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USGS2002

Pharmaceuticals, hormones, and other organic wastewater contaminants in U.S. streams, 1999-2000: A national reconnaissance

To provide the first nationwide reconnaissance of the occurrence of pharmaceuticals, hormones, and other organic wastewater contaminants (OWCs) in water resources, the U.S. Geological Survey used five newly developed analytical methods to measure concentrations of 95 OWCs in water samples from a network of 139 streams across 30 states during 1999 and 2000. The selection of sampling sites was biased toward streams susceptible to contamination (i.e. downstream of intense urbanization and livestock production). OWCs were prevalent during this study, being found in 80% of the streams sampled. The compounds detected represent a wide range of residential, industrial, and agricultural origins and uses with 82 of the 95 OWCs being found during this study. The most frequently detected compounds were coprostanol (fecal steroid), cholesterol (plant and animal steroid), N , N -diethyltoluamide (insect repellant), caffeine (stimulant), triclosan (antimicrobial disinfectant), tri(2-chloroethyl)phosphate (fire retardant), and 4-nonylphenol (nonionic detergent metabolite). Measured concentrations for this study were generally low and rarely exceeded drinking-water guidelines, drinking-water health advisories, or aquatic-life criteria. Many compounds, however, do not have such guidelines established. The detection of multiple OWCs was common for this study, with a median of seven and as many as 38 OWCs being found in a given water sample. Little is known about the potential interactive effects (such as synergistic or antagonistic toxicity) that may occur from complex mixtures of OWCs in the environment. In addition, results of this study demonstrate the importance of obtaining data on metabolites to fully understand not only the fate and transport of OWCs in the hydrologic system but also their ultimate overall effect on human health and the environment.

Environmental Science & Technology↗
USGS2002

Photochemical changes in cyanide speciation in drainage from a precious metal ore heap

In drainage from an inactive ore heap at a former gold mine, the speciation of cyanide and the concentrations of several metals were found to follow diurnal cycles. Concentrations of the hexacyanoferrate complex, iron, manganese, and ammonium were higher at night than during the day, whereas weak-acid-dissociable cyanide, silver, gold, copper, nitrite, and pH displayed the reverse behavior. The changes in cyanide speciation, iron, and trace metals can be explained by photodissociation of iron and cobalt cyanocomplexes as the solutions emerged from the heap into sunlight-exposed channels. At midday, environmentally significant concentrations of free cyanide were produced in a matter of minutes, causing trace copper, silver, and gold to be mobilized as cyanocomplexes from solids. Whether rapid photodissociation is a general phenomenon common to other sites will be important to determine in reaching a general understanding of the environmental risks posed by routine or accidental water discharges from precious metal mining facilities.

Environmental Science & Technology↗
USGS2002

Effects of dietary methylmercury on reproduction of fathead minnows

We examined effects of dietary methylmercury (MeHg) on reproduction of fathead minnows (Pimephales promelas). Juvenile fish were fed one of four diets until sexual maturity (phase 1): a control diet (0.06 μg Hg g -1 dry weight) and three diets contaminated with MeHg at 0.88 (low), 4.11 (medium), and 8.46 μg Hg g -1 dry weight (high). At sexual maturity, male and female fish were paired, again fed one of the four diets, and allowed to reproduce (phase 2). To assess effects of MeHg during gametogenesis, some fish were fed diets during phase 2 that differed from those during phase 1. Spawning success of pairs fed the same diet during phases 1 and 2 was 75% for controls and 46%, 50%, and 36% for the low-, medium-, and high-MeHg treatments, respectively. Spawning success of pairs fed a contaminated diet during phase 1 and a control diet during phase 2 was 63%, 40%, and 14% for the low-, medium-, and high-MeHg treatments, respectively, whereas exposure to dietary MeHg only during phase 2 did not reduce spawning success. Dietary MeHg delayed spawning, and days to spawning was positively correlated with concentration of total mercury in the carcasses of test fish. MeHg reduced the instantaneous rate of reproduction of fish fed the same diets during phases 1 and 2. Both the gonadosomatic index and reproductive effort of female fish were inversely correlated with mercury in carcasses, whereas developmental and hatching success of embryos, 7-d survival, and 7-d growth of larvae were unrelated to mercury concentrations in parental fish or their diets. MeHg decreased reproduction of adult fathead minnows at dietary concentrations encountered by predatory fishes in aquatic systems with MeHg-contaminated food webs, implying that exposed fish populations could be adversely affected by this widespread contaminant.

Environmental Science & Technology↗
USGS2002

Corn leaf nitrate reductase - A nontoxic alternative to cadmium for photometric nitrate determinations in water samples by air-segmented continuous-flow analysis

Development, characterization, and operational details of an enzymatic, air-segmented continuous-flow analytical method for colorimetric determination of nitrate + nitrite in natural-water samples is described. This method is similar to U.S. Environmental Protection Agency method 353.2 and U.S. Geological Survey method 1-2545-90 except that nitrate is reduced to nitrite by soluble nitrate reductase (NaR, EC 1.6.6.1) purified from corn leaves rather than a packed-bed cadmium reactor. A three-channel, air-segmented continuous-flow analyzer-configured for simultaneous determination of nitrite (0.020-1.000 mg-N/L) and nitrate + nitrite (0.05-5.00 mg-N/L) by the nitrate reductase and cadmium reduction methods-was used to characterize analytical performance of the enzymatic reduction method. At a sampling rate of 90 h-1, sample interaction was less than 1% for all three methods. Method detection limits were 0.001 mg of NO2- -N/L for nitrite, 0.003 mg of NO3-+ NO2- -N/L for nitrate + nitrite by the cadmium-reduction method, and 0.006 mg of NO3- + NO2- -N/L for nitrate + nitrite by the enzymatic-reduction method. Reduction of nitrate to nitrite by both methods was greater than 95% complete over the entire calibration range. The difference between the means of nitrate + nitrite concentrations in 124 natural-water samples determined simultaneously by the two methods was not significantly different from zero at the p = 0.05 level.

Environmental Science & Technology↗
USGS2002

In-situ evidence for uranium immobilization and remobilization

The in-situ microbial reduction and immobilization of uranium was assessed as a means of preventing the migration of this element in the terrestrial subsurface. Uranium immobilization (putatively identified as reduction) and microbial respiratory activities were evaluated in the presence of exogenous electron donors and acceptors with field push−pull tests using wells installed in an anoxic aquifer contaminated with landfill leachate. Uranium(VI) amended at 1.5 μM was reduced to less than 1 nM in groundwater in less than 8 d during all field experiments. Amendments of 0.5 mM sulfate or 5 mM nitrate slowed U(VI) immobilization and allowed for the recovery of 10% and 54% of the injected element, respectively, as compared to 4% in the unamended treatment. Laboratory incubations confirmed the field tests and showed that the majority of the U(VI) immobilized was due to microbial reduction. In these tests, nitrate treatment (7.5 mM) inhibited U(VI) reduction, and nitrite was transiently produced. Further push−pull tests were performed in which either 1 or 5 mM nitrate was added with 1.0 μM U(VI) to sediments that already contained immobilized uranium. After an initial loss of the amendments, the concentration of soluble U(VI) increased and eventually exceeded the injected concentration, indicating that previously immobilized uranium was remobilized as nitrate was reduced. Laboratory experiments using heat-inactivated sediment slurries suggested that the intermediates of dissimilatory nitrate reduction (denitrification or dissimilatory nitrate reduction to ammonia), nitrite, nitrous oxide, and nitric oxide were all capable of oxidizing and mobilizing U(IV). These findings indicate that in-situ subsurface U(VI) immobilization can be expected to take place under anaerobic conditions, but the permanence of the approach can be impaired by disimilatory nitrate reduction intermediates that can mobilize previously reduced uranium.

Environmental Science & Technology↗
USGS2003

Sources of sulfate supporting anaerobic metabolism in a contaminated aquifer

Field and laboratory techniques were used to identify the biogeochemical factors affecting sulfate reduction in a shallow, unconsolidated alluvial aquifer contaminated with landfill leachate. Depth profiles of 35 S-sulfate reduction rates in aquifer sediments were positively correlated with the concentration of dissolved sulfate. Manipulation of the sulfate concentration in samples revealed a Michaelis−Menten-like relationship with an apparent K m and V max of approximately 80 and 0.83 μM SO 4 - 2 ·day - 1 , respectively. The concentration of sulfate in the core of the leachate plume was well below 20 μM and coincided with very low reduction rates. Thus, the concentration and availability of this anion could limit in situ sulfate-reducing activity. Three sulfate sources were identified, including iron sulfide oxidation, barite dissolution, and advective flux of sulfate. The relative importance of these sources varied with depth in the alluvium. The relatively high concentration of dissolved sulfate at the water table is attributed to the microbial oxidation of iron sulfides in response to fluctuations of the water table. At intermediate depths, barite dissolves in undersaturated pore water containing relatively high concentrations of dissolved barium (∼100 μM) and low concentrations of sulfate. Dissolution is consistent with the surface texture of detrital barite grains in contact with leachate. Laboratory incubations of unamended and barite-amended aquifer slurries supported the field observation of increasing concentrations of barium in solution when sulfate reached low levels. At a deeper highly permeable interval just above the confining bottom layer of the aquifer, sulfate reduction rates were markedly higher than rates at intermediate depths. Sulfate is supplied to this deeper zone by advection of uncontaminated groundwater beneath the landfill. The measured rates of sulfate reduction in the aquifer also correlated with the abundance of accumulated iron sulfide in this zone. This suggests that the current and past distributions of sulfate-reducing activity are similar and that the supply of sulfate has been sustained at these sites.

Environmental Science & Technology↗
USGS2002

15N NMR investigation of the reduction and binding of TNT in an aerobic bench scale reactor simulating windrow composting

T15NT was added to a soil of low organic carbon content and composted for 20 days in an aerobic bench scale reactor. The finished whole compost and fulvic acid, humic acid, humin, and lignocellulose fractions extracted from the compost were analyzed by solid-state CP/MAS and DP/MAS 15N NMR. 15N NMR spectra provided direct spectroscopic evidence for reduction of TNT followed by covalent binding of the reduced metabolites to organic matter of the composted soil, with the majority of metabolite found in the lignocellulose fraction, by mass also the major fraction of the compost. In general, the types of bonds formed between soil organic matter and reduced TNT amines in controlled laboratory reactions were observed in the spectra of the whole compost and fractions, confirming that during composting TNT is reduced to amines that form covalent bonds with organic matter through aminohydroquinone, aminoquinone, heterocyclic, and imine linkages, among others. Concentrations of imine nitrogens in the compost spectra suggestthat covalent binding bythe diamines 2,4DANT and 2,6DANT is a significant process in the transformation of TNT into bound residues. Liquid-phase 15N NMR spectra of the fulvic acid and humin fractions provided possible evidence for involvement of phenoloxidase enzymes in covalent bond formation.

Environmental Science & Technology↗
USGS2002

15N NMR investigation of the covalent binding of reduced TNT amines to soil humic acid, model compounds, and lignocellulose

The five major reductive degradation products of TNT-4ADNT (4-amino-2,6-dinitrotoluene), 2ADNT (2-amino-4,6-dinitrotoluene), 2,4DANT (2,4-diamino-6-nitrotoluene), 2,6DANT (2,6-diamino-4-nitrotoluene), and TAT (2,4,6-triaminotoluene)-labeled with 15N in the amine positions, were reacted with the IHSS soil humic acid and analyzed by 15N NMR spectrometry. In the absence of catalysts, all five amines underwent nucleophilic addition reactions with quinone and other carbonyl groups in the soil humic acid to form both heterocyclic and nonheterocyclic condensation products. Imine formation via 1,2-addition of the amines to quinone groups in the soil humic acid was significant with the diamines and TAT but not the monoamines. Horseradish peroxidase (HRP) catalyzed an increase in the incorporation of all five amines into the humic acid. In the case of the diamines and TAT, HRP also shifted the binding away from heterocyclic condensation product toward imine formation. A comparison of quantitative liquid phase with solid-state CP/MAS 15N NMR indicated that the CP experiment underestimated imine and heterocyclic nitrogens in humic acid, even with contact times optimal for observation of these nitrogens. Covalent binding of the mono- and diamines to 4-methylcatechol, the HRP catalyzed condensation of 4ADNT and 2,4DANT to coniferyl alcohol, and the binding of 2,4DANT to lignocellulose with and without birnessite were also examined.

Environmental Science & Technology↗
USGS2002

Mercury(II) sorption to two Florida Everglades peat: Evidence for strong and weak binding and competition by dissolved organic matter released from the peat

The binding of mercury(II) to two peats from Florida Everglades sites with different rates of mercury methylation was measured at pH 6.0 and 0.01 M ionic strength. The mercury(II) sorption isotherms, measured over a total mercury(II) range of 10 - 7.4 to 10 - 3.7 M, showed the competition for mercury(II) between the peat and dissolved organic matter released from the peat and the existence of strong and weak binding sites for mercury(II). Binding was portrayed by a model accounting for strong and weak sites on both the peat and the released DOM. The conditional binding constants (for which the ligand concentration was set as the concentration of reduced sulfur in the organic matter as measured by X-ray absorption near-edge structure spectroscopy) determined for the strong sites on the two peats were similar ( K peat,s = 10 21.8±0.1 and 10 22.0±0.1 M - 1 ), but less than those determined for the DOM strong sites ( K dom,s = 10 22.8 ± 0.1 and 10 23.2 ± 0.1 M - 1 ), resulting in mercury(II) binding by the DOM at low mercury(II) concentrations. The magnitude of the strong site binding constant is indicative of mercury(II) interaction with organic thiol functional groups. The conditional binding constants determined for the weak peat sites ( K peat,w = 10 11.5 ± 0.1 and 10 11.8 ± 0.1 M - 1 ) and weak DOM sites ( K dom,w = 10 8.7 ± 3.0 and 10 7.3 ± 4.5 M - 1 ) were indicative of mercury(II) interaction with carboxyl and phenol functional groups.

Environmental Science & Technology↗
USGS2002

TBA biodegradation in surface-water sediments under aerobic and anaerobic conditions

The potential for [U-14C] TBA biodegradation was examined in laboratory microcosms under a range of terminal electron accepting conditions. TBA mineralization to CO2 was substantial in surface-water sediments under oxic, denitrifying, or Mn(IV)-reducing conditions and statistically significant but low under SO4-reducing conditions. Thus, anaerobic TBA biodegradation may be a significant natural attenuation mechanism for TBA in the environment, and stimulation of in situ TBA bioremediation by addition of suitable terminal electron acceptors may be feasible. No degradation of [U-14C] TBA was observed under methanogenic or Fe(III)-reducing conditions.

Environmental Science & Technology↗
USGS2002

VOCs, pesticides, nitrate, and their mixtures in groundwater used for drinking water in the United States

Samples of untreated groundwater from 1255 domestic drinking-water wells and 242 public supply wells were analyzed as part of the National Water-Quality Assessment Program of the U.S. Geological Survey between 1992 and 1999. Wells were sampled to define the regional quality of the groundwater resource and, thus, were distributed geographically across large aquifers, primarily in rural areas. For each sample, as many as 60 volatile organic compounds (VOCs), 83 pesticides, and nitrate were analyzed. On the basis of previous studies, nitrate concentrations as nitrogen &ge;3 mg/L were considered to have an anthropogenic origin. VOCs were detected more frequently (44%) than pesticides (38%) or anthropogenic nitrate (28%). Seventy percent of the samples contained at least one VOC, pesticide, or anthropogenic nitrate; 47% contained at least two compounds; and 33% contained at least three compounds. The combined concentrations of VOCs and pesticides ranged from about 0.001 to 100 &mu;g/L, with a median of 0.02 &mu;g/L. Water from about 12% of the wells contained one or more compounds that exceeded U.S. Environmental Protection Agency drinking-water standards or human health criteria, primarily because of nitrate concentrations exceeding the maximum contaminant level in domestic wells. A mixture is defined as a unique combination of two or more particular compounds, regardless of the presence of other compounds that may occur in the same sample. There were 100 mixtures (significantly associated with agricultural land use) that had a detection frequency between 2% and 19%. There were 302 mixtures (significantly associated with urban land use) that had a detection frequency between 1% and <2%. Only 14 compounds (seven VOCs, six pesticides, and nitrate) contributed over 95% of the detections in these 402 mixtures; however, most samples with these mixtures also contain a variety of other compounds.

Environmental Science & Technology↗
USGS2002

Evaluating behavior of oxygen, nitrate, and sulfate during recharge and quantifying reduction rates in a contaminated aquifer

This study evaluates the biogeochemical changes that occur when recharge water comes in contact with a reduced aquifer. It specifically addresses (1) which reactions occur in situ, (2) the order in which these reactions will occur if terminal electron acceptors (TEAs) are introduced simultaneously, (3) the rates of these reactions, and (4) the roles of the aqueous and solid-phase portions of the aquifer. Recharge events of waters containing various combinations of O 2 , NO 3 , and SO 4 were simulated at a shallow sandy aquifer contaminated with waste fuels and chlorinated solvents using modified push−pull tests to quantify rates. In situ rate constants for aerobic respiration (14.4 day - 1 ), denitrification (5.04−7.44 day - 1 ), and sulfate reduction (4.32−6.48 day - 1 ) were estimated. Results show that when introduced together, NO 3 and SO 4 can be consumed simultaneously at similar rates. To distinguish the role of aqueous phase from that of the solid phase of the aquifer, groundwater was extracted, amended with NO 3 and SO 4 , and monitored over time. Results indicate that neither NO 3 nor SO 4 was reduced during the course of the aqueous-phase study, suggesting that NO 3 and SO 4 can behave conservatively in highly reduced water. It is clear that sediments and their associated microbial communities are important in driving redox reactions.

Environmental Science & Technology↗
USGS2002

Anaerobic methane oxidation in a landfill-leachate plume

The alluvial aquifer adjacent to Norman Landfill, OK, provides an excellent natural laboratory for the study of anaerobic processes impacting landfill-leachate contaminated aquifers. We collected groundwaters from a transect of seven multilevel wells ranging in depth from 1.3 to 11 m that were oriented parallel to the flow path. The center of the leachate plume was characterized by (1) high alkalinity and elevated concentrations of total dissolved organic carbon, reduced iron, and methane, and (2) negligible oxygen, nitrate, and sulfate concentrations. Methane concentrations and stable carbon isotope (δ 13 C) values suggest anaerobic methane oxidation was occurring within the plume and at its margins. Methane δ 13 C values increased from about −54‰ near the source to >−10‰ downgradient and at the plume margins. The isotopic fractionation associated with this methane oxidation was −13.6 ± 1.0‰. Methane 13 C enrichment indicated that 80−90% of the original landfill methane was oxidized over the 210-m transect. First-order rate constants ranged from 0.06 to 0.23 per year, and oxidation rates ranged from 18 to 230 μM/y. Overall, hydrochemical data suggest that a sulfate reducer-methanogen consortium may mediate this methane oxidation. These results demonstrate that natural attenuation through anaerobic methane oxidation can be an important sink for landfill methane in aquifer systems.

Environmental Science & Technology↗
USGS2002

Atmospheric mercury deposition during the last 270 years: A glacial ice core record of natural and anthropogenic sources

Mercury (Hg) contamination of aquatic ecosystems and subsequent methylmercury bioaccumulation are significant environmental problems of global extent. At regional to global scales, the primary mechanism of Hg contamination is atmospheric Hg transport. Thus, a better understanding of the long-term history of atmospheric Hg cycling and quantification of the sources is critical for assessing the regional and global impact of anthropogenic Hg emissions. Ice cores collected from the Upper Fremont Glacier (UFG), Wyoming, contain a high-resolution record of total atmospheric Hg deposition (ca. 1720−1993). Total Hg in 97 ice-core samples was determined with trace-metal clean handling methods and low-level analytical procedures to reconstruct the first and most comprehensive atmospheric Hg deposition record of its kind yet available from North America. The record indicates major atmospheric releases of both natural and anthropogenic Hg from regional and global sources. Integrated over the past 270-year ice-core history, anthropogenic inputs contributed 52%, volcanic events 6%, and background sources 42%. More significantly, during the last 100 years, anthropogenic sources contributed 70% of the total Hg input. Unlike the 2−7-fold increase observed from preindustrial times (before 1840) to the mid-1980s in sediment-core records, the UFG record indicates a 20-fold increase for the same period. The sediment-core records, however, are in agreement with the last 10 years of this ice-core record, indicating declines in atmospheric Hg deposition.

Environmental Science & Technology↗
USGS2002

Preserving the distribution of inorganic arsenic species in groundwater and acid mine drainage samples

The distribution of inorganic arsenic species must be preserved in the field to eliminate changes caused by metal oxyhydroxide precipitation, photochemical oxidation, and redox reactions. Arsenic species sorb to iron and manganese oxyhydroxide precipitates, and arsenite can be oxidized to arsenate by photolytically produced free radicals in many sample matrices. Several preservatives were evaluated to minimize metal oxyhydroxide precipitation, such as inorganic acids and ethylenediaminetetraacetic acid (EDTA). EDTA was found to work best for all sample matrices tested. Storing samples in opaque polyethylene bottles eliminated the effects of photochemical reactions. The preservation technique was tested on 71 groundwater and six acid mine drainage samples. Concentrations in groundwater samples reached 720 ??g-As/L for arsenite and 1080 ??g-As/L for arsenate, and acid mine drainage samples reached 13 000 ??g-As/L for arsenite and 3700 ??g-As/L for arsenate. The arsenic species distribution in the samples ranged from 0 to 90% arsenite. The stability of the preservation technique was established by comparing laboratory arsenic speciation results for samples preserved in the field to results for subsamples speciated onsite. Statistical analyses indicated that the difference between arsenite and arsenate concentrations for samples preserved with EDTA in opaque bottles and field speciation results were analytically insignificant. The percentage change in arsenite:arsenate ratios for a preserved acid mine drainage sample and groundwater sample during a 3-month period was -5 and +3%, respectively.

Environmental Science & Technology↗
USGS2002

Black carbon from the Mississippi river: Quantities, sources, and potential implications for the global carbon cycle

Black carbon (BC) may be a major component of riverine carbon exported to the ocean, but its flux from large rivers is unknown. Furthermore, the global distribution of BC between natural and anthropogenic sources remains uncertain. We have determined BC concentrations in suspended sediments of the Mississippi River, the 7th largest river in the world in terms of sediment and water discharge, during high flow and low flow in 1999. The 1999 annual flux of BC from the Mississippi River was 5 × 10 - 4 petagrams (1 Pg = 10 15 g = 1 gigaton). We also applied a principal components analysis to particulate-phase high molecular weight polycyclic aromatic hydrocarbon isomer ratios in Mississippi River suspended sediments. In doing so, we determined that ∼27% of the BC discharged from the Mississippi River in 1999 originated from fossil fuel combustion (coal and smelter-derived combustion), implicating fluvial BC as an important source of anthropogenic BC contamination into the ocean. Using our value for BC flux and the annual estimate for BC burial in ocean sediments, we calculate that, in 1999, the Mississippi River discharged ∼5% of the BC buried annually in the ocean. These results have important implications, not only for the global carbon cycle but also for the fluvial discharge of particulate organic contaminants into the world's oceans.

Louisiana↗
USGS2002

Response to comment on "Pharmaceuticals, hormones, and other organic wastewater contaminants in U.S. streams, 1999-2000: A national reconnaissance"

We concur with the response of Eckel to our recent publication in this Journal (1). As the author notes, the topic of emerging contaminants is currently receiving extensive media coverage and scientific notice, but there are earlier reports that foreshadow this current interest. Eckel’s comment regarding the detection of pharmaceuticals and other organic wastewater contaminants (OWC) at a Superfund landfill site (2) is well taken, as other reports confirm the presence of such compounds at waste-disposal and landfill sites (3). In fact, literature from more than 20 years ago documented the occurrence of OWCs in the environment (4-7). A significant difference between these reports and our study is that we have systematically documented the frequent presence and low concentrations of a broad suite of OWCs in a wide variety of streams across the United States.

Environmental Science & Technology↗
USGS2002

Response to comment on "Pharmaceuticals, hormones, and other organic wastewater contaminants in U.S. streams, 1999-2000: A national reconnaissance"

We thank Ericson et al. (1) for their careful review and thoughtful comments on the synthetic hormone data presented in our recent publication summarizing the results from the USGS nationwide reconnaissance for pharmaceuticals and other organic wastewater contaminants (2). Their efforts have helped raise the awareness of the difficulties in accurately measuring these compounds at the low concentrations that occur in the environment and reinforce the need for continued research in the area of analytical methods development for synthetic hormones

Environmental Science & Technology↗