J. Russell Hockett

Use of toxicity identification evaluation methods to characterize, identify, and confirm hexavalent chromium toxicity in an industrial effluent

Abstract A toxicity identification evaluation (TIE) was conducted on effluent from a major industrial discharger. Although initial monitoring typically showed only slight, intermittent, chronic toxicity to Ceriodaphnia dubia, a later sample showed substantial acute toxicity to C. dubia (48-h lc 50=9%). Acute phase I toxicity characterization tests were conducted on this acutely toxic sample; none of the phase I manipulations reduced sample toxicity. The toxic effluent sample was then treated with activated carbon, and cation, anion, and mixed-bed ion exchange. Acute toxicity was not reduced by treatment with activated carbon or cation exchange, but was completely removed by anion and mixed-bed ion exchange. Based on these data, we concluded that the causative toxicant(s) was likely an inorganic anion(s); chemical analysis detected hexavalent chromium (Cr[VI]) at concentrations sufficient to account for the observed acute toxicity. Although Cr[VI] could clearly explain the presence of acute toxicity, subsequent confirmation testing was designed to determine whether Cr[IV] was responsible for the low-level chronic toxicity more typical of the effluent. Concurrent chronic tests conducted on unaltered and anion-exchanged effluent showed that the presence of chronic toxicity was associated with chronically toxic concentrations of Cr[VI]. The source of Cr[VI] in the effluent was traced to a malfunctioning heat exchanger; after this malfunction was corrected, neither chronic toxicity nor appreciable Cr[VI] was observed in the effluent again.

The relative importance of waterborne and dietborne arsenic exposure on survival and growth of juvenile rainbow trout

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.

Using an interlaboratory study to revise methods for conducting 10-d to 42-d water or sediment toxicity tests with Hyalella azteca.

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.

The acute toxicity of major ion salts to Ceriodaphnia dubia. II. Empirical relationships in binary salt mixtures

Many human activities increase concentrations of major geochemical ions (Na+1 , K+1 , Ca+2 , Mg+2 , Cl-1 , SO4-2 , and HCO3-1 /CO3-2 ) 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.

Contrasting effects of chloride on growth, reproduction, and toxicant sensitivity in two genetically distinct strains of Hyalella azteca

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.

Relative sensitivity of an amphipod Hyalella azteca, a midge Chironomus dilutus, and a unionid mussel Lampsilis siliquoidea to a toxic sediment.

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.

Evaluation of PCB bioaccumulation by Lumbriculus variegatus in field‐collected sediments

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.

The acute toxicity of major ion salts to Ceriodaphnia dubia. III. Mathematical models for mixture toxicity

Based on previous research on the acute toxicity of major ions (Na+ , K+ , Ca2+ , Mg2+ , Cl- , SO42- , and HCO3- /CO32- ) 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.

Influence of dilution water ionic composition on acute major ion toxicity to the mayfly Neocloeon triangulifer

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 Na2 SO4 , with the median lethal concentration (LC50) of 1338 mg SO4 /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 CaCO3 ) resulted in doubling of LC50s for sodium salts, and an approximately 1.5-fold increase in LC50 for MgSO4 . 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 Na2 SO4 and NaCl did not appear as strong as when hardness was varied; but for MgSO4 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, SO4 , 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.