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Seven-day sublethal toxicity tests were performed with the freshwater invertebrates Ceriodaphnia dubia, Hyalella azteca, and Chironomus dilutus to determine the effects of per- or polyfluorinated alkyl substances (PFAS) of varying chain length within four classes: perfluoroalkyl carboxylic acids (PFCAs), perfluoroalkyl sulfonic acids (PFSAs), perfluoroalkane sulfonamides, and fluorotelomer sulfonic acids. In general, toxicity increased with increasing chain length, but the slopes of these relationships varied markedly by species and chemical class. The toxicity of individual PFCAs was similar among species. The toxicity of PFSAs was similar to PFCAs for C. dubia and H. azteca, whereas PFSAs were much more toxic to C. dilutus, with median effect concentrations (EC50s) as low as 0.022 mg perfluorooctane sulfonate (PFOS)/L and 0.012 mg perfluorononane sulfonate (PFNS)/L. Despite the high sensitivity to PFOS and PFNS, C. dilutus was not very sensitive to structurally similar fluorotelomer sulfonates (6:2 and 8:2). Perfluoroalkane sulfonamides were the most toxic class tested among all species (e.g., EC50s of 0.011 and 0.017 mg perfluorooctane sulfonamide/L for C. dilutus and H. azteca, respectively). The differences in toxicity among species and chemical classes suggest that mechanisms of PFAS toxicity may differ as a function of both. Environ Toxicol Chem 2024;43:359-373. Published 2023. This article is a U.S. Government work and is in the public domain in the USA., (Published 2023. This article is a U.S. Government work and is in the public domain in the USA.)

Rainbow trout (Oncorhynchus mykiss) was exposed through the diet to a mixture of non-ionic organic chemicals for 28 d, followed by a depuration phase, in accordance with OECD method 305. The mixture included hexachlorobenzene (HCB), 2,2',5,5'-tetrachlorobiphenyl (PCB-52), 2,2',5,5'-hexachlorobiphenyl (PCB-153), decachlorobiphenyl (PCB-209), decabromodiphenyl ether (BDE209), decabromodiphenyl ethane (DBDPE), bis-(2-ethylhexyl)-3,4,5,6-tetrabromophthalate (TBPH), perchloro-p-terphenyl (p-TCP), perchloro-m-terphenyl (m-TCP), and perchloro-p-quaterphenyl (p-QTCP), the latter six of which are considered highly hydrophobic based on n-octanol/water partition coefficients (K OW ) greater than 10 8 . All chemicals had first-order uptake and elimination kinetics except p-QTCP, whose kinetics could not be verified due to limitations of analytical detection in the elimination phase. For HCB and PCBs, the growth-corrected elimination rates (k 2g ), assimilation efficiencies (α), and biomagnification factors (BMF L ) corrected for lipid content compared well with literature values. For the highly hydrophobic chemicals, elimination rates were faster than the rates for HCB and PCBs, and α's and BMF L s were much lower than those of HCB and PCBs, i.e., ranging from 0.019 to 2.8%, and from 0.000051 to 0.023 (g-lipid/g-lipid), respectively. As a result, the highly hydrophobic organic chemicals were found be much less bioavailable and bioaccumulative than HCB and PCBs. Based on the current laboratory dietary exposures, none of the highly hydrophobic substances would be expected to biomagnify, but Trophic Magnification Factors (TMFs) > 1 have been reported from field studies for TBPH and DBDPE. Additional research is needed to understand and reconcile the apparent inconsistencies in these two lines of evidence for bioaccumulation assessment., (© 2023. This is a U.S. Government work and not under copyright protection in the US; foreign copyright protection may apply.)

The open literature was searched for laboratory toxicity data for marine/estuarine organisms exposed to dichlorodiphenyltrichloroethane (DDT) and its degradation products of dichlorodiphenyldichloroethylene (DDE), dichlorodiphenyldichloroethane (DDD), dichlorodiphenylchloroethylene (DDMU), and dichlorodiphenylchloroethane (DDMS). The goal of the review was to determine water-column toxicity values that could be used for porewater-based assessment of sediment toxicity. Data for individual compounds (and isomers thereof) in this group were very limited; most available data were for mixtures of multiple compounds, some defined and others undefined. Further, the majority of relevant studies involved exposure to spiked or field-contaminated sediment (rather than waterborne exposure), which requires inferring concentration in porewater from bulk sediment. Comparing data on the basis of effect concentrations for water or inferred concentration in sediment pore water, the lower reported effect concentrations were in the range of 0.05 to 0.1 µg/L, generally in studies of longer duration and/or evaluating sub-lethal effects. Because field exposures are generally to mixtures of these compounds in varied proportions, additional data on chemical-specific toxicity would aid in pore-water based toxicity assessment for marine/estuarine sediments contaminated with DDT-related chemicals., (© 2023. This is a U.S. Government work and not under copyright protection in the US; foreign copyright protection may apply.)

The results of a series of experiments on the acute toxicity of major geochemical ions (Na + , K + , Ca 2+ , Mg 2+ , Cl - , SO 4 2- , HCO 3 - /CO 3 2- ) to fathead minnows (Pimephales promelas) are reported. Tests of individual major ion salts in various dilution waters demonstrated that the toxicities of Na, Mg, and K salts decrease as the overall ion content of the dilution water increases. For Na and Mg salts, this is attributable to Ca content as previously reported for Ceriodaphnia dubia. For K salts, the cause is unclear, but it is not due to Na as reported for C. dubia. In an unregulated test at high pH (9.3), NaHCO 3 was also found to be twice as toxic compared to when the pH was reduced to 8.4. Experiments with binary salt mixtures indicated the existence of multiple independent mechanisms of action. These include K-specific toxicity and Ca/Mg-specific toxicity previously reported for C. dubia, but also apparent toxicities related to SO 4 and to high pH/alkalinity in CO 3 /HCO 3 -dominated exposures. Previous work with C. dubia also suggested a general ion toxicity involving all ions that was correlated with osmolarity. For fathead minnow, similar correlations were observed, but multiple mechanisms were indicated. At higher Ca, this general toxicity could be attributable to osmotic effects, but at lower Ca, osmolarity may be more a covariate than a cause, with this toxicity being related to a combined effect of ions other than via osmolarity. Environ Toxicol Chem 2022;41:2078-2094. © 2022 SETAC. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA., (© 2022 SETAC. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA.)

Mathematical models are presented for the acute median lethal concentrations of major geochemical ions (Na + , K + , Ca 2+ , Mg 2+ , Cl - , SO 4 2- , HCO 3 - /CO 3 2- ) to fathead minnows (Pimephales promelas), based on an extensive series of experiments presented in a companion article. Toxicity relationships across different dilution waters, individual salts, and salt mixtures suggest six independent mechanisms of toxicity to consider in modeling efforts, including Mg/Ca-specific toxicity, osmolarity-related toxicity, SO 4 -specific toxicity, K-specific toxicity, effects of high pH/alkalinity, and a multiple ion-related toxicity at low Ca distinct from the other mechanisms. Models are evaluated using chemical activity-based exposure metrics pertinent to each mechanism, but concentration-based alternative models that are simpler to apply are also addressed. These models are compared to those previously provided for Ceriodaphnia dubia, and various issues regarding their application to risk assessments are discussed. Environ Toxicol Chem 2022;41:2095-2106. © 2022 SETAC. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA., (© 2022 SETAC. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA.)

Testicular oocytes in wild adult bass (Micropterus spp.) are considered a potential indication of exposure to estrogenic compounds in municipal, agricultural, or industrial wastewater. However, our ability to interpret links between testicular oocyte occurrence in wild fish species and environmental pollutants is limited by our understanding of normal and abnormal gonadal development. We previously reported low-to-moderate testicular oocyte prevalence (7%-38%) among adult male bass collected from Minnesota waters with no known sources of estrogenic compounds. In the present study, two experiments were conducted in which smallmouth bass (Micropterus dolomieu) fry were exposed to control water or 17-α-ethinylestradiol (EE2) during gonadal differentiation, then reared in clean water for an additional period. Histological samples were evaluated at several time points during the exposure and grow-out periods, and the sequence and timing of gonadal development in the presence of estrogen were compared with that of control fish. Testicular oocytes were not observed in any control or EE2-exposed fish. Among groups exposed to 1.2 or 5.1 ng/L EE2 in Experiment 1 or 3.0 ng/L EE2 in Experiment 2, ovaries were observed in 100% of fish up to 90 days after exposure ceased, and approximately half of those ovaries had abnormal characteristics, suggesting that they likely developed in sex-reversed males. Groups exposed to 0.1, 0.4, or 1.0 ng/L in Experiment 2 developed histologically normal ovaries and testes in proportions not significantly different from 1:1. These findings suggest that, while presumably able to cause sex reversal, juvenile exposure to EE2 may not be a unique cause of testicular oocytes in wild bass, although the long-term outcomes of exposure are unknown. Environ Toxicol Chem 2022;41:1416-1428. © 2022 SETAC. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA., (© 2022 SETAC. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA.)

Passive sampling to quantify net partitioning of hydrophobic organic contaminants between the porewater and solid phase has advanced risk management for contaminated sediments. Direct porewater ( C free ) measures represent the best way to predict adverse effects to biota. However, when the need arises to convert between solid-phase concentration ( C total ) and C free , a wide variation in observed sediment-porewater partition coefficients ( K TOC ) is observed due to intractable complexities in binding phases. We propose a stochastic framework in which a given C total is mapped to an estimated range of C free through variability in passive sampling-derived K TOC relationships. This mapping can be used to pair estimated C free with biological effects data or inversely to translate a measured or assumed C free to an estimated C total . We apply the framework to both an effects threshold for polycyclic aromatic hydrocarbon (PAH) toxicity and an aggregate adverse impact on an assemblage of species. The stochastic framework is based on a "bioavailability ratio" (BR), which reflects the extent to which potency-weighted, aggregate PAH partitioning to the solid-phase is greater than that predicted by default, K OW -based K TOC values. Along a continuum of C total , we use the BR to derive an estimate for the probability that C free will exceed a threshold. By explicitly describing the variability of K TOC and BR, estimates of risk posed by sediment-associated contaminants can be more transparent and nuanced.

The brominated flame retardant bis(2-ethylhexyl)-3,4,5,6-tetrabromophthalate (TBPH) is used widely in consumer items including polyurethane foam used in furniture. Information on its bioaccumulation in aquatic species is limited. In the current study, sediment bioaccumulation tests with the oligochaete Lumbriculus variegatus were performed on a spiked natural sediment equilibrated for 14.5 months. Analysis showed the TBPH used to spike the sediment contained a small amount (0.046% by mass) of mono-(2-ethylhexyl)-3,4,5,6-tetrabromophthalate (TBMEHP), a potential biotransformation product of the parent chemical. Steady-state biota-sediment accumulation factors (BSAFs) of 0.254 and 1.50 (kg organic carbon/kg lipid) were derived for TBPH and TBMEHP, respectively. TBPH had biphasic elimination behavior where 94% of the body burden was depleted within the first 12 h of elimination (i.e., half-life of 1.2 h or less) and the remaining 6% eliminated very slowly thereafter (half-life of 15 days). There was little evidence for biotransformation of either chemical by L. variegatus. This investigation confirms the extremely hydrophobic behavior of TBPH and its impact on its bioavailability.

An emerging Multi-Ion Toxicity (MIT) model for assessment of environmental salt pollution is based on the premise that major ion toxicity to aquatic organisms is related to a critical disturbance of the trans-epithelial potential across the gills (ΔTEP), which can be predicted by electrochemical theory. However, the model has never been evaluated physiologically. We directly tested key assumptions by examining the individual effects of eight different salts (NaCl, Na 2 SO 4 , MgCl 2 , MgSO 4 , KCl, K 2 SO 4 , CaCl 2 , and CaSO 4 ) on measured TEP in three different fish species (fathead minnow, Pimephales promelas = FHM; channel catfish, Ictalurus punctatus = CC; bluegill, Lepomis macrochirus = BG). A geometric concentration series based on previously reported 96-h LC50 values for FHM was used. All salts caused concentration-dependent increases in TEP to less negative/more positive values in a pattern well-described by the Michaelis-Menten equation. The ΔTEP responses for different salts were similar to one another within each species when concentrations were expressed as a percentage of the FHM LC50. A plateau was reached at or before 100 % of the LC50 where the ΔTEP values were remarkably consistent, with only 1.4 to 2.2-fold variation. This relative uniformity in the ΔTEP responses contrasts with 28-fold variation in salt concentration (in mmol L -1 ), 9.6-fold in total dissolved solids, and 7.9-fold in conductivity at the LC50. The Michaelis-Menten Km values (salt concentrations causing 50 % of the ΔTEP max ) were positively related to the 96-h LC50 values. ΔTEP responses were not a direct effect of osmolarity in all species and were related to specific cation rather than specific anion concentrations in FHM. These responses were stable for up to 24 h in CC. The results provide strong physiological support for the assumptions of the MIT model, are coherent with electrochemical theory, and point to areas for future research., (Copyright © 2020 Elsevier B.V. All rights reserved.)

The survival and growth of juvenile fathead minnows were investigated at various combinations of waterborne exposure to arsenate and of dietborne exposure to oligochaete worms which had been exposed to inorganic arsenic. Previous work with rainbow trout established that dietborne arsenic can reduce fish growth at environmentally relevant concentrations and could be more important than waterborne exposures. This was found to be less true for fathead minnows, which were less sensitive to dietborne exposures than rainbow trout, while being as or more sensitive to waterborne exposures. When assessed on the basis of accumulation of total As by the fish, further differences between fathead minnows and rainbow trout were evident. Fathead minnows accumulated relatively more arsenic from water versus diet than trout, and the accumulations at which growth effects occurred in minnows were different for dietborne and waterborne exposure, whereas they were the same for trout. These results suggest complex relationships involving arsenic speciation, toxicokinetics, and toxicodynamics, and underscore a need for care in relating effects information to real-world exposures. The present study also demonstrated the challenges in testing and interpreting growth effects in long-term exposures to fish, because the expression of toxicity can be confounded by the relationship of fish growth to size, the feeding regime, and wet weight versus dry weight relationships., (Published by Elsevier B.V.)

The effects on juvenile rainbow trout survival, growth, food consumption, and food conversion efficiency from dietborne exposures to inorganic arsenic (arsenite, arsenate) and to the organoarsenicals monomethylarsonate (MMA), dimethylarsinate (DMA), and arsenobetaine (AsB) were investigated in two experiments: (1) a 28-d exposure using live diets of oligochaete worms separately exposed via water to these five arsenic compounds and (2) a 56-d exposure using pellet diets prepared from commercial fish food to which arsenite, MMA, or DMA were added. In the live diet experiment, the degree to which worms could be contaminated with the organoarsenicals was limited by toxicity to the worms and other experimental constraints, so that their toxicity relative to inorganic arsenic could not be fully established, but AsB was concluded to have low toxicity, consistent with published results for mammals. For the pellet diet experiment, MMA and DMA were found to be at least an order of magnitude less toxic than inorganic As on the basis of concentration in the diet, as well as much less toxic on the basis of accumulation in the fish. The need to consider speciation in aquatic risk assessments for arsenic was further demonstrated by tissue analyses of three macroinvertebrate species from a mining-impacted stream, which showed large variations in both total arsenic and the relative amounts of inorganic and organic arsenic. Additionally, although effects of arsenic on trout appear to be well correlated with inorganic arsenic, worms were found to be more sensitive to waterborne DMA than to inorganic arsenic, showing that low toxicity of organoarsenicals cannot be assumed for all aquatic organisms. Various difficulties in evaluating and applying studies on dietborne exposures and fish growth are also discussed., (Published by Elsevier B.V.)

In previous work we intensively studied the acute responses of the cladoceran Ceriodaphnia dubia to major geochemical ions (Na + , K + , Ca 2+ , Mg 2+ , Cl - , SO 4 2- , and HCO 3 - /CO 3 2- ), culminating in the development of models to predict acute toxicity from ionic composition. To quantitatively evaluate whether the toxicological behavior of major ions observed for C. dubia extends to chronic toxicity, we conducted 58 chronic toxicity tests with individual major salts and binary mixtures thereof. Chronic responses paralleled those demonstrated previously for acute exposure, specifically 1) similar relative toxicity of individual salts; 2) different Na salts showing similar potency when exposure is expressed as osmolarity; 3) toxicity of Mg, Ca, and K salts related to cation activity; 4) decreased toxicity of Na and Mg salts when Ca activity is increased at less than toxic concentrations; 5) additive behavior for salt mixtures sharing a common cation; and 6) independent behavior for salt mixtures with dissimilar cations, except Mg/Ca mixtures which appeared additive. Acute-to-chronic ratios were fairly consistent among salts, with values of approximately 1.8 for acute 50% lethal concentration (LC50) to chronic 50% effect concentration (EC50) and 2.8 for LC50/EC20 when expressed on an activity basis. Adjusting the previous acute toxicity model for acute-to-chronic ratios yielded chronic models that predict chronic toxicity within the range of intertest variability. Because these models are informed by a wide range of ion mixtures, they should provide robust assessment tools for natural waters enriched with major ions. Environ Toxicol Chem 2019;38:769-783. © Published 2018 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America., (© Published 2018 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America.)

Direct measurement of the n-octanol partition coefficients (K OW ) for highly hydrophobic organic chemicals is extremely difficult because of the extremely low concentrations present in the water phase. n-Butanol/water partition coefficients (K BW ) are generally much lower than K OW due to the increased solubility of solute in the alcohol saturated aqueous phase, and therefore become easier to measure. We measured the K BW for 25 neutral organic chemicals having measured log K OW s ranging from 2 to 9 and 4 additional highly hydrophobic chemicals, with unmeasured K OW s, having estimated log K OW s ranging from 6 to 18. The measured log K BW and log K OW values were linearly related, r 2  = 0.978, and using the regression developed from the data, K OW s were predicted for the 4 highly hydrophobic chemicals with unmeasured K OW s. The resulting predictions were orders of magnitude lower than those predicted by a variety of computational models and suggests the estimates of K OW in the literature for highly hydrophobic chemicals (i.e., log K OW greater than 10) are likely incorrect by several orders of magnitude., (Published by Elsevier Ltd.)

Bioaccumulation of highly hydrophobic chemicals (log K OW  > 8) from contaminated sediments by Lumbriculus variegatus has been studied for relatively few chemicals, and the measured and model predicted biota-sediment accumulation factors (BSAFs) can differ by orders of magnitude. In the current study, sediment bioaccumulation tests with L. variegatus were performed on sediments dosed with chemicals having a wide range of predicted n-octanol/water partition coefficients (K OW ; 10 6 -10 18 ), including some higher than most highly hydrophobic chemicals studied to date. The highly hydrophobic chemicals had biphasic elimination kinetics with compartments A and B having fast and slow elimination kinetics, respectively, and for compartment B, elimination followed first-order kinetics. For compartment A with fast elimination kinetics, the mechanism and its kinetic-order could not be determined. Steady-state BSAFs (kg organic carbon/kg lipid) of 0.015, 0.024, and 0.022 were derived for tetradecachloro-p-terphenyl, tetradecachloro-m-terphenyl, and octadecachloro-p-quaterphenyl, respectively. The high uncertainty in predicted K OW s for highly hydrophobic chemicals limited the comparison and evaluation of predicted BSAFs from the Arnot-Gobas food web model and BSAFs measured in this study. The results of this study point to the need to perform dietary assimilation efficiency studies with highly hydrophobic compounds to resolve uncertainties surrounding the estimation of their K OW and the need to understand mechanism and models for the biphasic elimination kinetics.

Freshwater mussels (order Unionoida) are one of the most imperiled groups of animals in the world. However, many ambient water quality criteria and other environmental guideline values do not include data for freshwater mussels, in part because mussel toxicity test methods are comparatively new and data may not have been available when criteria and guidelines were derived. The objectives of the present study were to evaluate the acute toxicity of sodium chloride (NaCl) and potassium chloride (KCl) to larvae (glochidia) and/or juveniles of a unionid mussel (fatmucket, Lampsilis siliquoidea) and to determine the potential influences of water hardness (50, 100, 200, and 300 mg/L as CaCO 3 ) and other major ions (Ca, K, SO 4 , or HCO 3 ) on the acute toxicity of NaCl to the mussels. From the KCl test, the 50% effect concentration (EC50) for fatmucket glochidia was 30 mg K/L, similar to or slightly lower than the EC50s for juvenile fatmucket (37-46 mg K/L) tested previously in our laboratory. From the NaCl tests, the EC50s for glochidia increased from 441 to 1597 mg Cl/L and the EC50s for juvenile mussels increased from 911 to 3092 mg Cl/L with increasing water hardness from 50 to 300 mg/L. Increasing K from 0.4 to 1.9 mg/L, SO 4 from 13 to 40 mg/L, or HCO 3 from 44 to 200 mg/L in the 50 mg/L hardness water did not substantially change the NaCl EC50s for juvenile mussels, whereas increasing Ca from 9.9 to 42 mg/L increased the EC50s by a factor of 2. The overall results indicate that glochidia were equally or more sensitive to NaCl and KCl compared with juvenile mussels and that the increased water hardness ameliorated the acute toxicity of NaCl to glochidia and juveniles. These responses rank fatmucket among the most acutely sensitive freshwater organisms to NaCl and KCl. Environ Toxicol Chem 2018;37:3041-3049. © 2018 SETAC. This article is a US government work and, as such, is in thepublic domain in the United States of America., (© 2018 SETAC. This article is a US government work and, as such, is in thepublic domain in the United States of America.)

Field and laboratory studies have shown that mayflies (Ephemeroptera) tend to be relatively sensitive to elevated major ion concentrations, but little is known about how ionic composition influences these responses. The present study evaluated the acute toxicity of major ion salts to the mayfly Neocloeon triangulifer over a range of background water quality conditions. The mayfly was particularly sensitive to Na 2 SO 4 , with the median lethal concentration (LC50) of 1338 mg SO 4 /L being lower than LC50s reported for 7 other species at that hardness. Increasing hardness of the dilution water from 30 to 150 mg/L (as CaCO 3 ) resulted in doubling of LC50s for sodium salts, and an approximately 1.5-fold increase in LC50 for MgSO 4 . Potassium salt toxicity was not strongly influenced by hardness, consistent with findings for other species. When hardness was held constant but the Ca to Mg ratio was manipulated, the ameliorative effect on Na 2 SO 4 and NaCl did not appear as strong as when hardness was varied; but for MgSO 4 the amelioration relative to Ca activity was similar between the 2 experiments. The toxicity of K salts to N. triangulifer was similar to Na salts on a millimolar basis, which contrasts with several other species for which K salts have been much more toxic. In addition, the toxicity of KCl to N. triangulifer was not notably affected by Na concentration, as has been shown for Ceriodaphnia dubia. Finally, plotting LC50s in terms of ion activity (Cl, SO 4 , Na, Mg, or K) over the range of Ca activities in dilution water resulted in significant positive relationships, with comparable slopes to those previously observed for C. dubia over the same range of Ca activities. Environ Toxicol Chem 2018;37:1330-1339. © 2018 SETAC., (© 2018 SETAC.)

Based on previous research on the acute toxicity of major ions (Na + , K + , Ca 2+ , Mg 2+ , Cl - , SO 4 2- , and HCO 3 - /CO 3 2- ) to Ceriodaphnia dubia, a mathematical model was developed for predicting the median lethal concentration (LC50) for any ion mixture, excepting those dominated by K-specific toxicity. One component of the model describes a mechanism of general ion toxicity to which all ions contribute and predicts LC50s as a function of osmolarity and Ca activity. The other component describes Mg/Ca-specific toxicity to apply when such toxicity exceeds the general ion toxicity and predicts LC50s as a function of Mg and Ca activities. This model not only tracks well the observed LC50s from past research used for model development but also successfully predicts LC50s from new toxicity tests on synthetic mixtures of ions emulating chemistries of various ion-enriched effluents and receiving waters. It also performs better than a previously published model for major ion toxicity. Because of the complexities of estimating chemical activities and osmolarity, a simplified model based directly on ion concentrations was also developed and found to provide useful predictions. Environ Toxicol Chem 2018;37:247-259. Published 2017 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America., (Published 2017 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America.)

Testicular oocytes (TOs) have been found in black bass (Micropterus spp.) from many locations in North America. The presence of TOs is often assumed to imply exposure to estrogenic endocrine disrupting compounds (EDCs); however, a definitive causal relationship has yet to be established, and TO prevalence is not consistently low in fish from areas lacking evident EDC sources. This might indicate any of a number of situations: 1) unknown or unidentified EDCs or EDC sources, 2) induction of TOs by other stressors, or 3) testicular oocytes occurring spontaneously during normal development. In the present study, we analyzed TO occurrence in smallmouth bass (Micropterus dolomieu) from 8 populations in northeastern Minnesota watersheds with differing degrees of human development and, hence, presumed likelihood of exposure to anthropogenic chemicals. Three watersheds were categorized as moderately developed, based on the presence of municipal wastewater discharges and higher human population density (4-81 per km 2 ), and 5 watersheds were minimally developed, with very low human population density (0-1 per km 2 ) and minimal built environment. Testicular tissues from mature fish were evaluated using a semiquantitative method that estimated TO density, normalized by cross-sectional area. Testicular oocyte prevalence and density among populations from moderately developed watersheds was higher than in populations from minimally developed watersheds. However, TO prevalence was unexpectedly high and variable (7-43%) in some populations from minimally developed watersheds, and only weak evidence was found for a relationship between TO density and watershed development, suggesting alternative or more complex explanations for TO presence in smallmouth bass from this region. Environ Toxicol Chem 2017;36:3424-3435. © 2017 SETAC., (© 2017 SETAC.)

Many human activities increase concentrations of major geochemical ions (Na +1 , K +1 , Ca +2 , Mg +2 , Cl -1 , SO 4 -2 , and HCO 3 -1 /CO 3 -2 ) in freshwater systems, and can thereby adversely affect aquatic life. Such effects involve several toxicants, multiple toxicity mechanisms, various ion interactions, and widely varying ion compositions across different water bodies. Previous studies of individual salt toxicities have defined some useful relationships; however, adding single salts to waters results in atypical compositions and does not fully address mixture toxicity. To better understand mechanisms and interactions for major ion toxicity, 29 binary mixture experiments, each consisting of 7 to 8 toxicity tests, were conducted on the acute toxicity of major ion salts and mannitol to Ceriodaphnia dubia. These tests showed multiple mechanisms of toxicity, including: 1) nonspecific ion toxicity, correlated with osmolarity and to which all ions contribute; and 2) cation-dependent toxicities for potassium (K), magnesium (Mg), and calcium (Ca) best related to their chemical activities. These mechanisms primarily operate independently, except for additive toxicity of Mg-dependent and Ca-dependent toxicities. These mixture studies confirmed ameliorative effects of Ca on sodium (Na) and Mg salt toxicities and of Na on K salt toxicity, and further indicated lesser ameliorative effects of Ca on K salt toxicity and Mg on Na salt toxicity. These results provide a stronger basis for assessing risks from the complex mixtures of ions found in surface waters. Environ Toxicol Chem 2017;36:1525-1537. Published 2016 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America., (Published 2016 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America.)

The ions Na + , K + , Ca 2+ , Mg 2+ , Cl - , SO 4 2- , and HCO 3 - /CO 3 2- (referred to in the present study as "major ions") are present in all freshwaters and physiologically required by aquatic organisms but can increase to harmful levels from a variety of anthropogenic activities. It is also known that the toxicities of major ion salts can vary depending on the concentrations of other ions, and understanding these relationships is key to establishing appropriate environmental limits. The authors present a series of experiments with Ceriodaphnia dubia to evaluate the acute toxicity of 12 major ion salts and to determine how toxicity of these salts varies as a function of background water chemistry. All salts except CaSO 4 and CaCO 3 were acutely toxic below saturation, with the lowest median lethal concentrations found for K salts. All 10 salts that showed toxicity also showed some degree of reduced toxicity as the ionic content of the background water increased. Experiments that independently varied Ca:Mg ratio, Na:K ratio, Cl:SO 4 ratio, and alkalinity/pH demonstrated that Ca concentration was the primary factor influencing the toxicities of Na and Mg salts, whereas the toxicities of K salts were primarily influenced by the concentration of Na. These experiments also indicated multiple mechanisms of toxicity and suggested important aspects of dosimetry; the toxicities of K, Mg, and Ca salts were best related to the chemical activity of the cation, whereas the toxicities of Na salts also reflected an influence of the anions and were well correlated with osmolarity. Understanding these relationships between major ion toxicity and background water chemistry should aid in the development of sensible risk-assessments and regulatory standards. Environ Toxicol Chem 2016;35:3039-3057. Published 2016 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America., (Published 2016 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America.)

Studies have been conducted to refine US Environmental Protection Agency, ASTM International, and Environment Canada standard methods for conducting 42-d reproduction tests with Hyalella azteca in water or in sediment. Modifications to the H. azteca method include better-defined ionic composition requirements for exposure water (i.e., >15 mg/L of chloride and >0.02 mg/L of bromide) and improved survival, growth, and reproduction with alternate diets provided as increased rations over time in water-only or whole-sediment toxicity tests. A total of 24 laboratories volunteered to participate in the present interlaboratory study evaluating the performance of H. azteca in 42-d studies in control sand or control sediment using the refined methods. Improved growth and reproduction of H. azteca was observed with 2 alternate diets of 1) ramped diatoms (Thalassiosira weissflogii) + ramped Tetramin or 2) yeast-cerophyll-trout chow (YCT) + ramped Tetramin, especially when compared with results from the traditional diet of 1.8 mg YCT/d. Laboratories were able to meet proposed test acceptability criteria and in most cases had lower variation in growth or reproduction compared with previous interlaboratory studies using the traditional YCT diet. Laboratory success in conducting 42-d H. azteca exposures benefited from adherence to several key requirements of the detailed testing, culturing, and handling methods. Results from the present interlaboratory study are being used to help revise standard methods for conducting 10-d to 42-d water or sediment toxicity exposures with H. azteca. Environ Toxicol Chem 2016;35:2439-2447. © 2016 SETAC., (© 2016 SETAC.)

At contaminated sediment sites, the bioavailability of contaminants in sediments is assessed using sediment-bioaccumulation tests with Lumbriculus variegates (Lv). The testing protocols recommend that ratio of total organic carbon (TOC) in sediment to L. variegatus (dry weight) (TOC/Lv) should be no less than 50:1. Occasionally, this recommendation is not followed, especially with sediments having low TOC, e.g., <1 %. This study evaluated the impacts and resulting biases in the testing results when the recommendation of "no less than 50:1" is not followed. In the study, seven sediments were tested with a series of TOC/Lv ratios that spanned the recommendation. With increasing loading of organisms, growth of the organisms decreased in six of the seven sediments tested. Residues of polychlorinated biphenyls (PCBs) in the L. variegatus were measured in six of the seven sediments tested, and differences in PCB residues among loading ratios across all sediments were small, i.e., ±50 %, from those measured at the minimum recommended ratio of 50:1 TOC/Lv. In all sediment, PCB residues increased with increasing loading of the organisms for the mono-, di-, and tri-chloro-PCBs. For tetra-chloro and heavier PCBs, residues increased with increasing loading of organisms for only two of the six sediments. PCB residues were not significantly different between TOC/Lv loadings of 50:1 and mid-20:1 ratios indicating that equivalent results can be obtained with TOC/Lv ratios into the mid-20:1 ratios. Overall, the testing results suggest that when testing recommendation of 50:1 TOC/Lv is not followed, potential biases in the biota-sediment accumulations factors from the sediment-bioaccumulation test will be small.

The acute and chronic toxicity of sulfate (tested as sodium sulfate) was determined in diluted well water (hardness of 100 mg/L and pH 8.2) with a cladoceran (Ceriodaphnia dubia; 2-d and 7-d exposures), a midge (Chironomus dilutus; 4-d and 41-d exposures), a unionid mussel (pink mucket, Lampsilis abrupta; 4-d and 28-d exposures), and a fish (fathead minnow, Pimephales promelas; 4-d and 34-d exposures). Among the 4 species, the cladoceran and mussel were acutely more sensitive to sulfate than the midge and fathead minnow, whereas the fathead minnow was chronically more sensitive than the other 3 species. Acute-to-chronic ratios ranged from 2.34 to 5.68 for the 3 invertebrates but were as high as 12.69 for the fish. The fathead minnow was highly sensitive to sulfate during the transitional period from embryo development to hatching in the diluted well water, and thus, additional short-term (7- to 14-d) sulfate toxicity tests were conducted starting with embryonic fathead minnow in test waters with different ionic compositions at a water hardness of 100 mg/L. Increasing chloride in test water from 10 mg Cl/L to 25 mg Cl/L did not influence sulfate toxicity to the fish, whereas increasing potassium in test water from 1 mg K/L to 3 mg K/L substantially reduced the toxicity of sulfate. The results indicate that both acute and chronic sulfate toxicity data, and the influence of potassium on sulfate toxicity to fish embryos, need to be considered when environmental guidance values for sulfate are developed or refined., (Published 2015 SETAC. This article is a US Government work and is in the public domain in the United States.)

The strain of Hyalella azteca (Saussure: Amphipoda) commonly used for aquatic toxicity testing in the United States has been shown to perform poorly in some standardized reconstituted waters frequently used for other test species. In 10-d and 42-d experiments, the growth and reproduction of the US laboratory strain of H. azteca was shown to vary strongly with chloride concentration in the test water, with declining performance observed below 15 mg/L to 20 mg/L. In contrast to the chloride-dependent performance of the US laboratory strain of H. azteca, growth of a genetically distinct strain of H. azteca obtained from an Environment Canada laboratory in Burlington, Ontario, Canada, was not influenced by chloride concentration. In acute toxicity tests with the US laboratory strain of H. azteca, the acute toxicity of sodium nitrate increased with decreasing chloride in a pattern similar not only to that observed for control growth, but also to previous acute toxicity testing with sodium sulfate. Subsequent testing with the Burlington strain showed no significant relationship between chloride concentration and the acute toxicity of sodium nitrate or sodium sulfate. These findings suggest that the chloride-dependent toxicity shown for the US laboratory strain may be an unusual feature of that strain and perhaps not broadly representative of aquatic organisms as a whole., (© 2015 SETAC.)

The objective of the present study was to evaluate the relative sensitivity of test organisms in exposures to dilutions of a highly toxic sediment contaminated with metals and organic compounds. One dilution series was prepared using control sand (low total organic carbon [TOC; <0.1%, low binding capacity for contaminants]) and a second dilution series was prepared using control sediment from West Bearskin Lake, Minnesota, USA (high TOC [∼10% TOC, higher binding capacity for contaminants]). Test organisms included an amphipod (Hyalella azteca; 10-d and 28-d exposures), a midge (Chironomus dilutus; 20-d and 48-d exposures started with <1-h-old larvae, and 13-d and 48-d exposures started with 7-d-old larvae), and a unionid mussel (Lampsilis siliquoidea; 28-d exposures). Relative species sensitivity depended on the toxicity endpoint and the diluent. All 3 species were more sensitive in sand dilutions than in West Bearskin Lake sediment dilutions. The <1-h-old C. dilutus were more sensitive than 7-d-old C. dilutus, but replicate variability was high in exposures started with the younger midge larvae. Larval biomass and adult emergence endpoints of C. dilutus exhibited a similar sensitivity. Survival, weight, and biomass of H. azteca were more sensitive endpoints in 28-d exposures than in 10-d exposures. Weight and biomass of L. siliquoidea were sensitive endpoints in both sand and West Bearskin Lake sediment dilutions. Metals, ammonia, oil, and other organic contaminants may have contributed to the observed toxicity., (© 2015 The Authors. Published by SETAC.)

Standard sediment-bioaccumulation test methods specify that Lumbriculus variegatus should not be fed during the 28-day exposure. This lack of feeding can lead to decreases in L. variegatus weight and lipid content during the 28-day exposure period. Differences in intrinsic nutritional content of sediments could lead to additional variability in organism performance and/or contaminant uptake. To evaluate the potential benefits of feeding, sediment-bioaccumulation tests were performed comparing treatments with and without supplemental feeding with tropical fish food and also comparing performance food introduced as blended slurry versus fine flakes. The ration of food provided had to be limited to 6 mg/300-mL beaker with 250 mg of L. variegatus (ww) receiving three feedings per week to maintain acceptable dissolved oxygen (DO) in the test chambers. Relative weight change during exposure varied across sediments in the absence of food from very little change to as much as a 40 % decrease from starting weight. Feeding slurry and flake foods increased the total weight of recovered organisms by 32 and 48 %, respectively, but they did not decrease variability in weight changes across sediments. Lipid contents of the organisms decreased similarly across all feeding treatments during the test. At test termination, lipid contents of L. variegatus across unfed, slurry-fed, and flake-fed treatments were not significantly different per Tukey's honest significant difference test with 95 % family-wise confidence. Feeding resulted in polychlorinated biphenyl residues in L. variegatus being generally slightly less (median 78 %) and slightly greater (median 135 %) than the unfed treatments with slurry and flake formulated foods, respectively.

Review of data from several contaminated sediment sites suggested that biota-sediment accumulation factors (BSAFs) declined with increasing contaminant concentrations in the sediment. To evaluate the consistency and possible causes of this behavior, polychlorinated biphenyl (PCB)-contaminated sediment samples from the Hudson, Grasse, and Fox River Superfund sites were used in sediment bioaccumulation tests with the freshwater oligochaete, Lumbriculus variegatus, with PCB concentrations in interstitial water (IW) quantified using polyoxymethylene passive samplers. Measured BSAFs tended to decrease with increasing PCB concentration in sediment, especially for the more highly chlorinated congeners. Measures of partitioning between sediment, IW, and oligochaetes showed that measured sediment-IW partition coefficients (KTOC ) tended to increase slightly with increasing sediment contamination, whereas the ratio of tissue PCB to IW PCB tended to decrease with increasing concentration in IW. Variation in accumulation among sediments was clearly influenced by bioavailability, as reflected by IW measurements, although the specific cause of varying KTOC was not clear. Calculated partitioning between IW and organism lipid (Klipid ) indicated that accumulation was generally 5 to 10-fold higher than would be predicted if Klipid was approximately equal to the n-octanol-water partition coefficient (KOW ). While affirming previous observations of decreasing BSAFs with increasing PCB contamination, the relatively shallow slope of the observed relationship in the current data may suggest that this concentration dependence is not a major uncertainty in sediment risk assessment, particularly if measurements of PCBs in IW are incorporated., (Copyright © 2013 SETAC.)

Globally, estimated costs to manage (i.e., remediate and monitor) contaminated sediments are in the billions of U.S. dollars. Biologically based approaches for assessing the contaminated sediments which pose the greatest ecological risk range from toxicity testing to benthic community analysis. In addition, chemically based sediment quality guidelines (SQGs) provide a relatively inexpensive line of evidence for supporting these assessments. The present study summarizes a mechanistic SQG based on equilibrium partitioning (EqP), which uses the dissolved concentrations of contaminants in sediment interstitial waters as a surrogate for bioavailable contaminant concentrations. The EqP-based mechanistic SQGs are called equilibrium partitioning sediment benchmarks (ESBs). Sediment concentrations less than or equal to the ESB values are not expected to result in adverse effects and benthic organisms should be protected, while sediment concentrations above the ESB values may result in adverse effects to benthic organisms. In the present study, ESB values are reported for 34 polycyclic aromatic hydrocarbon, 32 other organic contaminants, and seven metals (cadmium, chromium, copper, nickel, lead, silver, zinc). Also included is an overview of EqP theory, ESB derivation, examples of applying ESB values, and considerations when using ESBs. The ESBs are intended as a complement to existing sediment-assessment tools, to assist in determining the extent of sediment contamination, to help identify chemicals causing toxicity, and to serve as targets for pollutant loading control measures., (Copyright © 2012 SETAC.)

Previous work demonstrated reduced growth of rainbow trout receiving diets containing environmentally relevant concentrations of arsenic, but did not address the relative and combined potency of waterborne and dietborne exposures. In the current study, juvenile rainbow trout were exposed for 28d to a range of arsenic concentrations in water and in a live oligochaete diet, separately and in combination. In clean water, fish fed worms previously exposed to arsenate at 4 or 8mg As/L showed pronounced reductions in growth, but fish exposed to these same water concentrations and a clean diet experienced less or no effect. Increasing waterborne arsenate to 16 or 32mg As/L had substantial effects on both growth and survival, and simultaneous exposure via both routes intensified growth effects, but not mortality. Growth reduction was strongly correlated to total arsenic accumulation in the fish tissue, regardless of the route of exposure, but mortality was better correlated to waterborne arsenic concentration. The relative concentration of total arsenic in fish viscera and in the remaining carcass was not a useful indicator of exposure route. Speciation analysis showed that most arsenate was converted to arsenite within the worms, but organoarsenic species were not found. The greater toxicity of dietborne exposure when fish and prey were exposed to the same waterborne arsenate concentration emphasizes the need to address dietborne exposure when assessing the aquatic risks of arsenic contamination. This is of particular concern because risk from dietary exposure may occur at even lower water concentrations than used here when prey organisms are exposed for longer periods and via multiple routes., (Published by Elsevier B.V.)

The objective of this work is to present a critical review of the application of the tissue residue approach (TRA) in ecological risk and/or impact assessment (ERA) of chemical stressors and environmental criteria development. A secondary goal is to develop a framework for integrating the TRA into ecological assessments along with traditional, exposure concentration-based assessment approaches. Although widely recognized for its toxicological appeal, the utility of the TRA in specific applications will depend on numerous factors, such as chemical properties, exposure characteristics, assessment type, availability of tissue residue-response data, and ability to quantify chemical exposure. Therefore, the decision to use the TRA should include an evaluation of the relative strengths, limitations, and uncertainties among exposure and residue-based methods for characterizing toxicological effects. Furthermore, rather than supplanting exposure concentration-based toxicity assessments, the TRA can be highly effective for evaluating and reducing uncertainty when used in a complementary manner (e.g., when evaluating multiple lines of evidence in field studies). To address limitations with the available tissue residue-response data, approaches for extrapolating residue-based toxicity data across species, tissues, and exposure durations are discussed. Some of these approaches rely on predicted residue-response relationships or toxicological models that have an implicit residue-response basis (e.g., biotic ligand model). Because risk to an organism is a function of both its exposure potential and inherent sensitivity (i.e., on a residue basis), bioaccumulation models will be required not only for translating tissue residue criteria into corresponding water and sediment criteria, but also for defining the most vulnerable species in an assemblage (i.e., highly exposed and highly sensitive species). Application of the TRA in ecological assessments and criteria development are summarized for bioaccumulative organic chemicals, TBT, and in situ bioassays using bivalve molluscs., (Copyright © 2010 SETAC.)

The volume of sediment required to perform a sediment toxicity bioassay is a major driver of the overall cost associated with that bioassay. Sediment volume affects bioassay cost because of sediment collection, transportation, storage, and disposal costs as well as labor costs associated with organism recovery at the conclusion of the exposure. The objective of the current study was to evaluate reduced sediment volume versions of the standard U.S. Environmental Protection Agency (U.S. EPA) 10-d acute Leptocheirus plumulosus method that uses a beaker size of 1,000 ml and 20 organisms. The test design used evaluated the effects of beaker size (250 and 100 ml) and associated sediment volume (75 and 30 ml, respectively) as well as organism loading density (10 and 20 organisms) on test endpoint responsiveness relative to the standard 10-d test method. These comparisons were completed with three different types of contaminated sediments: a field-collected polycyclic aromatic hydrocarbon (PAH)-contaminated sediment, a lead-spiked control sediment, and a control sediment spiked with mineral oil. Assessment criteria included test endpoint sensitivity, endpoint consistency, statistical power, water quality, and logistical assessments. Results indicate that the current U.S. EPA method is preferable to the reduced sediment volume methods we assessed, but that a 250-ml beaker/10 organism experimental design is of comparable utility and may be advantageous when reduced sediment volumes are desirable because of high contaminant (spiking studies) or sediment disposal costs. In addition, the results of the current study provide toxicity reference values for PAHs, lead, and an oil surrogate for petroleum hydrocarbons., (Copyright © 2010 SETAC.)

Ecological risk assessors face increasing demands to assess more chemicals, with greater speed and accuracy, and to do so using fewer resources and experimental animals. New approaches in biological and computational sciences may be able to generate mechanistic information that could help in meeting these challenges. However, to use mechanistic data to support chemical assessments, there is a need for effective translation of this information into endpoints meaningful to ecological risk-effects on survival, development, and reproduction in individual organisms and, by extension, impacts on populations. Here we discuss a framework designed for this purpose, the adverse outcome pathway (AOP). An AOP is a conceptual construct that portrays existing knowledge concerning the linkage between a direct molecular initiating event and an adverse outcome at a biological level of organization relevant to risk assessment. The practical utility of AOPs for ecological risk assessment of chemicals is illustrated using five case examples. The examples demonstrate how the AOP concept can focus toxicity testing in terms of species and endpoint selection, enhance across-chemical extrapolation, and support prediction of mixture effects. The examples also show how AOPs facilitate use of molecular or biochemical endpoints (sometimes referred to as biomarkers) for forecasting chemical impacts on individuals and populations. In the concluding sections of the paper, we discuss how AOPs can help to guide research that supports chemical risk assessments and advocate for the incorporation of this approach into a broader systems biology framework.

Minimum dissolved oxygen requirements are part of standard guidelines for toxicity testing of freshwater sediments with several benthic invertebrates, but the data underlying these requirements are somewhat sparse. We exposed three common test organisms to ranges of dissolved oxygen concentrations to determine their responses in 10-d exposures, relative to published guidelines for sediment toxicity tests. The oligochaete, Lumbriculus variegatus, showed 100% survival in all exposures down to the lowest concentration tested, 0.7 mg O(2)l(-1). Midge (Chironomus dilutus) larva showed a more pronounced response; while survival was less than 90% only below 1.0mg O(2)l(-1), the biomass endpoint showed EC(50), EC(20), and EC(10) values of 1.00 (0.91-1.10), 1.41 (1.16-1.71), and 1.67 (1.25-2.24) mg O(2)l(-1). The amphipod, Hyalella azteca, showed no adverse effects at concentrations as low as 2.12 mg O(2)l(-1). The combination of these data with other literature data suggest that DO minima in current North American 10-d sediment test guidelines are reasonable.

Studies of fish communities of streams draining mining areas suggest that sculpins (Cottus spp.) may be more sensitive than salmonids to adverse effects of metals. We compared the toxicity of zinc, copper, and cadmium to mottled sculpin (C. bairdi) and rainbow trout (Onchorhynchus mykiss) in laboratory toxicity tests. Acute (96-h) and early life-stage chronic (21- or 28-d) toxicity tests were conducted with rainbow trout and with mottled sculpins from populations in Minnesota and Missouri, USA, in diluted well water (hardness = 100 mg/L as CaCO3). Acute and chronic toxicity of metals to newly hatched and swim-up stages of mottled sculpins differed between the two source populations. Differences between populations were greatest for copper, with chronic toxicity values (ChV = geometric mean of lowest-observed-effect concentration and no-observed-effect concentration) of 4.4 microg/L for Missouri sculpins and 37 microg/L for Minnesota sculpins. Cadmium toxicity followed a similar trend, but differences between sculpin populations were less marked, with ChVs of 1.1 microg/L (Missouri) and 1.9 microg/L (Minnesota). Conversely, zinc was more toxic to Minnesota sculpins (ChV = 75 microg/L) than Missouri sculpins (chronic ChV = 219 microg/L). Species-average acute and chronic toxicity values for mottled sculpins were similar to or lower than those for rainbow trout and indicated that mottled sculpins were among the most sensitive aquatic species to toxicity of all three metals. Our results indicate that current acute and chronic water quality criteria for cadmium, copper, and zinc adequately protect rainbow trout but may not adequately protect some populations of mottled sculpins. Proposed water quality criteria for copper based on the biotic ligand model would be protective of both sculpin populations tested.

The hazard for photoactivated toxicity of polycyclic aromatic hydrocarbons (PAHs) has been clearly demonstrated; however, to our knowledge, the risk in contaminated systems has not been characterized. To address this question, a median lethal dose (LD50) for fluoranthene photoactivated toxicity in medaka (Orvzias latipes) embryos was determined experimentally and then compared with ultraviolet-A (UV-A; 320-400 nm) radiation exposures in a PAH-contaminated field site. The dose metric, J/cm2/ microg fluoranthene/g egg wet weight, provided the means to estimate risk as the depth where the LD50 level would be exceeded at realistic field PAH concentrations, based on estimates of UV-A exposure. The estimates were made using 30 years of solar radiation data for Duluth (MN, USA) and measurements of water-column UV-A transmittance in a PAH-contaminated field site. Medaka embryo failure was strongly related to tissue PAH concentration and UV-A exposure. The LD50 was estimated to be 12.64 J/cm2/ microg fluoranthene/g egg wet weight; the 95% confidence interval was 8.46 to 19.7 J/cm2/microg fluoranthene/g egg wet weight. Embryo failures were characterized by undifferentiated cell proliferation that occurred very early in development. No partial effects or embryo/larval malformations were observed. Estimates of the depth at which the LD50 would be exceeded in the contaminated field site ranged from 10.7 cm (clear-sky conditions and lowest attenuation) to 0.0 cm (cloudy conditions and highest attenuation). Similar calculations were done using water-column attenuation estimates from 12 sites across the Great Lakes (USA). For these, the depths at which the LD50 would be exceeded ranged from 0.00 to 271.6 cm under the conditions described above. These results suggest that PAH phototoxicity may be a risk factor in specific contaminated sites, and they provide a framework for assessing that risk.

Methods for assessing the long-term toxicity of sediments to Hyalella azteca and Chironomus tentans can significantly enhance the capacity to assess sublethal effects of contaminated sediments through multiple endpoints. Sublethal tests allow us to begin to understand the relationship between short-term and long-term effects for toxic sediments. We present an interlaboratory evaluation with long-term and 10-d tests using control and contaminated sediments in which we assess whether proposed and existing performance criteria (test acceptability criteria [TAC]) could be achieved. Laboratories became familiar with newly developed, long-term protocols by testing two control sediments in phase 1. In phase 2, the 10-d and long-term tests were examined with several sediments. Laboratories met the TACs, but results varied depending on the test organism, test duration, and endpoints. For the long-term tests in phase 1, 66 to 100% of the laboratories consistently met the TACs for survival, growth, or reproduction using H. azrteca, and 70 to 100% of the laboratories met the TACs for survival and growth, emergence, reproduction, and hatchability using C. tentans. In phase 2, fewer laboratories participated in long-term tests: 71 to 88% of the laboratories met the TAC for H. azteca, whereas 50 to 67% met the TAC for C. tentans. In the 10-d tests with H. azteca and C. tentans, 82 and 88% of the laboratories met the TAC for survival, respectively, and 80% met the TAC for C. tentans growth. For the 10-d and long-term tests, laboratories predicted similar toxicity. Overall, the interlaboratory evaluation showed good precision of the methods, appropriate endpoints were incorporated into the test protocols, and tests effectively predicted the toxicity of sediments.

The oligochaete, Lumbriculus variegatus, has several characteristics that make it desirable as a prey organism for conducting dietary exposure studies with fish. We conducted 21- and 30-d experiments with young fathead minnows (Pimephales promelas) and rainbow trout (Oncorhynchus mykiss), respectively, to determine whether a diet consisting solely of L. variegatus would support normal growth and to compare performance with standard diets (Artemia nauplii, frozen brine shrimp, or trout chow). All diets were readily accepted, and fish survived and grew well. Food conversion in both fathead minnows and rainbow trout was as high as or higher for the oligochaete diet compared with others, although this comparison is influenced by differences in ration, ingestion rate, or both. The oligochaete diet had gross nutritional analysis similar to the other diets, and meets fish nutrition guidelines for protein and essential amino acids. Methodologies and practical considerations for successfully using oligochaetes as an experimental diet are discussed. Considering their ready acceptance by fish, their apparent nutritional sufficiency, the ease of culturing large numbers, and the ease with which they can be loaded with exogenous chemicals, we believe that L. variegatus represents an excellent choice of exposure vector for exposing fish to toxicants via the diet.

Toxicity tests using standard effluent test procedures described by the U.S. Environmental Protection Agency were conducted with Ceriodaphnia dubia, fathead minnows (Pimephales promelas), and seven threatened and endangered (listed) fish species from four families: (1) Acipenseridae: shortnose sturgeon (Acipenser brevirostrum); (2) Catostomidae; razorback sucker (Xyrauchen texanus); (3) Cyprinidae: bonytail chub (Gila elegans), Cape Fear shiner (Notropis mekistocholas) Colorado pikeminnow (Ptychocheilus lucius), and spotfin chub (Cyprinella monacha); and (4) Poecillidae: Gila topminnow (Poeciliopsis occidentalis). We conducted 7-day survival and growth studies with embryo-larval fathead minnows and analogous exposures using the listed species. Survival and reproduction were also determined with C. dubia. Tests were conducted with carbaryl, ammonia--or a simulated effluent complex mixture of carbaryl, copper, 4-nonylphenol, pentachlorophenol and permethrin at equitoxic proportions. In addition, Cape Fear shiners and spotfin chub were tested using diazinon, copper, and chlorine. Toxicity tests were also conducted with field-collected effluents from domestic or industrial facilities. Bonytail chub and razorback suckers were tested with effluents collected in Arizona whereas effluent samples collected from North Carolina were tested with Cape Fear shiner, spotfin chub, and shortnose sturgeon. The fathead minnow 7-day effluent test was often a reliable estimator of toxic effects to the listed fishes. However, in 21 % of the tests, a listed species was more sensitive than fathead minnows. More sensitive species results varied by test so that usually no species was always more or less sensitive than fathead minnows. Only the Gila topminnow was consistently less sensitive than the fathead minnow. Listed fish species were protected 96% of the time when results for both fathead minnows and C. dubia were considered, thus reinforcing the value of standard whole-effluent toxicity tests using those two species. If the responses of specific listed species are important for management decisions, our study supports the value in developing culture and testing procedures for those species.

Assessment of contaminant impacts to federally identified endangered, threatened and candidate, and state-identified endangered species (collectively referred to as "listed" species) requires understanding of a species' sensitivities to particular chemicals. The most direct approach would be to determine the sensitivity of a listed species to a particular contaminant or perturbation. An indirect approach for aquatic species would be application of toxicity data obtained from standard test procedures and species commonly used in laboratory toxicity tests. Common test species (fathead minnow, Pimephales promelas; sheepshead minnow, Cyprinodon variegatus; and rainbow trout, Oncorhynchus mykiss) and 17 listed or closely related species were tested in acute 96-hour water exposures with five chemicals (carbaryl, copper, 4-nonylphenol, pentachlorophenol, and permethrin) representing a broad range of toxic modes of action. No single species was the most sensitive to all chemicals. For the three standard test species evaluated, the rainbow trout was more sensitive than either the fathead minnow or sheepshead minnow and was equal to or more sensitive than listed and related species 81% of the time. To estimate an LC50 for a listed species, a factor of 0.63 can be applied to the geometric mean LC50 of rainbow trout toxicity data, and more conservative factors can be determined using variance estimates (0.46 based on 1 SD of the mean and 0.33 based on 2 SD of the mean). Additionally, a low- or no-acute effect concentration can be estimated by multiplying the respective LC50 by a factor of approximately 0.56, which supports the United States Environmental Protection Agency approach of multiplying the final acute value by 0.5 (division by 2). When captive or locally abundant populations of listed fish are available, consideration should be given to direct testing. When direct toxicity testing cannot be performed, approaches for developing protective measures using common test species toxicity data are available.

Biologically directed fractionation techniques are a fundamental tool for identifying the cause of toxicity in environmental samples, but few are available for studying mixtures of organic chemicals in aquatic sediments. This paper describes a method for extracting organic chemicals from sediments and then re-introducing them into water column toxicity tests in a way that mimics, at least in part, the partitioning processes that govern bioavailability in sediment. This involves transferring solvent extracts of sediment into triolein and then placing the mixture inside low-density polyethylene dialysis tubing in a configuration similar to semipermeable membrane devices (SPMDs) used for environmental monitoring. For four model compounds, SPMDs were shown to effectively maintain water column exposure in static systems for 10-14 d, with partition coefficients similar to K(OW). Toxicity tests indicated that the SPMDs were compatible with four of five freshwater organisms tested and could be used to measure both lethal and sublethal end points. An example application showed good correspondence between organism responses in intactsediment and extracts in SPMDsfor both field-collected and spiked sediments. The SPMD-based method offers a simple, flexible test design, amenable to several different test organisms, and the ability to work with complex mixtures of contaminants while maintaining partitioning behavior similar to that within intact sediments.

A visualization approach is developed and presented for depicting and interpreting bioaccumulation relationships and data (i.e., bioaccumulation factors [BAFs], biota-sediment accumulation factors [BSAFs], and chemical residues in fish) using water-sediment chemical concentration XY plots. The approach is based on five basic parameters that affect bioaccumulation of nonionic organic chemicals: The distribution of chemical between sediment and water, the hydrophobicity of the compound (expressed as the n-octanol/water partition coefficient, K(OW)), the relationship of food chains to water and sediment, the length of the food chains, and the degree to which the chemical is metabolized. The visualization approach using water-sediment XY plots captures and visually presents the existing bioaccumulation knowledge in a form that is readily understandable from chemical, biological, and ecological aspects and, therefore, useful in the assessment, communication, and management of risk for persistent bioaccumulative toxicants.

The risk of photoactivated PAH toxicity in contaminated aquatic systems has not been well characterized. To document risk, amphipods (Gammarus spp.) were collected from two polycyclic aromatic hydrocarbon (PAH)-contaminated sites in the lower St. Louis River and Duluth Harbor, USA (Hog Island and USX) as well as a reference site (Chipmunk Cove) and were exposed in two separate, replicate tests to controlled intensities of solar radiation for 3 d. Contaminated site organisms died significantly faster compared to control site organisms. In all tests, mortality was strongly related to ultraviolet-A (UV-A; 320-400 nm) dose. Ultraviolet-B (280-320 nm) radiation did not increase mortality. To compare susceptibility among populations, regressions of arcsine-transformed, proportionate mortality versus UV dose were completed for each, and the slopes were statistically compared. Response slopes for the two contaminated site populations were both significantly greater than the reference site population (p = 0.0001 for test 1; p = 0.0002 for test 2). These results indicate that organisms residing in PAH-contaminated environments can accumulate PAH concentrations sufficient to be at risk for photoactivated toxicity. Although amphipods are not typically at risk of PAH-photoactivated toxicity because they are largely protected from exposure to sunlight, they are representative surrogates for species that may be similarly protected at some life stages (and thus able to accumulate significant PAH tissue concentrations) but not at others.

Uptake of sediment-associated contaminants by the oligochaete Lumbriculus variegatus was evaluated after 1, 3, 7, 14, 28, and 56 d of exposure to a field-collected sediment contaminated with DDT and its metabolites, dichlorodiphenyldichloroethane (DDD) and dichlorodiphenyldichloroethylene (DDE), or to a field-collected sediment contaminated with polycyclic aromatic hydrocarbons (PAHs). Depuration of contaminants by oligochaetes in a control sediment or in water was also evaluated over a 7-d period after 28 d of exposure to the field-collected sediments. Accumulation of PAHs with a log octanol-water partitioning coefficient (log Kow) <5.6 typically reached a peak at day 3, followed by a lower plateau between days 7 and 56 of the sediment exposure. Similarly, 4,4'-DDT exhibited a peak in accumulation at day 14 followed by a decline at days 28 and 56. In contrast, accumulation of PAHs with a log Kow >5.6 or DDD and DDE typically exhibited a steady increase from day 1 to about day 14 or 28, followed by a plateau. Therefore, exposures conducted for a minimum of 14 to 28 d better reflected steady-state concentrations for DDT and its metabolites and for PAHs. Depuration rates for DDT and its metabolites and high-Kow PAHs were much higher in organisms held in clean sediment relative to both water-only depuration and model predictions. This suggests that depuration in clean sediment may artificially accelerate depuration of hydrophobic compounds. Comparisons between laboratory-exposed L. variegatus and oligochaetes collected in the field from these sediments indicate that results of laboratory tests can be extrapolated to the field with a reasonable degree of certainty.

After exposure for 21 d to sediment spiked with Cd, Pb, Cu, or Zn, oligochaetes (Lumbriculus variegatus) held in clean water depurated metal rapidly over the first few hours but much more slowly from 8 h up to 32 h. Results are consistent with previous work suggesting a 6-h depuration period as generally appropriate for sediment bioaccumulation studies with L. variegatus.

Tests were performed with the freshwater invertebrates Hyalella azteca, Chironomus tentans, and Lumbriculus variegatus to determine the acute toxicity of six phthalate esters, including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butylbenzyl phthalate (BBP), di-n-hexyl phthalate (DHP), and di-2-ethylhexyl phthalate (DEHP). It was possible to derive 10-d LC50 (lethal concentration for 50% of the population) values only for the four lower molecular weight esters (DMP, DEP, DBP, and BBP), for which toxicity increased with increasing octanol-water partition coefficient (Kow) and decreasing water solubility. The LC50 values for DMP, DEP, DBP, and BBP were 28.1, 4.21, 0.63, and 0.46 mg/L for H. azteca; 68.2, 31.0, 2.64, and > 1.76 mg/L for C. tentans; and 246, 102, 2.48, and 1.23 mg/L for L. variegatus, respectively. No significant survival reductions were observed when the three species were exposed to either DHP or DEHP at concentrations approximating their water solubilities.

Seven phthalate esters were evaluated for their 10-d toxicity to the freshwater invertebrates Hyalella azteca and Chironomus tentans in sediment. The esters were diethyl phthalate (DEP), di-n-butyl phthalate (DBP), di-n-hexyl phthalate (DHP), di-(2-ethylhexyl) phthalate (DEHP), diisononyl phthalate (DINP), diisodecyl phthalate (DIDP), and a commercial mixture of C7, C9, and C11 isophthalate esters (711P). All seven esters were tested in a sediment containing 4.80% total organic carbon (TOC), and DBP alone was tested in two additional sediments with 2.45 and 14.1% TOC. Sediment spiking concentrations for DEP and DBP were based on LC50 (lethal concentration for 50% of the population) values from water-only toxicity tests, sediment organic carbon concentration, and equilibrium partitioning (EqP) theory. The five higher molecular weight phthalate esters (DHP, DEHP, DINP, DIDP, 711P), two of which were tested and found to be nontoxic in water-only tests (i.e., DHP and DEHP), were tested at single concentrations between 2,100 and 3,200 mg/kg dry weight. Preliminary spiking studies were performed to assess phthalate ester stability under test conditions. The five higher molecular weight phthalate esters in sediment had no effect on survival or growth of either C. tentans or H. azteca, consistent with predictions based on water-only tests and EqP theory. The 10-d LC50 values for DBP and H. azteca were >17,400, >29,500, and >71,900 mg/kg dry weight for the low, medium, and high TOC sediments, respectively. These values are more than 30x greater than predicted by EqP theory and may reflect the fact that H. azteca is an epibenthic species and not an obligative burrower. The 10-d LC50 values for DBP and C. tentans were 826, 1,664, and 4.730 mg/kg dry weight for the low, medium, and high TOC sediments, respectively. These values are within a factor of two of the values predicted by EqP theory. Pore-water 10-d LC50 values for DBP (dissolved fraction) and C. tentans in the three sediments were 0.65, 0.89, and 0.66 of the water-only LC50 value of 2.64 mg/L, thereby agreeing with EqP theory predictions to within a factor of 1.5. The LC50 value for DEP and C. tentans was >3,100 mg/kg dry weight, which is approximately 10x that predicted by EqP theory. It is postulated that test chemical loss and reduced organism exposure to pore water may have accounted for the observed discrepancies with EqP calculations for DEP

We evaluated the effectiveness of Ambersorb, a carbonaceous resin, in reducing bioavailability of polycyclic aromatic hydrocarbons (PAHs) in contaminated sediments collected from the field. In laboratory studies, sediment pore-water concentrations of eight unsubstituted PAHs were significantly decreased after resin addition. Reduced PAH concentrations in oligochaete tissues from a laboratory bioaccumulation test, along with increased survival/reproduction and reduced photo-enhanced toxicity and sediment avoidance, also resulted from sediment treatment with Ambersorb. Resin amendment also decreased pore-water PAH concentrations in field deployed sediments but did not improve benthic invertebrate colonization. Prediction of partitioning of PAHs between solid and aqueous phases in the test sediments was complicated by the presence of coal and soot. However, accurate predictions of bioavailability were achieved based on pore-water chemistry. Overall, these studies show that the addition of high affinity sorbents effectively reduces pore-water PAH concentrations and bioavailability and suggests that sorbent addition may serve as an option for in situ remediation of some contaminated sediments.