In Situ Measurement of PCB Pore Water Concentration Profiles in

Apr 7, 2011 - The study site at South Basin, adjacent to the former Hunters Point Naval Shipyard, San Francisco Bay, CA, has been extensively describe...
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In Situ Measurement of PCB Pore Water Concentration Profiles in Activated Carbon-Amended Sediment Using Passive Samplers Amy M. P. Oen,*,† Elisabeth M. L. Janssen,‡ Gerard Cornelissen,†,§,|| Gijs D. Breedveld,†,^ Espen Eek,† and Richard G. Luthy‡ †

Department of Environmental Technology, Norwegian Geotechnical Institute, 0806 Oslo, Norway Department of Civil and Environmental Engineering, Stanford University, Stanford, California USA 94305-4020 § Department of Plant and Environmental Sciences, University of Life Sciences, Ås, Norway Department of Applied Environmental Sciences, Stockholm University, 10691 Stockholm, Sweden ^ Department of Geosciences, University of Oslo, 0316 Oslo, Norway

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bS Supporting Information ABSTRACT: Vertical pore water profiles of in situ PCBs were determined in a contaminated mudflat in San Francisco Bay, CA, 30 months after treatment using an activated carbon amendment in the upper layer of the sediment. Pore water concentrations were derived from concentrations of PCBs measured in two passive samplers; polyethylene (PE, 51 μm thick) and polyoxymethylene (POM, 17 μm thick) at different sediment depths. To calculate pore water concentrations from PCB contents in the passive samplers, an equilibrium approach and a first-order uptake model were applied, using five performance reference compounds to estimate pore water sampling rates. Vertical pore water profiles showed good agreement among the measurement and calculation methods with variations within a factor of 2, which seems reasonable for in situ measurements. The close agreements of pore water estimates for the two sampler materials (PE and POM) and the two methods used to translate uptake in samplers to pore water concentrations demonstrate the robustness and suitability of the passive sampling approach. The application of passive samplers in the sediment presents a promising method for site monitoring and remedial treatment evaluation of sorbent amendment or capping techniques that result in changes of pore water concentrations in the sediment subsurface.

’ INTRODUCTION Persistent and hydrophobic contaminants accumulate in sediment and thus have the potential to pose long-term ecological and human risks.1 Remediation strategies, whether by dredging, capping, or in situ treatment, aim to mitigate these risks. One possible in situ sediment remediation strategy is the application of a strong sorbent amendment like activated carbon (AC), which has been shown to reduce contaminant availability in sediment due to its strong sorption of hydrophobic organic compounds (HOCs).29 To assess the effectiveness of sediment remediation strategies, there is a need to establish monitoring methods to document remediation performance. The use of passive samplers can be such a tool to measure freely dissolved concentrations of HOCs in aquatic environments.10 The advantage of passive samplers lies in their ability to measure very low aqueous concentrations of HOCs without the conventional and labor-intensive method of sampling and extracting large volumes of surface water. In addition, effects of dissolved organic carbon are circumvented, especially in pore water. Field deployment of passive samplers to measure concentrations of HOCs in the overlying water has included the use of r 2011 American Chemical Society

semipermeable membrane devices (SPMDs),1113 low-density polyethylene (PE),14,15 polydimethylsiloxane (PDMS) as tubing and coatings on glass fibers (solid-phase microextraction, SPME),15 as well as polyoxymethylene (POM).15,16 Although field deployment of passive samplers in the overlying water has become more common, there are only a limited number of studies that have utilized passive samplers to assess in situ pore water concentrations of HOCs in sediment. These studies involve the placement of passive samplers directly into the sediment under laboratory conditions1721 or under field conditions where the passive samplers are placed in the top layer of sediment and are used to calculate one composite pore water concentration value.2123 For these field studies, van der Heijden and Jonker22 successfully deployed SMPE to measure in situ pore water concentrations of polycyclic aromatic hydrocarbons (PAHs) in the upper 3 cm of sediment assuming equilibrium Received: January 15, 2011 Accepted: March 27, 2011 Revised: March 17, 2011 Published: April 07, 2011 4053

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Environmental Science & Technology had been achieved during 4 weeks of exposure. Fernandez et al.21 placed PE impregnated with performance reference compounds (PRCs) in sediment at a field site in Boston Harbor for 1 week of exposure to determine pore water concentrations of PAHs in the upper 16 cm of sediment. Tomaszewski and Luthy23 have also used PE impregnated with PRCs to determine sediment pore water concentrations of polychlorinated biphenyls (PCBs) at a depth of 515 cm in a contaminated mudflat in San Francisco Bay, CA. The aim of the present study is to measure in situ PCB pore water concentrations in vertical profiles from 0 to 40 cm depth below the sediment surface by utilizing two polymer passive samplers PE and POM mounted on a sediment-penetrating rod. This novel application circumvents traditional methods of determining vertical pore water profiles, which include sediment coring and either centrifugation to press out the pore water or employing continuously mixed sediment slurries with the addition of passive samplers.24,25 Furthermore, direct measurement of pore water concentrations is more representative of field conditions, particularly for AC-amended sediments as centrifugation or mixed sediments slurries would enhance the transfer of HOCs from the sediment particles to the AC particles23 and thus probably underestimate actual pore water concentrations. Whereas three previous studies have used passive samplers in situ to measure pore water concentrations in surface sediment, this is the first study to deploy passive samplers in the field to measure freely dissolved concentrations of PCBs in a continuous vertical profile in the sediment. Vertical profiles are advantageous as they provide another dimension (depth) to pore water concentrations and performance assessments of sediment remediation. Although such profiles have been determined using core sediment samples and laboratory measurements, field results are essential as well in order to assess the effectiveness of remedial measures, monitor conditions within the biologically active layer, and inform management decisions.

’ MATERIALS AND METHODS Materials. Additive-free low-density PE (51 μm, Brentwood Plastics, St. Louis, MO) and POM (Astrup, Norway,17 μm, obtained by slicing block cylinders on a lathe equipped with a high-precision razor blade exactly as in Cornelissen et al.15) were precleaned by submerging the materials 24 h in each solvent (hexane, methanol, deionized water) and then allowed to dry at 20 C for 12 h between each solvent rinse. Unexposed laboratory blanks were analyzed and all 118 PCB congeners comprised 0.05). The percent depletion data for the PE (Figure S3 of the Supporting Information) show linear depletion such that it is clear that the approach to equilibrium for the PE is slow and ongoing, as observed earlier for PE under similar conditions and deployment times.23 Figure S4 (of the Supporting Information) summarizes total percent PRC depletion with sediment depth after the total 154 days of deployment. Impregnated PRCs show 20 to 80% depletion from POM and 2 to 90% depletion from PE depending on the degree of chlorination of the five PRCs. The least chlorinated congener, PCB 29 (trichlorobiphenyl), shows greatest depletion whereas the most highly chlorinated congener, PCB 192 (hepta-chlorobiphenyl), shows the least depletion after 154 days of deployment. Although the approach to equilibrium does not require 100% depletion of the PRCs, greater than 90% depletion would have been a strong line of evidence that equilibrium had been achieved. An overall assessment of the PRC depletion data presented in parts ac of Figure 2 and Figures S2S4 of the Supporting Information suggest that equilibrium was not achieved for the PE and possibly not achieved for all of the PRCs in the POM passive samplers within 154 days of deployment. Uptake of in situ PCBs in the POM passive samplers at three different sediment depths for the five exposure times are shown in parts df of Figure 2. Similar results at all sediment depths, including measurements for selected PCBs (PCB 43, PCB 95, PCB 153, PCB 180) and the different homologue groups, are presented in Figures S2 and S3 of the Supporting Information. Uptake of native PCBs in POM over the time exposure series suggests that equilibrium could have been established for the POM after about 100 days where the uptake curves appear to stabilize after 100 days and as mentioned previously, PCB concentrations measured after 100 and 154 days were not significantly different (t test, p > 0.05) for all but the deepest sediment layer. The small disparities between the uptake of native PCBs and the depletion of PRCs observed for the POM could reflect 4056

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Figure 3. Vertical pore water concentration profiles calculated based on (a) assuming equilibrium has been achieved in the POM after 100 days of exposure, (b) depletion of PRCs from the PE and assuming a first-order process uptake model, and (c) depletion of the PRCs from the POM assuming a first-order process uptake model. The dotted lines in (a) and (c) represent the range of concentrations for differences in KPOM values due to differences in the thickness of the POM.

differences in the mass transfer conditions in the aqueous boundary layer. Perhaps the porous media influences the PRC depletion more than native PCB uptake as sediment and AC particles adjacent to the sampler retard the complete elimination of PRCs leading to pseudoequilibrium conditions in the boundary layer with concentrations of PRCs in the pore water greater than zero. This could explain why uptake of in situ PCBs from the sediment to the POM could approach equilibrium, whereas PRCs remain in the POM with not all of the PRCs being fully depleted. Vertical Pore Water Profiles. Because of the varying equilibrium assessment observations presented above, three methods were employed for calculating the vertical, PCB-concentration pore water profiles as shown in Figure 3: (i) assuming equilibrium has been achieved for 17 μm thick POM (POM-17) after about 100 days of exposure in the field, (ii) using the depletion of PRCs from the PE and assuming a first-order process uptake model, and (iii) using the depletion of the PRCs from the POM assuming a first-order process uptake model. Assuming equilibrium, eq 2 was applied to PCB-uptake data in the POM-17. Utilizing the KPOM values35 presented in Table S1 of the Supporting Information for POM that is 76 μm thick (KPOM-76), the vertical pore water profile is determined and illustrated in part a of Figure 3. A sensitivity analysis was conducted for the KPOM-76 values, because POM-17 was utilized in the present study and, as shown by Cornelissen et al.,15 log KPOM values can vary by up to 0.3 log units depending on the thickness of the POM. Thus, the range of pore water concentrations as measured using POM and assuming equilibrium are also shown in part a of Figure 3, for which the log KPOM values are assumed to vary (0.3 log units.

Data in part b of Figure 3 show the vertical pore water concentration profile for PE samplers using the PRC depletion data and eq 3. Concentrations are calculated using the log KPE values27 presented in Table S1 of the Supporting Information. Tomaszewski and Luthy23 utilized a molar volume adjustment to account for differences between the three PRCs used in their study and the HOC of interest. No molar adjustment has been applied here since the five PRCs utilized cover most of the congeners present (94%) in the field contaminated sediments. The application of these uptake models (eq 2 and 3) to SPMDs and PEDs is well-established. However, there is less experience with their application and validation for POM. To our current knowledge, the only study utilizing PRCs for POM36 aimed at measuring PAHs and PCBs in groundwater wells. In those systems, more than 90% dissipation of the PRCs was found and thus equilibrium was assumed. However, in the present study after 154 days of exposure, it was unclear if equilibrium in the POM has been achieved or not. Therefore, the first-order process uptake model was applied to the POM measurements and illustrated in part c of Figure 3. The vertical pore water concentration profile represents the average concentrations and standard deviations for the five retrieval data sets. As in part a of Figure 3, a sensitivity analysis has been conducted for the KPOM-76 values ((0.3 log units) with the results presented as a range of pore water concentrations. The vertical pore water concentration profiles for in situ PCBs in Figure 3 show good agreement for the three different methods that were used to determine the PCB concentrations. Average pore water concentrations in the top 30 cm of sediment ranged from 0.4 to 2.2 ng/l assuming equilibrium had been achieved in the POM, 2.4 to 3.0 ng/l using depletion of PRCs from the PE, 4057

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Environmental Science & Technology and 0.6 to 5.2 ng/l using depletion of PRCs from the POM. Tomaszewski and Luthy23 report a PCB pore water concentration of 7.1 ( 1.8 ng/l in the top 15 cm of sediment 18 months post-treatment (measured in the field with PE and calculated using PRC depletion, Table S4 of the Supporting Information), which represented a 60% reduction of pore water concentrations between the AC-amended (treated) and untreated plots. Similar observations have been reported by Cho et al.27 where 4666% reductions in PCB uptake into SPMDs were observed in the ACamended sediment at Hunter’s Point. The lower currently reported values document a reduction in the PCB pore water concentrations 30 months post-treatment and thus indicate continued effectiveness of the AC amendment (Figure S5 of the Supporting Information). Hale37 has modeled reductions of PCBs over time as measured using PE for a minimally mixed Hunter’s Point sediment with a 3% AC dosage. For PCB 101, the percent reduction after 18 months is about 60% and improves to 80% after 30 months. The average PCB pore water concentration in the top 15 cm for the PE data presented here is about 3 ng/l. This value translates to a reduction of 80%, which is in good agreement with the modeled reductions.37 Average PCB pore water concentrations in the deeper sediment layers ranged from 0.9 to 5.0 ng/l, 5.2 to 9.2 ng/l, and 1.8 to 10.5 ng/l for the three calculation methods employed, respectively. These concentrations are greater than the pore water concentrations in the AC-amended layer; however, they are not as large as pore water concentrations for untreated sediment, which ranged from 13 to 56 ng/l (Table S4 of the Supporting Information). This can be due to traces of AC present in the deeper layer as a result of inhomogeneous distribution during application of the AC as reported by Cho et al.27 In general, the PCB pore water concentrations values only varied by maximally a factor of 2 between the different methods of measurement and calculation, which seems reasonable for in situ measurements. The lower pore water concentrations determined for the POM assuming equilibrium suggest that equilibrium was probably not achieved for the POM. However, these differences (factor of 2) are within the variability of equilibrium partition coefficients for the passive samplers, which can also vary by a factor of at least two,15 and the spatial and temporal variability present in field studies. Implications and Recommendations. Measurements of pore water concentrations are probably the most appropriate chemical indicator of the bioavailable fraction of contaminants in a sediment ecosystem. Passive sampling is an effective method for measuring such in situ pore water concentrations and thus provides a rapid and time-averaged measurement of contaminant availability in sediments. The close agreement among pore water estimates for the two sampler materials (PE and POM) and the different methods used to translate uptake in samplers to pore water concentrations demonstrate the robustness and suitability of the passive sampling approach. These close agreements also support previous studies that have successfully used PRCs to compensate for nonequilibrium conditions.21,23 Thus, shorter deployment times and correcting for PRC depletion could be sufficient for determining pore water concentrations, assuming site specific information is available for the exchange rate coefficients. The deployment time length, however, is probably dependent on the level of contamination at the site. Fernandez et al.21 found 1 week to be sufficient for measuring PAHs in a field site at Boston Harbor. However, when measuring pore water concentrations following dredging,

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capping or amending the sediment, longer deployment times are probably needed due to the expected lower pore water concentrations. Our studies indicate that 12 months is probably sufficient under such conditions. Knowledge regarding vertical pore water concentrations also reflects the effectiveness of in situ treatment as it provides another dimension (depth) to pore water measurements, which is useful when assessing sediment capping and amendment remediation treatments and processes occurring within the biologically active layer. A better understanding of the performance of different sampler materials (e.g., PE and POM) and uniformity in methodologies to calculate pore water concentrations will allow sediment managers and researchers to make a well-informed choice for monitoring and study designs for sediment site remediation.

’ ASSOCIATED CONTENT

bS

Supporting Information. Additional information for the passive sampler  water partition coefficients figures illustrating observations from all sediment depths is provided. This material is available free of charge via the Internet at http://pubs.acs.org.

’ AUTHOR INFORMATION Corresponding Author

*Phone: þ47 2202 3052, e-mail: [email protected].

’ ACKNOWLEDGMENT Project funding was provided through the Strategic Environmental Research and Development Program (SERDP, ER1552), the Norwegian Geotechnical Institute’s research stipend as well as a Leiv Eiriksson stipend and the Opticap project (both funded by the Norwegian Research Council). We gratefully thank Jeanne E. Tomaszewski for communications and data sharing from her field studies at Hunter’s Point. ’ REFERENCES (1) Apitz, S. E.; Davis, J. W.; Finkelstein, K.; Hohreiter, D. W.; Hoke, R.; Jensen, J. H.; Jersak, J.; Kirtay, V. J.; Mack, E. E.; Magar, V. S.; Moore, D.; Reible, D.; Stahl, R. G., Jr. Assessing and managing contaminated sediments: Part I, developing an effective investigation and risk evaluation strategy. Integr. Environ. Assess. Manag. 2005, 1 (1), 2–8. (2) Zimmerman, J. R.; Ghosh, U.; Millward, R. N.; Bridges, T. S.; Luthy, R. G. Addition of carbon sorbents to reduce PCB and PAH bioavailability in marine sediments: Physicochemical tests. Environ. Sci. Technol. 2004, 38 (20), 5458–5464. (3) Millward, R. N.; Bridges, T. S.; Ghosh, U.; Zimmerman, J. R.; Luthy, R. G. 2005. Addition of activated carbon to sediments to reduce PCB bioaccumulation by a polychaete (Neanthes arenaceodentata) and an amphipod (Leptocheirus plumulosus). Environ. Sci. Technol. 2005, 39 (8), 28802887. (4) Werner, D.; Higgins, C. P.; Luthy, R. G. The sequestration of PCBs in Lake Hartwell sediment with activated carbon. Water Res. 2005, 39 (10), 2105–2113. (5) Cornelissen, G.; Breedveld, G. D.; Naes, K.; Oen, A. M. P.; Ruus, A. Bioaccumulation of native polycyclic aromatic hydrocarbons from sediment by a polychaete and a gastropod: Freely dissolved concentrations and activated carbon amendment. Environ. Toxicol. Chem. 2006, 25 (9), 2349–2355. (6) Cho, Y. M.; Smithenry, D. W.; Ghosh, U.; Kennedy, A. J.; Millward, R. N.; Bridges, T. S.; Luthy, R. G. Field methods for amending 4058

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