Global Aquatic Passive Sampling (AQUA-GAPS): Using Passive

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Environ. Sci. Technol. 44, 860–864

Global Aquatic Passive Sampling (AQUA-GAPS): Using Passive Samplers to Monitor POPs in the Waters of the World1 RAINER LOHMANN* University of Rhode Island, Narragansett, Rhode Island DEREK MUIR Environment Canada, Burlington, Ontario

RAINER LOHMANN/ACS DOI 10.1021/ ES800518G

A global passive sampling network for POPs is needed in aquatic environments.

The Stockholm Convention (SC) on persistent organic pollutants (POPs) has highlighted the global risk(s) posed by 1 Editor’s Note: This manuscript was submitted prior to ES&T changing its manuscript parameters for Viewpoints. For the new format, please read the details at http://pubs.acs.org/doi/abs/ 10.1021/es903081n.

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organic contaminants that are persistent, bioaccumulate, are prone to long-range transport, and have the potential to cause adverse effects in humans and wildlife (1). As a result of the SC, monitoring programs are underway to record concentrations of POPs across the globe over time, with atmospheric sampling and human milk as the recommended media (2). The global atmospheric passive sampling (GAPS) program, which utilizes passive air sampling devices at monitoring sites on all continents, mostly in remote regions, has demonstrated the potential for global coverage (3, 4). While data from GAPS addresses the atmospheric compartment and potentially plants and soils exchanging with air, it does not readily address prevailing concentrations or trends in aquatic environments. A major concern with POPs is their biomagnification with top predators that rely on aquatic food webs, including humans, polar bears, seabirds, toothed whales, and seals (2, 5, 6). Often, the consumption of fish, and of marine mammals, is one of the main routes of exposure for humans (7). Hence, being able to sample the presence and longerterm trends of POPs in the water column would provide invaluable information related to long-term (human and aquatic wildlife) exposure. Additionally, monitoring POPs in water would provide vital information on whether reductions in primary emissions of POPs result in reduced concentrations of POPs in receiving waters, and ultimately in global ocean waters and aquatic foodchains. Conversely, as air concentrations of POPs are reduced due to bans and controls on use, oceans could become a major source of POPs to the air-this has been inferred from Arctic and Great Lakes air and water monitoring data (8–10). Deploying passive samplers at these sites coupled with matching air sampling (e.g., (11)) would enable a direct estimation of the direction of air-water exchange fluxes as a response to changing atmospheric concentrations. Concentrations of POPs in receiving surface waters reflect the balance between emissions delivered via rivers and those via atmospheric deposition, rerelease from POPs accumulated in sediments, and volatilization (12). Tracking POPs in water thus provides an important, unique perspective on the effectiveness of reducing emissions and lowering of exposure. Concentrations of POPs in surface water are directly linked to their bioaccumulation in the foodchain (13, 14); hence, knowing dissolved concentrations in the water enables a direct prediction of concentrations in aquatic species using bioaccumulation factors or lipid-water partitioning and food web (trophic) models (15, 16). In several parts of the world, bivalve molluscs are being used as sentinel organisms to reflect on water quality (e.g., “mussel watch”, refs 2, 17–19). Using bivalves for (bio)monitoring has the advantages of directly obtaining data on species consumed by humans, and information on bioaccumulation and bioavailability of POPs under field conditions. However, working with live organisms has several drawbacks that render their global use difficult at best. For example, there is no single species that could be used across the entire world. Purchasing, deploying, and analyzing bivalves is costly and requires trained personnel. Bivalves are generally deployed 10.1021/es902379g

 2010 American Chemical Society

Published on Web 01/28/2010

TABLE 1. Comparison of Equilibrium Partitioning Constants (Kpassive-w) for Different Passive Sampler Matrices Kpassive-w 500 100 200 500

µm µm µm µm

POM sheet PE sheet PDMS tubing silicone rubber sheet

phenanthrene

anthracene

fluoranthene

pyrene

chrysene

benzo(a)pyrene

ref

3.2 3.78 3.23 4.11

3.42 4.37 4.02 4.21

3.67 4.85 4.39 4.62

3.67 5.02 4.41 4.68

4.27 5.56 4.73 5.25

4.42 6.22 4.9 5.69

(41) (41) (41) (42)

near shore, where global trends of POPs are difficult to discern. Lastly, by their very nature, organisms vary individually (lipid content, physiological parameters, seasonal growth, and reproduction, etc.) (2) and in response to their environment, making it challenging to compare results from different stations. We do not suggest replacing sentinel species as biomonitors, but note that they are not well suited to be used as a (new) global tool for monitoring POPs at background sites.

The Case for Passive Samplers For the reasons discussed above we suggest that use of passive samplers in the waters of the world to monitor POPs is most timely. The same type of passive samplers can be used across all waters of the world, ensuring statistically comparable results. Passive samplers are inexpensive, can be deployed by personnel with minimal training, and are sufficiently well characterized to obtain meaningful results. Thus the sampling technology has been established and there is crucial scientific need. A major advantage of passive samplers is that they accumulate nonpolar (apolar) POPs prefentially compared to water, with equilibrium/enrichment factors of 104 to >106 (Table 1) (20, 21). This means that a mere 2 g of polyethylene (PE), for example, effectively captures the equivalent of 20-2000 L of water. This translates into lower detection limits, a higher certainty of reported concentrations, and less concern about contamination: all essential traits to have passive samplers successfully deployed as a global monitoring tool. Certainly, different samplers have been successfully used. Initially, semipermeable membrane devices (SPMDs) in their linear uptake range were used to mimic uptake of PCBs and pesticides by fish (22). More recently, other samplers have become more popular for detecting POPs in surface waters, such as PE, polyoxymethylene (POM),

FIGURE 1. KPE-w as a function of Kow for hydrophobic organic contaminants (based on 21, 41, 42, 44, 45). (Unified Kow values were used, so values differ slightly from those originally published; DDTs were excluded from the best fit linear regression).

silicone-based samplers, and others (20, 23–25). Historically, SPMDs have been most widely used and investigated, but can prove challenging to prepare and analyze due to the use of triolein: one major reason single-matrix samplers are used more frequently. However, as many of these passive samplers are optimized to equilibrate quickly in contaminated environments where detection limits are not of concern (e.g., solid-phase microextraction [SPME] fibers, thin PE, POM and silicone sheets and tubing), these samplers will not be suitable for continuous monitoring of POPs at remote sites. The ideal samplers will combine low cost, high reproducibility, and strong enrichment of POPs with a sufficiently long time to reach equilibrium. Hence, we suggest focusing on passive samplers thick enough to accumulate substantial amounts of POPs at remote sites and equilibrate within weeks to months. By including performance reference compounds in the samplers, the in situ exchange kinetics can be established (26). This will enable scientists to determine for which compounds equilibrium has been reached (i.e., smaller molecular weight POPs with high diffusivities in the passive sampler); for others, results will be corrected for nonequilibrium. At equilibrium (or corrected for nonequilibrium), freely dissolved concentrations (Cw,diss) can be deduced as Cw,diss ) Cpassive/Kpassive-w

(1)

where Kpassive-w is the passive sampler-water partitioning coefficient (Vwater/mpassive), Cpassive is the POP molar concentration in the passive sampler (nPOP/mpassive), and Cw,diss is the freely dissolved molar concentration (nPOP/Vwater). In case of samplers being deployed longer than the time required to reach equilibrium for a given POP, the results are not truly “time-averaged”, but instead reflect more recent pollution events (27). This is of concern in dynamic environments with strongly fluctuating POP concentrations, but we do not expect this to be of concern at the coastal to remote sites targeted for passive sampling, as site selection would heed this limitation. The authors confess to a preference for PE samplers, based on their own experience working with them (11, 28). PE samplers have been found to be very reproducible, more so than other passive samplers (29). PE has been used by numerous groups, and has been validated for a range of apolar POPs (21). The results from different research groups with different PE suppliers all agree very well for apolar contaminants (PAHs, hexachlorobenzene [HCB] and PCBs; see Figure 1). This suggests that PE has the potential to be universally used for global monitoring, with expected comparable results, as PE samplers’ partitioning behavior is known under a range of temperatures and salinities (21). Comparisons suggest that derived dissolved concentrations from PE samplers are within a factor of 2-3 of snapshot water samples extracted with standard solvents (21, 28). PE sheets have also been found to be biomimetic, i.e., that they emulate the body burden of benthic biota (30, 31). They are very inexpensive (PE is the polymer of choice for plastic grocery bags), rugged, and easy to handle, all of which should facilitate their worldwide deployment. Commercial PE VOL. 44, NO. 3, 2010 / ENVIRONMENTAL SCIENCE & TECHNOLOGY

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TABLE 2. Predicted Percent Equilibrium Reached for Different POPs in PE Samplers As a Function of Thickness and Deployment Length (Based on Correlation of log DPE versus log MW (log DPE = -10.2 log MW + 9.6; r2 = 0.77, n = 7); Values from 21, 43) % equilibrium reached 50 µm Deff in PE g1.0 g1.0 g1.0 g1.0

× × × ×

10-14 10-15 10-16 10-17

g1.0 × 10-18

PAHs

PCBs

PCDD/Fs

PBDEs

phenanthrene pyrene benzo(a)pyrene

Cl1B Cl2-3Bs Cl4-5Bs Cl6-7Bs

Cl4DD/Fs Cl5-7DD/Fs

Br2-3DEs Br4DEs

Cl8-10Bs

OCDD/Fs

Br5DEs

Br1DE

sheeting costs on the order of $0.40/m2 (USD), which is a sufficient amount of material to provide samplers to ∼10 sites. Table 1 summarizes the proficiency of PE over other materials. Equilibration times for various apolar POPs in PE as a function of thickness and deployment length are summarized in Table 2. A 50-µm thick PE sampler equilibrates within 2 months with low molecular weight POPs, such as PAHs up to benzo(a)pyrene, pentachlorinated biphenyls, hexachlorocyclohexanes [HCHs], HCB, and 2,3,7,8-tetrachlorodibenzo-p-dioxin [TCDD], while higher molecular weight POPs will remain in the kinetic uptake phase. Equilibrium depends most strongly on the POPs’ diffusion coefficient in PE and on its thickness, but less on the actual deployment time (Table 2). Very high molecular weight compounds (octabrominated diphenyl ethers [BDEs], mirex) remain in the linear uptake phase in 50-µm PE samplers after 2 months, suggesting that other samplers could be used to target these POPs. We note that PEs are uniquely suited to sample apolar or weakly polar compounds, which covers all compounds currently identified as POPs except for perfluorinated alkyl acids (PFAs) such as perfluorooctanesulfonic acid (PFOS). The PFAs are a special case, since, unlike most apolar POPs, they can be analyzed in relatively small volumes (0.5-1 L) in most of the world’s oceans (32). Once passive sampling of POPs in the water has been successfully established, it seems logically desirable that the focus of the global monitoring network will widen toward currently used pesticides and persistent polar organics. A very large range of chemicals in commerce including some pharmaceuticals, microbicides, and other chemicals in personal care products, many with phenolic or carboxylic acid moieties which are anionic at ambient pHs, are emitted to water. These chemicals do not volatilize or strongly sorb to sediments. If they reach off-shore waters of large oligotrophic lakes and seas they may be relatively persistent. Current screening of chemicals for persistence and long-range transport is focused mainly on atmospheric transport. The potential for persistent polar organic chemicals such as perfluorooctanoic acid (PFOA) to be transported long distances in the oceans has only recently been recognized (33, 34). Passive samplers for polar organics, such as the polar organic chemical integrative sampler (POCIS) have been deployed in rivers and in marine environments near point sources (35–37). Therefore it may be possible to codeploy them or other devices optimized for polar compounds, similar to the current trend in the GAPS program to include both “normal” polyurethane foam PUF disks and adsorbent resin-coated (XAD) ones (38).

Where Should Passive Samplers be Deployed in the Water? The aim is to monitor background concentrations of water bodies, such as major lakes, seas, and oceans. Similarly to 862

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pentachlorobenzene HCB, HCHs aldrin, dieldrin, chlordane, DDT, endrin, heptachlor toxaphene

100 µm

1 week

2 months

2 months

100% 93% 35% 11%

100% 100% 90% 32%

100% 100% 51% 16%

4%

10%

5%

the sites currently chosen for the GAPS program, these would represent a mix of sites truly remote from industrial influences to those background sites in heavily populated and industrialized regions. Initially, we suggest making use of existing monitoring buoys in key locations such as the Great Lakes, and other major lakes across the world: e.g., Lakes Tschad, Malawi, and Victoria in Africa; Lake Lagado in Europe; and Lake Baikal in Asia. Furthermore, there are numerous buoys that could be used in seas, such as the North, Baltic, Mediterranean, Caspian, and Black in Eurasia and coastal ocean sites that are in place for mussel watch programs in North America and large parts of Asia. Lastly, many countries are installing or operating coastal observing systems, the aims of which vary from geotechnical warning systems to physical oceanography monitoring, to algal bloom or hypoxia recordings. Deploying passive samplers at remote ocean sites would open up unique possibilities to better understand the buffering capacity of oceans with respect to the global (re)cycling of POPs (39, 40). The only requirement for a given site is that it should be away from a major point source, and temperature (and salinity, where appropriate) data need to be available for the deployment period. As water temperatures do not fluctuate wildly, the temperature could even be recorded by hand during deployment and retrieval. We do not advocate including estuarine/harbor sites, as these reflect local or regional pollution events, privy to national or regional governmental action, as opposed to the long-range (global) transport of POPs addressed by the SC. We suggest deploying passive samplers as a combination of kinetic and equilibrium measuring devices which would result in deployment times of 1-2 months at each site. It should be noted that a potential problem for some sites is seasonal biofouling. However, the information provided by using performance reference compounds will also help understand the degree to which biofouling slowed down equilibration times in the field (26). Based on previous experience, this has not been a major problem, as equilibration times are fastest during warmer temperatures. Scientifically, it would be desirable to coordinate deployment times with the GAPS program, which would suggest deploying during the four seasons per yearsfor example by deploying 2 samplers in the water per season. Initially it seems prudent to deploy passive samplers in the mixed surface waters, where suites of sensors (temperature, salinity, etc.) are often deployed. For cold areas, the deployment would be restricted to the open water season. While we have successfully deployed PE samplers without protection (e.g., 11, 21, 28), nonetheless using stainless steel or copper casings will help guarantee retrieval of samplers and reduce biofouling. Fieldtesting of different deployment devices will help the community in question to find best solutions. This last point beckons the need for a major interlaboratory exercise, including codeployments of different samplers, combined with the training of local scientists in an

effort to create sustainable monitoring networks across the aquatic world. By using low-cost samplers, there will be a unique opportunity that this technology can be applied for additional local to regional studies by researchers across the world once they are trained within the initial deployment program.

A Call to Action In summary, we believe there are major benefits in starting global aquatic passive sampling (AQUA-GAPS) and propose the phased development of an AQUA-GAPS network of stations. The program could be started by initiating monitoring with PE samplers at accessible and relatively well studied key locations e.g., the Great Lakes, U.S. east coast, Baltic, North Seas, Mediterranean, or South China Seas. Investigators with access to ship time and buoys would be invited to participate to locate samplers and if capable, also analyze them. Although analyzing samples in a central lab would be desirable (akin to GAPS), we believe multiple laboratories could be involved provided existence of an interlaboratory quality assurance and training program. The list of POPs to be analyzed would be those readily detected by low-resolution GC-MS and for which analytical standards are readily available (e.g., legacy chlorinated pesticides, lindane, endosulfan, selected PCB congeners, chlorobenzenes, tetra- and pentaBDEs). The program would also encourage deployment of different passive devices for comparison with PE samplers. Some of the SC’s regional and subregional centers for POPs located near deployment sites might want to be involved for their roles of capacity building and technology transfer. We thus seek volunteer investigators to help conduct the initial monitoring phase including the associated costs for passive sampler deployment and analysis. With such cooperation, we can foresee improved monitoring of the global aquatic environment to enhance its and our long-term health. The authors have a background in studying the fate and transport of POPs. Dr Rainer Lohmann is currently an associate professor of oceanography, teaching “Marine Pollution” and “Marine & Environmental Organic Chemistry”. His areas of expertise include the global transport and fate of POPs with a focus on the role of oceans, and the use of passive samplers to detect organic pollutants and predict their bioaccumulation. Derek Muir is a senior research scientist with the Aquatic Ecosystem Protection Research Division of Environment Canada at the Canada Centre for Inland Waters in Burlington, ON. His research interests include identification of new persistent organic pollutants and measurements of these contaminants in lake and oceans waters to support studies of bioaccumulation and biomagnification. Please address all correspondence regarding this article to [email protected].

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