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Disposition of Wastewater-Associated Polybrominated Diphenyl Ethers in a Freshwater Receiving Stream

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Disposition of Wastewater-Associated Polybrominated Diphenyl Ethers in a Freshwater Receiving Stream W&M ScholarWorks Dissertations, Theses, and Masters Projects Theses, Dissertations, & Master Projects 2006 Disposition of Wastewater-Associated Polybrominated Diphenyl Ethers in a Freshwater Receiving Stream Mark Joseph La Guardia College of William & Mary - Arts & Sciences Follow this and additional works at: https://scholarworks.wm.edu/etd Part of the Environmental Sciences Commons, and the Hydrology Commons Recommended Citation La Guardia, Mark Joseph, "Disposition of Wastewater-Associated Polybrominated Diphenyl Ethers in a Freshwater Receiving Stream" (2006). Dissertations, Theses, and Masters Projects. William & Mary. Paper 1539626851. https://dx.doi.org/doi:10.21220/s2-5pjx-m003 This Thesis is brought to you for free and open access by the Theses, Dissertations, & Master Projects at W&M ScholarWorks. It has been accepted for inclusion in Dissertations, Theses, and Masters Projects by an authorized administrator of W&M ScholarWorks. For more information, please contact [email protected]. Disposition of Wastewater-Associated Polybrominated Diphenyl Ethers In a Freshwater Receiving Stream A Thesis Presented to The Faculty of the Department of Chemistry The College of William and Mary in Virginia In Partial Fulfillment Of the Requirements for the Degree of Master of Science by Mark Joseph La Guardia 2006 APPROVAL SHEET This thesis is submitted in partial fulfillment of the requirements for the degree of Master of Science Marlt J. La Guardia Approved by the Committee, December 2006 TABLE OF CONTENTS Page List of Tables iv List of Figures v Abstract viii Introduction 2 Study Goal 19 Study Site and Sample Location 21 Samples, Methodology and Quality Control 29 Results 42 Discussion 64 Conclusion 84 Appendix 87 References 101 Vita 106 iii LIST OF TABLES Table Page 1. Technical flame-retardant (penta-, octa-, and deca-PBDEs) compositions (%, w/w) 5 2. PBDEs detected in various environmental and biological matrixes 8 3. Sample ID, location, % lipids and %TOC 24 4. PBDE congener analysis, Relative Retention Indices (RRIs) and major fragmentation ions (El and ECNI) 36 5. Matrix spiking solution 41 6. PBDEs (pg/kg, dry weight) in wastewater sludge, Roxboro WWTP, NC. 47 7a. PBDEs (pg/kg, %TOC) in sediments from Marlowe/Storys Creek and tributaries, collected 2002 53 7b. PBDEs (pg/kg, %TOC) in sediments from Marlowe/Storys Creek and tributaries, collected 2005, plus analytical blanks 54 8. PBDEs (pg/kg, %lipid) in biota collected at Roxboro WWTP outfall and analytical blank 59 9. Matrix (NaSC> 4, sediments and fish tissue) PBDEs fortified recoveries and replicate analysis 63 LIST OF FIGURES Figure Page 1. Representative PBDE structure 4 2. Tetra- to hexa-BDEs in biosolids compared to DE-71 composition 16 3. Hyco River subbasin, North Carolina, U.S. (NCDENR, 2000) 22 4a. Sample locations on lower Marlowe/Storys Creek, Person County, NC. 27 4b. Sample locations on upper Marlowe/Storys Creek and tributaries (Ghent and Storys Creeks), Person County, NC. 28 5a. Representative chromatograph of 27 PBDEs, ptclb and DCDE by on-column injection, ECNI-SIM (DB-5HT, 30 m, 0.25mm i.d., 0.1 pm) 33 5b. Representative chromatograph of 27 PBDEs, ptclb and DCDE by split/splitless injection, ECNI-SIM (DB-5HT, 30 m, 0.25mm i.d., 0.1 pm) 33 6. BDE-209 comparison using on-column and split/splitless injectors 35 7. Relative Retention Indices (RRIs) formula 39 8. ECNI “full-scan” spectra of octa-PBDEs illustrating differences in spectra as a function of bromine positioning 43 9. ECNI-SIM chromatograph of PBDEs in wastewater sludge (#5BW001) 45 10. El chromatograph of PBDE major ions in wastewater sludge (#5BW001) 46 11. ECNI-SIM comparison of sludge collected in 2005 and 2002 48 12a. El spectra of hexabromocyclododecane (HBCD) in sludge 50 12b. El spectra of 1,2-bis (2,4,6-tribromophenoxy) ethane (TBE) in sludge 50 v LIST OF FIGURES (continued) Figures Page 13. ECNI-SIM chromatograph of PBDEs in sediments (#0BS016) and (#5BS003) 51 14. El chromatograph of PBDE major ions in sediment (#5BS003) 52 15. ECNI-SIM chromatograph of PBDEs in biota (#0BF072) 56 16a. El chromatograph of tri- trough hexa-PBDEs major ions in biota (#0BF072) 57 16b. El chromatograph of hepta- through deca-PBDEs major ions in biota (#0BF072) 58 17a. Roxboro WWTP sludge (2002 and 2005) tri- through hexa-PBDEs 65 17b. Roxboro WWTP sludge (2002 and 2005) hepta- through deca-PBDEs 65 18. BDE-209 transfers to Roxboro WWTP (USEPA, TRI. 2006) 67 19. Penta-formulation (DE-71) compared to Roxboro WWTP sludge (2002 and 2005) and U.S. sludges (n=l 1) 69 20. Total PBDEs in Marlowe/Storys Creek surficial sediments, collected from Roxboro WWTP to 10.8 km downstream 71 21a. Marlowe/Storys Creek surficial sediment congener profiles (tri through octa-PBDEs), 2002 and 2005 73 21b. Marlowe/Storys Creek surficial sediments congener profiles (nona- through deca-PBDEs), 2002 and 2005 73 vi LIST OF FIGURES (continued) Figures Page 22. Tetra- through hepta-PBDEs homologue of surficial sediments and sludge (2002 and 2005) compared to DE-71 76 23 a. PBDEs in biota (tri- through hexa-PBDEs) 77 23b. PBDEs in biota (hepta- through deca-PBDEs) 77 24. Chromatograph of PBDEs in creek chub compared to common carp BDE-209 exposure study 81 25. Chromatograph of PBDEs in sunfish compared to rainbow trout BDE-209 exposure study 82 vii ABSTRACT Polybrominated diphenyl ethers (PBDEs) are commonly used brominated flame- retardants (BFRs). They are environmentally persistent and have become widely distributed. PBDEs can bioaccumulate and disrupt biological processes, e.g. the endocrine system. However, identification of their major routes of release into the environment is lacking. To date, the majority of PBDEs detected in biota contain six or fewer bromines, presumably from the recently discontinued commercial penta-PBDE product. However, the dominant PBDE product in commerce, the deca- formulation (containing >97% decabromodiphenyl ether (BDE-209), by weight), remains in commerce, as it is believed to pose comparatively minimal risk. Nonetheless, concerns exist over the possible debromination of deca- into more bioaccumulative congeners. However, this has only been shown under laboratory conditions. To evaluate the potential for debromination under realistic environmental conditions the distribution of PBDE congeners was tracked in a variety of matrices from a wastewater treatment plant (WWTP) sludge to receiving stream sediments and associated aquatic biota. Samples were collected in 2002 and 2005. GC/MS identified tri- through deca-PBDEs in these matrices. BDE-209 was the major congener in sludge (58.8 and 37.4 mg/kg, d.w., respectively), sediments (6.2 to 3150 mg/kg, %TOC) and some biota (non-detect to 21,650 pg/kg, l.w.). Also detected in these matrixes were 22 additional PBDEs, other major congers BDE- 206, -99 and -47 in sludge, -206, -207 and -99 in sediments and BDE-47, -99 and - 153 in biota. Sludge congener profiles were similar to the penta- and deca- formulations, suggesting minimal -209 debromination during wastewater treatment. Similar profiles were also observed in surficial sediments collected at the outfall and several km downstream, again indicating minimal debromination. Sludge and sediments contained additional BFRs of emerging concern, e.g. hexabromocyclododecane (< 8 mg/kg) and 1,2-bis (2,4,6-tribromophenoxy) ethane (<1.1 mg/kg). Sunfish (Lepomis gibbosus), creek chub (Semotilus atromaculatus) and crayfish (Cambarus puncticambarus sp. c) collected in 2002 near the outfall and sunfish collected in 2005, were depurated and whole body PBDE analyses conducted. Sunfish (2002, 2005) profiles were similar, but -209 (2880 pg/kg) was only detected in the 2002 sample. BDE-179, -184, -188, -201 and -202 were also detected in these biota samples, but not in sludges or sediments. A previous laboratory study identified these same BDE-209 debromination products in fish. This suggests that metabolic debromination of -209 does occur in the aquatic environment under realistic conditions. Hence risk assessments that assume no BDE-209 debromination may underestimate associated bioaccumulation and toxicity attributable to the less brominated congeners produced. Disposition of Wastewater-Associated Polybrominated Diphenyl Ethers In a Freshwater Receiving Stream INTRODUCTION Polybrominated diphenyl ethers (PBDEs) [Figure 1] are widely used flame- retardant additives in polymers and textiles. The demand for polymer-based products for electrical and electronic equipment, as well as automotive equipment, construction materials, and textiles has increased over the past decade. Accordingly, the demand for brominated flame-retardants (BFRs) for these products has doubled from an estimated 145,000 metric tonnes (MT) in 1990 to 310,000 MT in 2000 (Alaee et al., 2003). These continue to be produced at high volumes (237,727 and 223,482 MT for 2002 and 2003, respectively) (http://www.bsef.com/bromine/our industry/ (BSEF, 2006)). Of the BFRs, PBDEs were only surpassed by tetrabromobisphenol-A (TBBPA) in regards to production volume (2001 global demand 67,390 versus 119,700 MT respectively (BSEF, 2006)). PBDEs were typically produced commercially at three different levels of bromination, nominally penta-, octa- and deca-PBDEs. The deca-PBDE formulation made up 83.3% of the 2001 PBDE global market demand, followed by penta- 11.1% and octa- 5.6% (BSEF, 2006). PBDEs have been commonly used in furniture (polyurethane foam), wire and cable insulation (styrene copolymers), electronics and computers (high- impact polystyrene). The vast majority of the global penta-PBDE production was consumed in North America (e.g. 98% in 2001), mostly to flame retard polyurethane foams used in furniture padding (Renner, 2000a). However, unlike reactive BFRs like TBBPA, PBDEs are simply blended with the polymers during their formation and thus may migrate from products more readily (Alaee et al., 2003). 2 Since the 1981 report of PBDEs in fish from Sweden (Anderson and Blomkuist, 1981), subsequent papers have documented their widespread distribution in the environment (de Boer et al., 1998, Hale et al., 2001a and Renner, 2000b).
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