Sediment TIE Validation Study Using South Korean Domestic Species Glyptotendipes tokunagai to Evaluate Contamination with Two Heavy Metals and Ammonia

Toxicity tests are an important aspect of sediment quality assessments, but knowledge of the cause of toxicity is needed to determine effective management actions. Toxicity identification evaluation (TIE) methods were developed to meet this need. While TIE method manuals provide information on the procedures, little information on study design is presented. The level of variability associated with performing TIEs and how to account for it is also not addressed. The goal of this study was to collect data on both the spatial and temporal variability associated with sediment TIEs by use of the amphipod Eohaustorius estuarius 10-day survival test and then apply that information to make recommendations for designing future TIE studies. Ten stations were sampled at Consolidated Slip in Los Angeles Harbor, California, with samples collected 2 months apart. In the first stage, TIEs were conducted on whole sediment and pore water from 3 of the most toxic stations. In the second stage, focused TIEs were conducted on whole sediment from all stations. Chemical analysis for metals and organic contaminants was also performed. With a weight of evidence approach, it was determined that pyrethroid pesticides were the likely cause of toxicity, with a lesser contribution from polycyclic aromatic hydrocarbons (PAHs). Results of the individual TIEs fell into 3 broad categories: TIEs in which treatments for organic chemicals and pyrethroids were effective; TIEs in which the treatment for pyrethroids was not effective but the treatment for organic contaminants was effective; and TIEs in which the treatment for pyrethroids was effective but the treatment for organic contaminants was not. This variability was used to calculate that at least 3 TIEs were necessary to make a confident assessment of the cause of toxicity. There was not substantial temporal variability in the TIE outcomes. Other recommendations are made regarding effective TIE study design. Integr Environ Assess Manag 2019;15:248-258. © 2018 SETAC.

A common method for determining whether contaminants in sediments represent an environmental risk is to perform toxicity tests. Toxicity tests indicate whether contaminants in sediments are bioavailable and capable of causing adverse biological effects (e.g., mortality, reduced growth or reproduction) to aquatic organisms. Several environmental management and regulatory programs concerned with contaminated sediments use this approach for assessing risk. However, a limitation of the toxicity testing approach is that the results indicate only if toxicity is present in a given sediment sample. Toxicity test results do not provide information on the cause of toxicity; that is, what specific toxic chemicals are responsible for the effects observed. Information on the cause of the effect is important in performing risk assessments and determining remedial actions at contaminated sediment sites. Methods called Toxicity Identification Evaluation (TIE) procedures were originally developed for industrial and municipal effluents to determine the causes of toxicity in waters affected by these discharges. The TIE approach combines toxicity testing with simple chemical manipulations to selectively alter the toxicity of specific classes of toxicants in a sample. These aqueous TIE methods were later adapted for use with contaminated sediment interstitial waters. Now, whole sediment TIE methods have been developed for both freshwater and marine sediments. This chapter will focus on the development of TIE methods for marine contaminated sediments. Like the aqueous-based TIE methods, the whole sediment TIE methods combine toxicity testing with chemical manipulations to selectively alter the toxicity of potential classes of sediment contaminants. By selectively altering the toxicity of potential classes of toxicants followed by comparison to the toxicity of an unmanipulated sample, it is possible to characterize and identify the causes of sediment toxicity. Currently, interstitial water and whole sediment TIE methods are designed to detect toxicity caused by cationic and anionic metals, nonionic organic compounds, and ammonia, although methods for other toxicants including hydrogen sulfide and specific pesticides are under development. This chapter will provide an overview of the TIE approach and methods for both marine interstitial waters and whole sediments. The chapter will conclude with a brief discussion of new applications for sediment TIEs as well as research needs for the continued development of sediment TIE methods.

Whole-sediment toxicity identification evaluation (TIE) techniques were employed on the Illinois River Complex (IRC), USA to identify the sources of sediment toxicity that may have contributed to the decline in benthic invertebrate populations. The TIE focused on three classes of contaminants: ammonia, metals, and organics. Sediment toxicity was assessed using the amphipod Hyalella azteca, and the focus of the TIE was on assessing spatial and temporal patterns of contamination. Past studies suggested that ammonia was the major source of contamination in IRC sediments. However, the present study suggested that polycyclic aromatic hydrocarbons (PAHs) were the primary contributor to sediment toxicity. Phase I testing showed 46% of the site trials (12 of 26) exhibited increased H. azteca survival (p < 0.05) with the addition of powdered coconut charcoal (organic amendment), whereas zeolite (ammonia amendment) and Resin Tech SIR 300 (cationic metals amendment) did not increase H. azteca survival. Phase II testing revealed PAH concentrations were high enough to cause the observed toxicity, confirming phase I results. Spatially, sediment toxicity as well as pore-water ammonia concentrations declined with distance downstream from suspected contaminant sources, indicating a potential dilution or remedial effect. Temporally, pore-water ammonia, metals, and PAH concentrations varied among sampling periods over an annual cycle for some sites near urbanized areas, while remaining temporally consistent at others. The results of the present study provide new information on the sources of toxicity within the IRC, and demonstrate the importance of evaluating spatial and temporal aspects in sediment TIEs. This is particularly important for evaluations in riverine systems in which hydrologic processes can result in large variation in sediment toxicity on temporal and spatial scales.

Removal of organic contaminant toxicity from sediments-early work toward development of a toxicity identification evaluation (TIE) method

Comparative analysis of whole sediment and porewater toxicity identification evaluation techniques for ammonia and non-polar organic contaminants

Toxicity caused by heavy metals in environmental samples can be assessed by performing a suite of toxicity identification evaluation (TIE) methods. The behavior of metals during TIEs can vary greatly according to sample matrix. Some approaches and precautions in using TIE to identify metal toxicants in a sample are discussed, using case studies from three effluent and one sediment TIEs. These approaches include responses of metals that erroneously suggest the presence of other toxicants, the bioavailability of metals retained by glass-fiber filtration, and cautionary steps in Phase III to avoid dilution water effects on sample toxicity.

Laboratory bioassays can provide an integrated assessment of the potential toxicity of contaminated sediments to aquatic organisms; however, toxicity as a sole endpoint is not particularly useful in terms of identifying remedial options. To focus possible remediation (e.g., source control), it is essential to know which contaminants are responsible for toxicity. Unfortunately, contaminated sediments can contain literally thousands of potentially toxic compounds. Methods which rely solely on correlation to identify contaminants responsible for toxicity are limited in several aspects: (a) actual compounds causing toxicity might not be measured, (b) concentrations of potentially toxic compounds may covary, (c) it may be difficult to assess the bioavailability of contaminants measured in a sediment, and (d) interactions may not be accounted for among potential toxicants (e.g., additivity). Toxicity identification evaluation (TIE) procedures attempt to circumvent these problems by using toxicity-based fractionation procedures to implicate specific contaminants as causative toxicants. Phase I of TIE characterizes the general physio-chemical nature of sample toxicants. Phase II employs methods to measure toxicants via different analytical methods, and Phase III consists of techniques to confirm that the suspect toxicants identified in Phases I and II of the TIE actually are responsible for toxicity. These TIE procedures have been used to investigate the toxicity of a variety of samples, including sediments. Herein we present a brief conceptual overview of the TIE process, and discuss specific considerations associated with sediment TIE research. Points addressed include: (a) selection and preparation of appropriate test fractions, (b) use of benthic organisms for sediment TIE work, and (c) methods for the identification of common sediment contaminants.

The Ballona Creek Estuary (BCE) in Los Angeles, California, is in a highly urbanized watershed, is contaminated by a variety of chemicals, and has prevalent sediment toxicity. Sediment cleanup targets for BCE have been established for Cu, Cd, Pb, Zn, chlordane, DDTs, PCBs, and PAHs, based on sediment quality guidelines. A sediment toxicity identification evaluation (TIE) was conducted to examine how these targets corresponded to toxicity observed with the estuarine amphipod Eohaustorius estuarius. Whole sediment and porewater TIEs were used to identify the cause of toxicity. Passive samplers were deployed to determine the bioavailable fraction of contaminants. Spiked sediment tests were conducted to determine the thresholds of toxicity for selected constituents. Toxicity was found to be widespread but temporally and spatially variable. Whole sediment and porewater TIEs both indicated pyrethroid pesticides were the most likely contaminant group contributing to the toxicity. Concentrations of the chemicals listed for cleanup were found to often exceed target values but were not observed at concentrations likely to cause toxicity. Bioavailable fractions of the target chemicals quantified using passive samplers did not exceed toxicity thresholds. Spiked sediment tests established 10 day LC50s for 4,4' DDE, 4, 4' DDT, α-chlordane, and cyfluthrin at >3050 μg/g, 266 μg/g, >2120 μg/g, and 0.33 μg/g organic carbon (OC), respectively. The cyfluthrin LC50 was within the range of concentrations observed in the estuary sediments, but LC50s for the other 3 chemicals were orders of magnitude greater than observed levels. The combination of TIE, sediment chemistry and the results from spiked sediment exposures indicate pyrethroid pesticides are more likely the cause of the observed toxicity than any of the contaminants targeted for cleanup. The results of this study indicate the importance of using a TIE approach to determine chemicals of concern and dose-response information to set cleanup targets, rather than using sediment quality guidelines. Integr Environ Assess Manag 2014;10:260-268. © 2013 SETAC.

Removal of ammonia toxicity in marine sediment TIEs: a comparison of Ulva lactuca, zeolite and aeration methods

Evaluation of phase II toxicity identification evaluation methods for freshwater whole sediment and interstitial water

A Toxicity Identification Evaluation of sediments from various reaches of the Calcasieu Estuary in Louisiana was performed to improve the technical basis for Total Maximum Daily Loads under development for this water body. The Toxicity Identification Evaluation methodology involved manipulations of the physical/chemical properties of sediment pore water samples in order to sequentially remove or bind each of the major classes of contaminant compounds and confounding factors. Toxicity tests were performed in conjunction with these manipulations to directly correlate reduction in toxicity with the specifically targeted contaminant classes. Toxicity of sediment porewaters from seven locations was evaluated using the amphipod, Ampelisca abdita and the mysid, Americamysis bahia. Toxicity Identification Evaluation results demonstrated improved survival after filtration, indicating that suspended particulates and associated contaminants were a significant source of toxicity. Subsequent treatments with column extraction and ethylene diamine tetra amino acid reduced toxicity, indicating both organics and metal constituents of pore waters as contributors to toxicity. The analysis of the filters used in the Toxicity Identification Evaluation revealed that particulate copper in the porewater was above criteria values, indicating that adverse exposure potential existed from the particulate phases, and that shifts in partitioning equilibrium could mediate dissolved-phase exposures. The identification of specific contaminant classes as well as particulate effects as sources of acute toxicity from Toxicity Identification Evaluation results indicate that in place sediment contamination as well as pore water flux and resuspension are likely contributors to habitat impairment that should be considered in Total Maximum Daily Load development.

In the present study, chinonomus riparius larvae were selected as a model organism, and 11 sediment samples from the Xihe River in Shenyang underwent toxicity identification evaluation (TIE) to identify sediment toxic pollutants. Heavy metals and organic pollutants were the main toxic pollutants through toxicity screening and characterization. The results of toxicity identification showed that the pollution level from Cd was most serious and that phenol and P-methyl phenol were the major organic pollutants. Moreover, a spiking test of Cd was conducted, which indicated that Cd was the main toxic pollutant of sediments at sites 4, 6, 7, 8, and 10. We confirm that TIE is the most effective method to determine the relationship between toxic effects and toxic pollutants. Environ Toxicol Chem 2021;40:3103-3110. © 2021 SETAC.

Application of toxicity identification evaluation procedure to toxic industrial effluent in South Korea

Temporal pattern of toxicity in runoff from the Tijuana River Watershed

Passaic river sediment interstitial water phase I toxicity identification evaluation