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-2003-0012-1294 

Andrea 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 Company 
1001 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 of the 

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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PFOA 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 of the 

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 

2 
INTRODUCTION 

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% of historical emissions, respectively (Prevedouros et al, 

2006). An additional potential source ofPFOA is the biodegradation of precursors 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 of these processes to air, water or soil. 

Purpose of environmental monitoring studies 

The purpose of the 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" of the 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 of perfluorinated 

compounds not associated with FCC Pascagoula. 

The purpose of this 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 

3 
in 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) 

4 
and 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 of the 

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 

5 
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 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 of the 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 

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12:52, 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 of Mexico 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. 

7 
Fish 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 of the 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 of the 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 

8 
Chemical Corporation. To fulfill this objective, six samples of the 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 

of the 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 

9 
quantification 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 13C-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 13C-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) 

10 
with 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 of 43 ± 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; 

11 
Table 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 storm water from highly 

developed (i.e. hardened) catchments in this region as the FCC plant has a high 

proportion of hardened 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 

12 
concentrations 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 

13 
ng/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). 

14 
PFHxA concentrations were examined to investigate the background 

concentrations of this perfluorinated compound prior to the replacement of processes 

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). 

15 
Several 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 of both 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 of 400 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 of perfluoronated 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 ). 

16 
Sludge 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 of results 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. 

17 
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Post GL, Louis JB, Cooper KR, Boros-Russo BJ, and Lippincott RL. 2009. Occurrence 

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20 
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21 
Table 1. Sur:fi t r 1 

' 

d d" 

' 

d tidal sta ge for 2008 samp r ffort 

Sample Arrival Sample 

Sam ole Location Date Time Latitude Lon2itude Mediarfidal Sta!!e 

Pascagoula River Upstream ofPOTW River mile 22 7/16/2008 7:44 30.52161 88.59185 Surface water- Flood 

Pascagoula River Upstream ofPOTW River mile 22 7116/2008 17:10 30.5216 88.5918 Surface water - Ebb 

Pascag_oula River Downstream ofPOTW River mile I 7/16/2008 11:29 30.35478 88.5666 Surface water - Flood 

Pascagoula River Downstream ofPOTW River mile I 7/16/2008 19:54 30.35988 88.56662 Surface water - Ebb 

Escatawpa River Upstream of confluence with the Pascagoula - River mile 3 7/16/2008 10:03 30.425 88.54108 Surface water - Flood 

Escatawpa River Upstream of confluence with the Pascagoula- River mile 3 7/16/2008 18:50 30.42503 88.54109 Surface water- Ebb 

Bayou Cassotte at the mouth of Pascagoula B<lY:- River mile 0 7117/2008 10:50 30.33263 88.51396 Surface water - Flood 

Bayou Cassott at the mouth ofPascag_oula Ba]'- River mile 0 7117/2008 20:40 30.3329 88.5139 Surface water- Ebb 

Mississippi Sound- Beyond mouth of the Pascagoula River 7/17/2008 9:46 30.32744 88.5668 Surface water- Flood 

Mississippi Sound- Beyond mouth of the Pascagoula River 7/17/2008 21:30 30.32742 88.56682 Surface water - Ebb 

Grand Bay NERR- ncar Biological sample location 7/17/2008 7:57 30.35715 88.41813 Surface water- Flood 

Grand Bay NERR- near Biological sample location 7117/2008 18:37 30.35725 88.4182 Surface water - Ebb 

Effluent from Pascagoula POTW to Pascagoula River Effluent 8/18/2008 8:01 Effluent 

Effluent from FCC to POTW- 24 hr. composite sample Effluent 8113/2008 Effluent 

Stormwater sample from FCC Storm water 8/11/2008 15:08 Storm water 

West Jackson County Landfarm irrigation water Irrigation Water 7/31/2008 13:20 Irrigation water 

Industrial process water sujl]Jiied to FCC by Jackson County Port Authority Supply_ Water 7/31/2008 11:02 Supply water 

Potable water from City of Pascagoula water system prior to treatment Potable Water 7/3112008 11:23 Potable water 

Monitor Well MW -17 Groundwater 7/30/2008 13:21 Groundwater 

Monitor Well MW-28 Groundwater 7/30/2008 13:49 Groundwater 

Monitor Well MW-63 Groundwater 7/30/2008 12:52 Groundwater 

22 
Table 2. Surf: 

... 

t -- - ----=-r r ---o 1 -- - -· t ' d d" ' d tidal for 2010 r f:D 

Sam_IDe Sam_IDe Sample 

Sample Location Date Time Latitude Lon!!itude Media/Tidal Sta11:e 

Pascagoula River Upstream ofPOTW River mile 22 7/26/2010 945 30.52162 88.59187 Surface Water;Fiood T

Pascagoula River Upstream ofPOTW River mile 22 7/26/20IO I825 30.52I52 88.59I78 Surface Water;Ebb Tid

Pascagoula River Downstream ofPOTW River mile I 7/26/20IO I352 30.35505 88.566 Surface Water;Fiood T

Pascagoula River Downstream ofPOTW River mile I 7/26/2010 2110 30.35488 88.53894 Surface Water;Ebb Tid

Escatawpa River Upstream of confluence with the Pascagoula- River mile 3 7/26/2010 1150 30.42524 88.54099 Surface Water;Fiood T

Escatawpa River Upstream of confluence with the Pascagoula- River mile 3 7/26/2010 1953 30.25504 88.32467 Surface Water;Ebb Ti

Bayou Cassott at the mouth of Pascagoula Bay- River mile 0 7/27/2010 1247 30.33292 88.51327 Surface Water;Fiood T

Bayou Cassott at the mouth of Pascagoula Bay- River mile 0 7/27/2010 1910 30.3329 88.5139 Surface Water;Ebb Ti

Mississippis Sound- Beyond mouth of the Pascagoula River 7/27/2010 1339 30.32746 88.56666 Surface Water;Fiood T

Mississip]Jis Sound- Beyond mouth of the Pascagoula River 7/27/2010 1955 30.32849 88.5674 Surface Water;Ebb Ti

Grand Bay NERR- near Biological sample location 7/27/2010 1037 30.35719 88.41813 Surface Water;Fiood T

Grand Bay NERR- ncar Biological sample location 7/27/2010 1735 30.35724 88.41805 Surface Water;Ebb Ti

Effluent from Pascagoula POTW to Pascagoula River 8/2112010 1020 NA NA Effluent 

Effluent from FCC to POTW - 24 hour composite 8/12/2010 I005 NA NA Effluent 

Stormwater sample from FCC 8/12/2010 929 NA NA Storm water 

West Jackson County Landfarm irrigation water 9/112010 1022 NA NA Irrigation water 

Industrial process water supplied to FCC by Jackson County Port Authority 8112/2010 1022 NA NA Supply water 

Monitor Well MW -17 First Chemical Corporation 8/12/2010 919 NA NA Groundwater 

Monitor Well MW-28 First Chemical Corporation 8/12/2010 945 NA NA Groundwater 

Monitor Well MW-63 Frist Chemical Corporation 8/12/2010 850 NA NA Groundwater 

Sludge from POTW landfarm 8/2112010 1035 NA NA Sludge 

23 
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 

P AS-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 

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

P AS-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 

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

fl rom th e B ase 1" me Stud Ly 1ll . 2006 are s h own fl 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 

P AS-Z-POTW-EFF -1 33 17 21 22 33 14 

PAS-Z-POTW-EFF-1 (lab dup) 16 

P AS-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 

P AS-G-MW28-0 1 NQ (7.8) 94 82 210 250 360 

P AS-G-MW28-0 1 (lab dup) 91 

P AS-G-MW 63-01 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 

25 
Table 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 

26 
Table 6. PFOA concentrations for fish samples collected in 2006 and 2008 from Mississippi Sound and Grand Bay. Sampl

Perfluorooctanoic acid (PFOA) and Perfluorohexanoic acid (PFHxA). Data is rounded to two significant figures and reporte

Sound Fish 

Sample Media 

ngjg =nanograms per gram or parts per billion LOD = Level of detection LOQ = Limit of quantitation 

ND =Compound not detected 

NQ =Compound detected between LOD and LOQ 

ND<LOD<NQ<LOQ 

NS = Not sampled 

NA =Not applicable 

2006 

Fish Carcass Fish Filet 

PFOA, (ng/g) PFOA, (ng/g) 

B =Reported concentration is within SX the concentration detected in matrix blank (control) samples 

UJ =listed reporting limit should be considered to be an estimated value 

2008 

27 
Table 7. PFOA concentrations for invertebrate samples collected from Mississippi Sound and Grand Bay in 2006 and 2008

for Perfluorooctanoic acid (PFOA) and Perfluorohexanoic acid (PFHxA). Data is rounded to two significant figures and rep

Sound Invertebrate 

ng/g =nanograms per gram or parts per billion LOD = Level of detection LOQ = Limit of quantitation 

ND =Compound not detected 

NQ =Compound detected between LOD and LOQ 

ND<LOD<NQ<LOQ 

NS =Not sampled 

NA = Not applicable 

B =Reported concentration is within SX the concentration detected in matrix blank (control) samples 

UJ =listed reporting limit should be considered to be an estimated value 

2006 2008 2008 

28 
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31 
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