/L. Published values of PFOA in shallow groundwaters are sparse in the literature as most studies have justifiably focused on drinking water wells which often pump groundwater from deeper aquifers. One such study examined PFOA concentrations in 115 drinking water wells surrounding Dupont's Washington Works plant on the Ohio River and found groundwater levels from 6 to 13,300 ng/L (Hoffman et al., 2011). Shultz et al. (2004) measured PFOA concentrations
up to 6,570,000 ng/L (6.57 mg/L) in shallow groundwaters beneath three US Air Forces fire training pads, where large amounts ofperfluoronated compounds were released over long periods in the form of aqueous film forming foams. Groundwaters from 0 to 33m depth beneath metropolitan Tokyo, Japan had PFOA concentrations from 0.1 to 94 ng/L (Murakami et al., 2009b).

16Sludge from the POTW plant (32- 33 ug/kg) during 2008 and 2010 had lower concentrations ofPFOA than during 2006 (68 ug/kg). The observed decrease may be representative of the inherent variability in PFOA concentrations from this sewage treatment plant. As discussed previously, sewage treatment plants may release more PFOA than they receive if the influent stream contains significant concentrations of
precursors that can degrade to form PFOA (Sinclair et a1 2006). However, other researchers have not observed PFOA increases during wastewater treatment (Schultz et al, 2006). PFOA concentrations from this and the baseline study are on the low end of the range measured in the 2001 3M study where sludge PFOA concentrations in six cities to ranged from <0.2 to 244 ug/kg. Guo et al. (2010) found PFOA concentrations in
wastewater sludge to range from below detection to 24.7 ug/kg in Korea. PFHxA concentrations in the same study were all below the LOD (<0.4 ug/kg) (Guo et al., 2010). PFOA and PFHxA concentrations in biota samples (speckled trout, channel catfish, and blue crabs) were all below the LOD (1.9- 3.6 ng/g) during the 2008 and 2010 study period. Given the low levels of these compounds in surface water samples in this study these results are not surprising. A large percentage ofresults from other studies in Europe and Asia have also been undetectable in fish (57- 85%; van Leeuwen et al., 2006; CSL, 2006; Berger et al., 2007; Gulkowska et al., 2006; Tseng et al., 2006) and
crustaceans (30- 100%; vanLeeuwen et al., 2006; Gulkowska et al., 2006; Nakata et al., 2006). Maximum PFOA values from these studies were as high as 18.7 ng/L for fish and 9.5 ng/L for crustaceans. Reported PFOA concentrations in fish from North American studies (Ontario and the Great Lakes) were 0.700 to 2.40 ng/kg (Martinet al., 2004; Furdui et al, 2005). Tomy et al. (2004) found PFOA concentrations at or below 0.5 ng/g in shrimp collected in the eastern Artie Ocean. Higher concentrations in fish and invertebrates have been found in other studies in areas known to be contaminated with perfluorinated compounds from production facilities, landfills, and wastewater treatment plants. Cumulatively, the results of this study show that on site stormwater and shallow groundwaters beneath the FCC site were the only samples that appear to have been impacted from FCC's production facility. Surface water PFOA concentrations were comparable to coastal waters from other regions of the world and have not increased significantly since 2006. PFHxA concentrations in surface waters appear to have decreased from 2008 to 2010 but the observed concentrations were all near the LOD and may reflect inherent variability in surface waters. Concentrations ofPFOA and PFHxA in fish and crabs were all undectable and do not suggest that fluorinated compounds are accumulating in biota in the study area.

17LITERATURE CITED

3M Environmental Laboratory 2001. Environmental Monitoring- Multi-City StudyWater, Sludge, Sediment, POTW Effluent and Landfill Leachate Samples- Executive Summary, June 25,2001.

Berger U., Holmstrom K., Glynn A., Berglund M., Ankarberg E., Tornkvist A. 2007. Perfluorinated alkyl substances in market basket food samples and fish from Lake Vattern and the Baltic Sea. Rapport till Naturvardsverket Programomrade Miljogiftssamordning Overenskommelse nr 219 0641 Dnr: 721-5953-06Mm. Stockholm/Uppsala 2007-04-03.

CSL (Central Science Laboratory). 2006. Perfluoroctane sulphonic acid (PFOS), perfluorooctanoic acid (PFOA) and related compounds in food, development and validation of a method and analysis ofTotal Diet Study samples. CSL report, FD 05/23. Central Science Laboratory.

de Voogt P, Berger U, de Coen W, de WolfW, Heimstad E, McLachlan M, van Leeuwen S, van Roon A 2006a. Perfluorinated organic compounds in the European environment (Perforce). Report to the EU, University of Amsterdam, Amsterdam, NL. ppl-126.

de Voogt P., Saez M., Serne P., Fahner W., van Roon A., and Mons M.N. 2006b. Perfluorinated alkilated substances in surface waters of the Netherlands. Poster presented
at the: Institute for Biodiversity and Ecosystem Dynamics, University of Amsterdam.SETAC Europe Annual Metting-The Hague.

EPA, 2009. Provisional health advisories for PFOA and PFOS accessed on November 21, 2011 at http://www.epa.gov/oppt/pfoa/pubs/pfoainfo.html#provisional

Furdui, V.I., Stock, N., Whittle, D.M., Crozier, P., Reiner, E., Muir, D.C.G. and Mabury, S.A. 2005. Perfluoroalkyl contaminants in lake trout from the Great Lakes. ENV024 Furdui. "Fluoros" 9th International Symposium on Fluorinated Alkyl Organics in the Environment, August 2005, Toronto, Canada

Gulkowska A., Jiang Q., So M.K., Taniyasu S., Lam P.K.S., Yamashita N. 2006. Persistent perfluorinated acids in seafood collected from two cities of China. Environmental Science and Technology 40, 3736-3741.

Guo R., Sim WJ, Lee ES, Lee JH, Oh JE. 2010. Evaluation ofthe fate ofperfluoroalkyl compounds in wastewater treatment plants. Water Research 44, 3476-3486.

Hoese, H. D., and R. H. Moore. 1977. Fishes of the Gulf of Mexico, Texas, Louisiana and adjacent waters. Texas A&M University Press, College Station, TX.

18Hoffman K, Webster TF, Bartell SM, WeisskopfMG, Fletcher T. 2011. Private drinking
water wells as a source of exposure to fluorooctanoic acid (PFOA) in communities surrounding a fluoropolymer production facility. Environmental Health Prospectives 119, 92-97.

Johnson, Mark. "Evaluation of Methodologies for Deriving Health-Based Values for PFCs in Drinking Water" (PDF). Agency for Toxic Substances and Disease Registry. 20, 37.

Kallenbom R., Berger U., and Jamberg U. 2004. Perfluorinated alkylated substances (PFAs) in the nordic environment. A TemaNord report ofthe Norwegian Institute for Air Research (NILU) (Kjeller, Norway) and the Institute for Applied Environmental Research (ITM), Stockholm University (Stockholm, Sweden).

Llanso, R. J., S. S. Bell, and F. E. Vose. 1998. Food habits of red drum and spotted sea trout in a restored mangrove impoundment. Estuaries 21:294-306.

Loos, R., Wollgast,J., Huber,T., and Hanke,G. 2007. Polar herbicides, pharmaceutical products, perfluorooctanesulfonate (PFOS), perfluorooctanoate (PFOA), and nonylphenol and its carboxylates and ethoxylates in surface and tap waters around Lake Maggiore in Northern Italy. Anal.Bioanal.Chem. 387, 1469-1478.

Martin, J.W., Whittle, D.M., Muir, D.C.G. and Mabury, S.A. 2004a. Perfluoroalkyl contaminants in a food web from lake Ontario. Environ Sci Techno!. 38, 5379-5385.

Murakami M, Shinohara H, Takada H. 2009a. Evaluation of wastewater and street runoff

as sources ofperfluorinated surfactants. Chemosphere 74, 487-493.

Murakami M, Kuroda K, Sato N, Fukushi T, Takizawa S, Takada H. 2009b. Groundwater pollution by perfluorinated surfactants in Tokyo. Environ Sci Techno!. 43, 3480-3486.

Nakata H., Karman K., Nasu T., Cho H., Sinclair E., and Takemura A. 2006. Perfluorinated Contaminants in Sediments and Aquatic Organisms Collected from Shallow Water and Tidal Flat Areas of the Ariake Sea, Japan: Environmental Fate of Perfluorooctane Sulfonate in Aquatic Ecosystems. Environ Sci Techno!. 40, 4916-4921.

Nguyen VT, Reinhart N, and Karina JY. 20 11. Occurrence and source characterization of perfluorochemicals in an urban watershed. Chemosphere 82, 1277-1285.

Oono S, Harada KH, Mahmoud MA, Inoue K, Koizumi A (October 2008). "Current levels of airborne polyfluorinated telomers in Japan". 

### Chemosphere 73 (6): 932-937.

Overstreet, R. M., and R. W. Heard. 1978. Food of the red drum, 

### Sciaenops ocellata, from Mississippi Sound. Gulf Research Reports 6:131-135.

19Piekarz AM, Primbs T, Field JA, Barofsky DF, Simonich S (December 2007). "Semivolatile fluorinated organic compounds in Asian and western U.S. air masses". Environ. Sci. Techno!. 41 (24): 8248-55.

Post GL, Louis JB, Cooper KR, Boros-Russo BJ, and Lippincott RL. 2009. Occurrence and potential significance ifperfluorooctanoic acid (PFOA) detected in New Jersey public drinking water systems. Environ Sci Technol. 43, 4547-4554.

Prevedouros K, Cousins IT, Buck RC, Korzeniowski SH (2006). "Sources, fate and transport ofperfluorocarboxylates", Environ. Sci. Techno/. 40 

### (1): 32-44.

Saito, N., Harada, K., Inoue, K., Sasaki, K., Yoshinaga, T., Koizumi, A., 2004. Perfluorooctanoate and perfluorooctane sulfonate concentrations in surface
water in Japan. J. Occup. Health 46, 49-59.

Scharf, F. S., and K. K. Schlicht. 2000. Feeding habits ofred drum (Sciaenops ocellatus) in Galveston Bay, Texas: Seasonal diet variation and predator-prey size relationships. Estuaries 23:128-139.

Shultz MM, Barofsky DF, and Field JA. 2004. Quantitative determination of fluorotelomer sulfonates in groundwater by LC MS/MS. Environ. Sci. Techno!. 38, 1828- 1835.

Schultz MM, Higgins CP, Huset CA, Luthy RG, Barofsky DF, Field JA (2006). "Fluorochemical mass flows in a municipal wastewater treatment facility". Environ. Sci. Techno!. 40 (23): 7350-7357 I

Sinclair E, Kannan K (2006). "Mass loading and fate ofperfluoroalkyl surfactants in
wastewater treatment plants". Environ. Sci. Techno!. 40 (5): 1408-1414,

Skutlarek D., Exner M., Farber H. 2006. Perfluorinated surfactants in surface and drinking waters. Environ. Sci. Pollut. Res. 13, 299-307.

So,M.K., Miyake,Y., Yeung,W.Y., Ho,Y.M., Taniyasu,S., Rostkowski,P., Yamashita,N., Zhou,B.S., Shi,X.J., Wang,J.X., Giesy,J.P., Yu,H., and Lam,P.K. 2007. Perfluorinated compounds in the Pearl River and Yangtze River of China. Chemosphere 68,2085-2095.

Tanaka S., Fujii S., Lien N.P.H., Nozoe M., Fukagawa H., Wirojanagud W., Anton A. and Lindstrom G. 2006. A simple pre-treatment procedure in PFOS and PFOA water analysis and its' application in several countries. Organohalogen Compounds 68, 527- 530.

Tomy, G.T., Budakowski, W., Halldorson, T., Helm, P.A., Stern, G.A., Friesen, K., Pepper, K., Tittlemier, S.A. and Fisk, A.T. 2004. Fluorinated organic compounds in an eastern Arctic marine food web. Environmental Science and Technology 38, 6475-6481.

20Tseng C., Liu L., Chen C., and Ding W. 2006. Analysis ofperfluorooctanesulfonate and related fluorochernicals in water and biological tissue samples by liquid chromatographyion trap mass spectrometry. Journal of Chromatography A 1105, 119-126.

van Leeuwen, S.P.J, van der Veen, I., Leonards, P.E.G., de Boer, J. 2006. Perfluorinated compounds in edible dutch fish. Organohalogen Compounds 68, 535-538.

Walters, C. and K.S. Dillon. 2007. Water Quality. In Grand Bay National Estuarine Research Reserve: An Ecological Characterization (Peterson, M.S., G.L. Waggy and M.S. Woodrey, editors). Grand Bay National Estuarine Research Reserve, Moss Point, Mississippi. NOAA publication.

Weremiuk A.M., Gerstmann S., Hartmut F. (2006). Quantitative determination of perfluorinated surfactants in water by LC-ESI-MS/MS. J Sep Sci.29, 2251

- 2255.

Feng Xiao F, Sirncik MF, and Gulliver JS. 2011. Perfluoroalkyl acids in urban
storrnwater runoff: Influence ofland use. Water Research. Revision submitted

Yamashita N, Kannan K, Taniyasu S, Horii Y, Petrick G, Garno T (2005). "A global
survey ofperfluorinated acids in oceans". Mar. Pollut. Bull. 51 (8-12): 658-68. doi: 10.1 016/j.rnarpolbul.2005.

21Table1.Sur:fitr1'dd"'dtidalstagefor2008samprffortSampleArrivalSampleSamoleLocationDateTimeLatitudeLon2itudeMediarfidalSta!!eSamnleIDnumberPascagoulaRiverUpstreamofPOTWRivermile227/16/20087:4430.5216188.59185Surfacewater-FloodPAS-W-PR-RM22-1PascagoulaRiverUpstreamofPOTWRivermile227116/200817:1030.521688.5918Surfacewater-EbbPAS-W-PR-RM22-2Pascag_oulaRiverDownstreamofPOTWRivermileI7/16/200811:2930.3547888.5666Surfacewater-FloodPAS-W-PR-RMOI-1PascagoulaRiverDownstreamofPOTWRivermileI7/16/200819:5430.3598888.56662Surfacewater-EbbPAS-W-PR-RMOI-2EscatawpaRiverUpstreamofconfluencewiththePascagoula-Rivermile37/16/200810:0330.42588.54108Surfacewater-FloodPAS-W-E-RM03-lEscatawpaRiverUpstreamofconfluencewiththePascagoula-Rivermile37/16/200818:5030.4250388.54109Surfacewater-EbbPAS-W-E-RM03-2BayouCassotteatthemouthofPascagoulaB<lY:-Rivermile07117/200810:5030.3326388.51396Surfacewater-FloodPAS-W-BC-RM00-1BayouCassottatthemouthofPascag_oulaBa]'-Rivermile07117/200820:4030.332988.5139Surfacewater-EbbPAS-W-BC-RM00-2MississippiSound-BeyondmouthofthePascagoulaRiver7/17/20089:4630.3274488.5668Surfacewater-FloodPAS-W-MS-1MississippiSound-BeyondmouthofthePascagoulaRiver7/17/200821:3030.3274288.56682Surfacewater-EbbPAS-W-MS-2GrandBayNERR-ncarBiologicalsamplelocation7/17/20087:5730.3571588.41813Surfacewater-FloodPAS-W-GB-1GrandBayNERR-nearBiologicalsamplelocation7117/200818:3730.3572588.4182Surfacewater-EbbPAS-W-GB-2EffluentfromPascagoulaPOTWtoPascagoulaRiverEffluent8/18/20088:01EffluentPAS-Z-POTWEFF-1EffluentfromFCCtoPOTW-24hr.compositesampleEffluent8113/2008EffluentPAS-Z-FCC-EFF-1StormwatersamplefromFCCStormwater8/11/200815:08StormwaterPAS-Z-FCC-SW-1WestJacksonCountyLandfarmirrigationwaterIrrigationWater7/31/200813:20IrrigationwaterPAS-Z-POTW-IR-1Industrialprocesswatersujl]JiiedtoFCCbyJacksonCountyPortAuthoritySupply_Water7/31/200811:02SupplywaterPAS-Z-Ind-H20-lPotablewaterfromCityofPascagoulawatersystempriortotreatmentPotableWater7/311200811:23PotablewaterPAS-D-1MonitorWellMW-17Groundwater7/30/200813:21GroundwaterPAS-G-MW17-0lMonitorWellMW-28Groundwater7/30/200813:49GroundwaterPAS-G-MW28-0lMonitorWellMW-63Groundwater7/30/200812:52GroundwaterPAS-G-MW63-0l22Table2.Surf:tr1t...-------=-r---o----·'dd"'dtidalfor2010rf:DSam_IDeSam_IDeSample-SampleLocationDateTimeLatitudeLon!!itudeMedia/TidalSta11:eSampleIDnumberPascagoulaRiverUpstreamofPOTWRivermile227/26/201094530.5216288.59187SurfaceWater;FioodTidePAS-W-PR-RM22-IPascagoulaRiverUpstreamofPOTWRivermile227/26/20IOI82530.52I5288.59I78SurfaceWater;EbbTidePAS-W-PR-RM22-2PascagoulaRiverDownstreamofPOTWRivermileI7/26/20IOI35230.3550588.566SurfaceWater;FioodTidePAS-W-PR-RMOI-IPascagoulaRiverDownstreamofPOTWRivermileI7/26/2010211030.3548888.53894SurfaceWater;EbbTidePAS-W-PR-RMOl-2EscatawpaRiverUpstreamofconfluencewiththePascagoula-Rivermile37/26/2010115030.4252488.54099SurfaceWater;FioodTidePAS-W-E-RM03-1EscatawpaRiverUpstreamofconfluencewiththePascagoula-Rivermile37/26/2010195330.2550488.32467SurfaceWater;EbbTidePAS-W-E-RM03-2BayouCassottatthemouthofPascagoulaBay-Rivermile07/27/2010124730.3329288.51327SurfaceWater;FioodTidePAS-W-BC-RM00-1BayouCassottatthemouthofPascagoulaBay-Rivermile07/27/2010191030.332988.5139SurfaceWater;EbbTidePAS-W-BC-RM00-2MississippisSound-BeyondmouthofthePascagoulaRiver7/27/2010133930.3274688.56666SurfaceWater;FioodTidePAS-W-MS-1Mississip]JisSound-BeyondmouthofthePascagoulaRiver7/27/2010195530.3284988.5674SurfaceWater;EbbTidePAS-W-MS-2GrandBayNERR-nearBiologicalsamplelocation7/27/2010103730.3571988.41813SurfaceWater;FioodTidePAS-W-GB-1GrandBayNERR-ncarBiologicalsamplelocation7/27/2010173530.3572488.41805SurfaceWater;EbbTidePAS-W-GB-2EffluentfromPascagoulaPOTWtoPascagoulaRiver8/21120101020NA NAEffluentPAS-Z-POTW-EFF-1EffluentfromFCCtoPOTW-24hourcomposite8/12/2010I005NA NAEffluentPAS-Z-FCC-EFF-1StormwatersamplefromFCC8/12/2010929NANAStormwaterPAS-Z-FCC-SW-1WestJacksonCountyLandfarmirrigationwater9/1120101022NANAIrrigationwaterPAS-Z-POTW-IR-1IndustrialprocesswatersuppliedtoFCCbyJacksonCountyPortAuthority8112/20101022NANASupplywaterPAS-Z-IND-H20-1MonitorWellMW-17FirstChemicalCorporation8/12/2010919NANAGroundwaterPAS-G-MW17-01MonitorWellMW-28FirstChemicalCorporation8/12/2010945NANAGroundwaterPAS-G-MW28-0IMonitorWellMW-63FristChemicalCorporation8/12/2010850NA NAGroundwaterPAS-G-MW63-0lSludgefromPOTWlandfarm8/21120101035NANASludgePAS-X-POTW-S-I23

### Table 3

2008 Depth Sample ORP Turbidity DO cone. Sample ID number Total (ft) depth (m) T·c JlH (mv) (NTU) (mg/L) Salinity

PAS-W-PR-RM22-I 16.8ft 2.507 30.9 6.85 68.5 9.1 5.69 0.04

PAS-W-PR-RM22-2 16.6ft 2.68 31.31 6.85 36.2 10.7 6.5 0.05

PAS-W-PR-RMOI-1 29.5ft 4.428 25.09 7.71 -8.6 2.7 1.92 31.31

PAS-W-PR-RMOI-2 24.4ft 3.454 27.64 7.85 35.8 5.3 4.89 25.9

PAS-W-E-RM03-I 18.7ft 2.976 26.o7 7.61 100.7 2 1.73 27.63

PAS-W-E-RM03-2 17.3ft 2.711 29.11 6.98 78.4 3.4 3.79 11.23

PAS-W-BC-RM00-1 42.7ft 5.886 25.16 7.76 4.1 14.8 2.37 31.48

PAS-W-BC-RM00-2 41.3ft 5.974 27.4 7.99 9.3 6.5 7.06 29.56

PAS-W-MS-1 4.9ft 0.835 29.11 8.08 60.1 14.4 5.87 24.98

PAS-W-MS-2 3.6ft 0.52 30.17 8.16 -0.5 14.5 5.24 25.39

PAS-W-GB-1 5.4ft 1.057 30.15 8.12 30.7 18.7 4.81 24.46

PAS-W-GB-2 3.6ft 0.75 32.78 7.99 I 29.4 2.66 23.69

PAS-Z-POTW-EFF-1 NA NA 23.97 7.53 185.3 7.7 7.13 0.6
PAS-Z-FCC-EFF-1 NA NA NA NA NA NA NA NA
PAS-Z-FCC-SW-1 NA NA 26.35 5.38 202 77.6 7.16 0.38
PAS-Z-POTW-IR-1 NA NA 31.04 7.69 312.5 974.5 4.2 0.38
PAS-Z-IND-H20-I NA NA 31.31 7.82 200.2 63.2 6.84 0.08
PAS-D-1 NA NA 29.69 7.58 222.7 -0.8 5.19 0.08
PAS-G-MWI7-0l NA NA 31.79 6.71 218.3 25.8 4.4 0.36

PAS-G-MW28-0 I NA NA 29.61 5.96 49 7.4 4.1 0.72

PAS-G-MW63-0 I NA NA 28.07 5.7 -35.4 12.5 2.36 0.4

2010 Depth Sample ORP Turbidity DO cone. Sample ID number Total (ft) depth (m) T·c pH (mv) (NTU) (mg!L) Salinity
PAS-W-PR-RM22-1 20.3 3.023 31.24 6.74 67.2 11.1 5.9 0.04
PAS-W-PR-RM22-2 21.6 3.002 31.92 6.99 8.4 12.6 6.08 0.04
PAS-W-PR-RM01-1 30.3 5.076 30.96 7.62 15 7.4 4.92 22.07
PAS-W-PR-RM01-2 34.6 5.078 31.88 7.54 3.4 7.5 6.34 17.09
PAS-W-E-RM03-1 20.4 3.063 31.11 6.55 81.9 7.9 4.22 12.98
PAS-W-E-RM03-2 19.2 3.061 31.52 6.61 10.9 4.3 5.31 5.95
PAS-W-BC-RM00-1 44.1 5.056 30.97 7.78 6.3 5.1 5.2 23.31
PAS-W-BC-RM00-2 43.8 5.972 30.87 8.03 -24.6 5.1 2.78 23.96
PAS-W-MS-1 4 1.001 32.78 8.1 -14.7 20.8 7.05 18.15
PAS-W-MS-2 2.2 0.287 33.52 8.32 -18.2 33.4 6.02 29.19
PAS-W-GB-1 4.8 1.429 30.93 7.8 40.2 28.2 6.26 21.92
PAS-W-GB-2 3.4 0.784 33.72 7.94 -33.5 24 6.91 21.36
PAS-Z-POTW-EFF-1 NA NA 30.57 7.41 4.8 -1.1 7.71 0.72
PAS-Z-FCC-EFF-1 NA NA 15.74 7.35 171.8 13 9.59 3.39
PAS-Z-FCC-SW-1 NA NA 29.76 8.25 55.3 36.1 14.77 0.405
PAS-Z-POTW-IR-1 NA NA 27.96 7.54 8.4 34 2.48 0.29
PAS-Z-IND-H20-1 NA NA 31.16 8.03 80.9 -1.9 14.15 0.07
PAS-G-MW17-01 NA NA 31.43 6.4 1.7 99.8 6.06 0.49
PAS-G-MW28-0 1 NA NA 27.86 7.19 72.5 14.7 8.99 0.33
PAS-G-MW63-0 1 NA NA 28.21 6.49 -81 76.6 5.86 0.46

24Table 4. Water sample PFOA and PFHxA results from 2008 and 2010. PFOA concentrations fl th B 

### 1" Stud

. 2006 h fl

. rom e ase me Ly 1ll are s own or companson. 2006* 2008a** 2008 2008 2010 2010 PFOA PFOA PFOAb PFHxA PFOA PFHxA
Samole ID number (nf!IL) (nf!IL) (nf!IL) (nf!IL) (nf!IL) (nf!IL)
PAS-W- PR- RM22-1 NQ (7.8) ND 2.9 3.7 1.7 ND
PAS-W-PR-RM22-1 (lab dup) 1.5 ND PAS-W-PR-RM22-2 NQ (7.8) ND 2.2 2.1 1.5 ND PAS-W-PR-RM01-1 NQ (13) ND 1.8 2.1 ND
PAS-W-PR-RM01-2 NQ (13) ND 2.4 1.3 2.2 ND PAS-W-E-RM03-1 NQ (13) ND 1.6 2 1.7 ND
PAS-W-E-RM03-2 NQ (13) ND 2.6 1.5 1.7 ND PAS-W-BC-RM00-1 NQ (13) ND 1.2 2.2 1.4
PAS-W-BC-RM00-2 NQ (13) ND 1.7 1.5 2.1 1.6
PAS-W-MS-1 NQ (13) ND 2.1 1.6 1.7 ND PAS-W-MS-2 NQ (13) ND 1.8 2.2 ND PAS-W-GB-1 NQ (7.8) ND 2.2 1.7 2.9 1.3
PAS-W-GB-1 (lab dup) 2.5 1.4
PAS-W-GB-2 ND (1.6) ND 3 2.8 2.7 ND
PAS-Z- POTW-EFF-1 33 17 21 22 33 14
PAS-Z-POTW-EFF-1 (lab dup) 16
PAS-Z- FCC-EFF-1 40 38 590 13 310 PAS-Z-FCC-EFF-1 (lab dup) 

### 11 45
PAS-Z-FCC-EFF-1-DUP 49 PAS-Z-FCC-SW-1 460 480 530 590 85 140 PAS-Z-FCC-SW-1 (lab dup) 500 PAS-Z-FCC-SW-1-DUP 700 PAS-Z-POTW-IR-1 

### 11 43 48 22 15 7.3 PAS-Z-POTW-IR-1 dup 17 8.6 PAS-Z-IND-H20-1 ND (1.6) NQ 2.8 1.6 ND PAS-Z-IND-H20-1 1.4 ND PAS-D-1 ND (1.6) ND 2.6 1.7 PAS-G-MW17-01 44 1000 1000 790 280 520 PAS-G- MW28-0 1 NQ (7.8) 94 82 210 250 360 PAS-G- MW28-0 1 (lab dup) 91
PAS-G-MW63-01 79 250 290 810 940 2900 PAS-G-MW63-01-DUP 260 950 3100

{pg/k_e} (pg/kg) (pg/kg) PP AS- X- POTW -S-1 68 32 6.6 33 2.5

25Table 5. Biota sample names, numbers, and size for Mississippi Sound and Grand Bay samples collected during the Baseline Study (2006) and this study (2008).



### Mississippi Sound Biota Samples 2006 2006 2008 2008 Sample Media Samole Number Size Inches Samole Number Size, Inches speckled trout

- Large PAS-X-MS-WF-L-1 18.5 PAS-X-MS-F2-L-1 15.75 speckled trout

- Large PAS-X-MS-WF-L-2 17.5 PAS-X-MS-F2-L-2 13.5 speckled trout

- Large PAS-X-MS-WF-L-3 16.5 PAS-X-MS-F2-L-3 11.75 speckled trout

- Small PAS-X-MS-WF-S-1 12 PAS- X-MS- F2-S-1 11.5 speckled trout

- Small PAS-X-MS-WF-S-2 12.5 PAS-X-MS-F2-S-2 11.625 speckled trout

- Small PAS-X-MS-WF-S-3 12.5 PAS-X-MS-F2-S-3 11.375 catfish

- Large PAS-X-MS-CF-L-1 15 PAS-X-MS-C-L-1 14 catfish

- Large PAS-X-MS-CF-L-2 17 PAS-X-MS-C-L-2 14 catfish- Large PAS-X-MS-CF-L-3 15.5 PAS-X-MS-C-L-3 15.5 catfish

- Small PAS-X-MS-CF-S-1 14 PAS-X-MS-C-S-1 12.75 catfish

- Small PAS-X-MS-CF-S-2 14 PAS-X-MS-C-S-2 9.625 catfish

- Small PAS-X-MS-CF-S-3 14.5 PAS-X-MS-C-S-3 9.5 blue crab PAS-X-MS-BC-1 5.5 PAS-X-MS-BC-1 6.375 blue crab PAS-X-MS-BC-2 6.2 PAS-X-MS-BC-2 6.75 blue crab PAS-X-MS-BC-3 7.8 PAS-X-MS-BC-3 6.25 blue crab PAS-X-MS-BC-4 9.4 PAS-X-MS-BC-4 6.5 blue crab PAS-X-MS-BC-5 9.2 PAS-X-MS-BC-5 6.5625 blue crab PAS-X-MS-BC-6 8.4 PAS-X-MS-BC-6 5.625

oyster PAS-X-MS -0-1 3 oyster PAS-X-MS-0-2 3.5 oyster PAS-X-MS-0-3 2.5 oyster PAS-X-MS-0-4 3.25 oyster PAS-X-MS-0-5 4.25 oyster PAS-X-MS-0-6 3



### Grand Bay Biota samples
2006 2006 2008 2008 Sample Media Samnle Number Size Inches Samnle Number Size Inches speckled trout

- Large PAS-X-GB-F2-L-1 NA PAS-X-GB-F2-L-1 12.5 speckled trout

- Large PAS-X-GB-F2-L-2 NA PAS-X-GB-F2-L-2 15.25 speckled trout

- Large PAS-X-GB-F2-L-3 NA PAS-X-GB-F2-L-3 17.875 speckled trout

- Small PAS-X-GB-F2-S-1 NA PAS-X-GB-F2-S-l 10.5 speckled trout

- Small PAS-X-GB-F2-S-2 NA PAS-X-GB-F2-S-2 10.5 speckled trout

- Small PAS-X-GB- F2-S- 3 NA PAS-X-GB-F2-S-3 10.375 catfish- Large PAS-X-GB-CF-L-1 15.5 PAS-X-GB-C-L-1 13.375 catfish- Large PAS-X-GB-CF-L-2 14.5 PAS-X-GB-C-L-2 13.125 catfish

- Large PAS-X-GB-CF-L-3 15 NS NS catfish

- Small PAS-X-GB-CF-S-1 12.25 PAS-X-GB-C-S-1 12.75 catfish

- Small PAS-X-GB-CF-S-2 9.25 PAS-X-GB-C-S-2 9.75 catfish

- Small PAS-X-GB-CF-S- 3 NA PAS-X-GB-C-S-3 9.25 catfish

- Small PAS- X-GB-CF-S-4 NA PAS- X-GB-C-S-4 9

blue crab PAS-X-GB-BC-1 5.1 PAS-X-GB-BC-1 7.125 blue crab PAS-X-GB-BC-2 5.1 PAS-X-GB-BC-2 5.5625 blue crab PAS-X-GB-BC-3 5.4 PAS-X-GB-BC-3 6 blue crab PAS-X-GB-BC-4 5.7 PAS-X-GB-BC-4 5.75 blue crab PAS-X-GB-BC-5 6.3 PAS-X-GB-BC-5 6.125 blue crab PAS-X-GB-BC-6 6.4 PAS-X-GB-BC-6 5.125

oyster PAS-X-GB-0-1 3 oyster PAS-X-GB-0-2 3 oyster PAS-X-GB-0-3 2.5 oyster PAS-X-GB-0-4 2.5 oyster PAS-X-GB-0-5 3.5 oyster PAS-X-GB-0-6 3

26Table6.PFOAconcentrationsforfishsamplescollectedin2006and2008fromMississippiSoundandGrandBay.SampleswereanalyzedforPerfluorooctanoicacid(PFOA)andPerfluorohexanoicacid(PFHxA).Dataisroundedtotwosignificantfiguresandreportedasreceived.SoundFishSampleMediangjg=nanogramspergramorpartsperbillionLOD=LevelofdetectionLOQ=LimitofquantitationND=CompoundnotdetectedNQ=CompounddetectedbetweenLODandLOQND<LOD<NQ<LOQNS=NotsampledNA=Notapplicable2006FishCarcassFishFiletPFOA,(ng/g)PFOA,(ng/g)B=ReportedconcentrationiswithinSXtheconcentrationdetectedinmatrixblank(control)samplesUJ=listedreportinglimitshouldbeconsideredtobeanestimatedvalue2008200827Table7.PFOAconcentrationsforinvertebratesamplescollectedfromMississippiSoundandGrandBayin2006and2008.SampleswereanalyzedforPerfluorooctanoicacid(PFOA)andPerfluorohexanoicacid(PFHxA).Dataisroundedtotwosignificantfiguresandreportedasreceived.SoundInvertebrateng/g=nanogramspergramorpartsperbillionLOD=LevelofdetectionLOQ=LimitofquantitationND=CompoundnotdetectedNQ=CompounddetectedbetweenLODandLOQND<LOD<NQ<LOQNS=NotsampledNA=NotapplicableB=ReportedconcentrationiswithinSXtheconcentrationdetectedinmatrixblank(control)samplesUJ=listedreportinglimitshouldbeconsideredtobeanestimatedvalue20062008200828EffluentwatersampledischargetoPOTW,IndustrialWatersupplysamplePotableWatersupplysampletJl.limonitorwellsMW17,28and63DownstreamPOTWmix.zone..._p...r........·-MississippiSoundwatersample-0.5milebeyondmouthofEastPascagoulaRiverICo-locatedwithbiologicalsamples.I------t'J,·.-trf.-7••TITLE:BaselineStudySamplingLocationsPascagoulaBaselineStudyIWorkPlanFirstChemicalCorp.,Pascagoula,MSOWN:IDES.:LWGCHKD:IAPPD:PROJECTNO.:18984786.06010CORPORATEREMEDIATIONGROUPAnAlliancebetweenDuPontandURSDiamond140CypressStationDrive,Suite140Houston,Texas77090WP\Pascagoula\18984356FirstChemBaselineStudy\Figure1SamplingLocations29DATE:IREV.:5/25/20061IIIFIGURENO.:LEGEND 

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### PFOA vs. Salinity

0.0035

0.003 4

### t 

# •

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# • 

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0 0 10 20 30 40
Salinity

Figure 3. PFOA concentrations vs. salinity for all surface water samples.

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