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USGS2019

Variability in results from mineralogical and organic geochemical interlaboratory testing of U. S. Geological Survey shale reference materials

The expansion of unconventional petroleum resource exploration and production in the United States has led to an increase in source rock characterization efforts, particularly related to bulk organic and mineralogical properties. To support the analytical and research needs of industry and academia, as well as internal work, the U.S. Geological Survey (USGS) has collected and prepared shale geochemical reference materials (GRMs) from several major shale petroleum systems in the U.S. The sources of these materials are the Late Cretaceous Boquillas (lower Eagle Ford-equivalent) Formation (roadcut near Del Rio, TX), Late Cretaceous Mancos Shale (outcrop near Delta, CO), Devonian–Mississippian Woodford Shale (outcrop near Ardmore, OK), Late Cretaceous Niobrara Formation (quarry near Lyons, CO), Middle Devonian Marcellus Shale (creek bed in LeRoy, NY), and Eocene Mahogany zone oil shale of the Green River Formation (oil shale mine near Rifle, CO). Of particular interest in the development of these GRMs has been the examination of variability between laboratories and specific methods or instruments in commonly made measurements, including major- and trace-element concentrations, X-ray diffraction (XRD) mineralogy, total organic carbon (TOC) content, and programmed pyrolysis (PP) parameters. For the component concentrations and parameters we measured, the techniques and instrument types included: (1) elemental analysis by X-ray fluorescence, inductively coupled plasma mass spectrometry, and instrumental neutron activation analysis; (2) XRD mineralogy with various preparatory methods (spray drying or micronizing with or without internal standard); (3) TOC by combustion with infrared detection after carbonate removal or the PP approach; (4) PP by Rock-Eval 2 or more recently developed instruments (Rock-Eval 6, Source Rock Analyzer or SRA, and Hydrocarbon Analyzer With Kinetics or HAWK). Overall, the results showed that the selected shales cover a wide range of source rock organic and mineralogical properties. Major- and trace-element chemistry results showed low heterogeneity consistent with other USGS GRMs. Comparison of TOC results showed coefficients of variation (COV) of around 5% and the most consistent organic geochemical results between different laboratories and methods. Arguably the most relevant PP measurement, S2 or kerogen hydrocarbon-generating potential (mg-HC/g-rock), showed a somewhat wider range of variability than TOC (COV ~10%), but was consistent between the three modern instruments and the industry-standard Rock-Eval 2. Major phase mineralogy (mineral concentrations ≥10 wt. %, organic-free basis) were comparable between laboratories, but variability in minor phase identification and quantification was observed. Utilization of these shale GRMs as quality control samples and testing materials is expected to help support analytical and experimental efforts in the continued development of unconventional petroleum resources.

Colorado, Texas, Oklahoma↗

USGS2008

Biogeochemical response of organic-rich freshwater marshes in the Louisiana delta plain to chronic river water influx

To help evaluate effects of Mississippi River inputs to sustainability of coastal Louisiana ecosystems, we compared porewater and substrate quality of organic-rich Panicum hemitomon freshwater marshes inundated by river water annually for more than 30 years (Penchant basin, PB) or not during the same time (Barataria basin, BB). In the marshes receiving river water the soil environment was more reduced, the organic substrate was more decomposed and accumulated more sulfur. The porewater dissolved ammonium and orthophosphate concentrations were an order of magnitude higher and sulfide and alkalinity concentrations were more than twice as high in PB compared with BB marshes. The pH was higher and dissolved iron concentrations were more than an order of magnitude lower in PB marshes than in BB marshes. The influx of nutrient-rich river water did not enhance end-of-year above-ground standing biomass or vertical accretion rates of the shallow substrate. The differences in porewater chemistry and substrate quality are reasonably linked to the long-term influx of river water through biogeochemical processes and transformations involving alkalinity, nitrate and sulfate. The key factor is the continual replenishment of alkalinity, nitrate and sulfate via overland flow during high river stage each year for several weeks to more than 6 months. This leads to a reducing soil environment, pooling of the phytotoxin sulfide and inorganic nutrients in porewater, and internally generated alkalinity. Organic matter decomposition is enhanced under these conditions and root mats degraded. The more decomposed root mat makes these marshes more susceptible to erosion during infrequent high-energy events (for example hurricanes) and regular low-energy events, such as tides and the passage of weather fronts. Our findings were unexpected and, if generally applicable, suggest that river diversions may not be the beneficial mitigating agent of wetland restoration and conservation that they are anticipated to be. ?? 2008 Springer Science+Business Media B.V.

Biogeochemistry↗

USGS2011

Using stable isotopes to understand hydrochemical processes in and around a Prairie Pothole wetland in the Northern Great Plains, USA

Millions of internally drained wetland systems in the Prairie Potholes region of the northern Great Plains (USA and Canada) provide indispensable habitat for waterfowl and a host of other ecosystem services. The hydrochemistry of these systems is complex and a crucial control on wetland function, flora and fauna. Wetland waters can have high concentrations of SO 2- 4 due to the oxidation of large amounts of pyrite in glacial till that is in part derived from the Pierre shale. Water chemistry including δ 18 O H2O , δ 2 H H2O , and δ 34 S SO4 values, was determined for groundwater, soil pore water, and wetland surface water in and around a discharge wetland in North Dakota. The isotopic data for the first time trace the interaction of processes that affect wetland chemistry, including open water evaporation, plant transpiration, and microbial SO 4 reduction.

Applied Geochemistry↗

USGS2002

X-ray spectrographic determination of cesium and rubidium

An x-ray spectrographic method for the determination of rubidium and cesium was developed, using the internal-standard method and a four-channel flat-crystal spectrograph. The sensitivity is within 0.1% for cesia and 0.02% for rubidia; the precision is within 10% of the amount present. Results agree well with those obtained by flame photometry and by radio-activation.

Analytical Chemistry↗

USGS2012

Contaminants in stream sediments from seven United States metropolitan areas: part II—sediment toxicity to the amphipod Hyalella azteca and the midge Chironomus dilutus

Relationships between sediment toxicity and sediment chemistry were evaluated for 98 samples collected from seven metropolitan study areas across the United States. Sediment-toxicity tests were conducted with the amphipod Hyalella azteca (28 day exposures) and with the midge Chironomus dilutus (10 day exposures). Overall, 33 % of the samples were toxic to amphipods and 12 % of the samples were toxic to midge based on comparisons with reference conditions within each study area. Significant correlations were observed between toxicity end points and sediment concentrations of trace elements, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), or organochlorine (OC) pesticides; however, these correlations were typically weak, and contaminant concentrations were usually below sediment-toxicity thresholds. Concentrations of the pyrethroid bifenthrin exceeded an estimated threshold of 0.49 ng/g (at 1 % total organic carbon) in 14 % of the samples. Of the samples that exceeded this bifenthrin toxicity threshold, 79 % were toxic to amphipods compared with 25 % toxicity for the samples below this threshold. Application of mean probable effect concentration quotients (PECQs) based on measures of groups of contaminants (trace elements, total PAHs, total PCBs,OCpesticides, and pyrethroid pesticides [bifenthrin in particular]) improved the correct classification of samples as toxic or not toxic to amphipods compared with measures of individual groups of contaminants. Sediments are a repository for many contaminants released into surface waters. Because of this, organisms inhabiting sediments may be exposed to a wide range of contaminants (United States Environmental Protection Agency (USEPA) United States Environmental Protection Agency 2000; American Society for Testing and Materials [ASTM] American Society for Testing and Materials International 2012). Contaminants of potential concern in sediments typically include trace elements (metals), organochlorine (OC) pesticides, polychlorinated biphenyls (PCBs), and polycyclic aromatic hydrocarbons (PAHs; Ingersoll et al. 2001). In 2000, the USEPA began to restrict the use of organophosphate pesticides, such as diazinon and chlorpyrifos (Spurlock and Lee 2008). These restrictions have led to increased use of pyrethroid pesticides, which have widespread applications in both agricultural and urban environments (Kuivila et al. 2012). Pyrethroids are hydrophobic compounds that have been observed to accumulate in sediments (Laskowski 2002). Toxicity of pyrethroids in field-collected sediment from small urban streams (Weston et al. 2005; Holmes et al. 2008; Ding et al. 2010; Domagalski et al. 2010) or with pyrethroids spiked into sediment (Amweg et al. 2006; Hintzen et al. 2009) have been evaluated primarily in 10 day lethality tests conducted with the amphipod Hyalella azteca . However, the sublethal effects in long-term exposures to pyrethroids in sediment have not been evaluated, and the distribution of pyrethroids sediments has not typically been evaluated in wadeable streams (Gilliom et al. 2006). This article is the second in a series that describe the results of a study of the distribution and toxicity of pyrethroids and other co-occurring trace elements and organic contaminants (PCBs, PAHs, OC pesticides) in stream sediments from 7 metropolitan areas across the United States (Moran et al. 2012). The study evaluated 98 sediment samples collected from streams ranging from undeveloped to highly urban and differs from previous studies by sampling larger wadeable streams and avoiding point sources (such as storm drains) and other inflows (Gilliom et al. 2006). Part 1 of the series characterizes sediment contaminants in relation to urbanization and other factors in the 7 metropolitan study areas (Nowell et al. 2012). Part 2 (this article) evaluates relationships between sediment chemistry and sediment toxicity in 28 day whole-sediment exposures conducted with the amphipod H. azteca and in 10 day whole-sediment exposure conducted with the midge Chironomus dilutus (USEPA United States Environmental Protection Agency 2000; ASTM American Society for Testing and Materials International 2012). Toxicity end points evaluated in the amphipod and midge exposures included the effects of these field-collected sediments on survival, weight, or biomass of the test organisms.

Georgia;Massachusetts;Texas;Colorado;Wisconsin;Uta↗

USGS1990

Partitioning and bioavailability of mercury in an experimentally acidified Wisconsin lake

We studied the partitioning of mercury (Hg) among air, water, sediments and fish at Little Rock Lake, a clear water seepage lake in north-central Wisconsin. The lake was divided with a sea curtain into two basins, one acidified with sulfuric acid to pH 5.6 for two years and the other an untreated reference site (mean pH 6.1), to document the effects of acidification. Trace-metal-free protocols were used to measure Hg at the picomolar level in air and water. Total gaseous Hg in air samples averaged 2.0 ng/m 3 . Total Hg in unfiltered water samples collected in 1986 after the fall overturn averaged about 1 ng/L in the acidified and reference basins. Mercury in surficial sediments was strongly correlated with volatile matter content and ranged from 10 to about 170 ng/g (dry weight) in both basins. Total Hg concentrations in whole, calendar age-1 yellow perch ( Perca flavescens ), sampled after one year of residence in the lake, averaged 114 ng/g (fresh weight) in the reference basin and 135 ng/g in the acidified basin – a highly significant ( p < 0.01) difference. The mean whole-body burden (quantity) of Hg in age-1 perch did not differ between basins after the first year, but was significantly greater in the treatment basin than in the reference basin after the second year of acidification. Differences between the two basins in the bioaccumulation of Hg were attributed to internal (within-lake) processes that influence the bioavailability of the metal. An initial Hg budget for the treatment basin of Little Rock Lake showed that atmospheric deposition and sedimentary remobilization of Hg are potentially important processes influencing its biogeochemical cycling and uptake by fish.

Wisconsin↗

USGS2021

Isotope fractionation from In Vivo methylmercury detoxification in waterbirds

The robust application of stable mercury (Hg) isotopes for mercury source apportionment and risk assessment necessitates the understanding of mass-dependent fractionation (MDF) due to internal transformations within organisms. Here, we used high energy-resolution XANES spectroscopy and isotope ratios of total mercury (δ202THg) and methylmercury (δ202MeHg) to elucidate the chemical speciation of Hg and the resultant MDF due to internal MeHg demethylation in waterbirds. In three waterbirds (Clark’s grebe, Forster’s tern, south polar skua), between 17-86% of the MeHg was demethylated to inorganic mercury (iHg) species primarily in the liver and kidneys as Hg-tetraselenolate (Hg(Sec)4) and minor Hg-dithiolate (Hg(SR)2) complexes. Tissular differences between δ202THg and δ202MeHg correlated linearly with %iHg (Hg(Sec)4 + Hg(SR)2), and were interpreted to reflect a kinetic isotope effect during in vivo MeHg demethylation. The product-reactant isotopic enrichment factor (εp/r) for the demethylation of MeHg  Hg(Sec)4 was −2.2 ± 0.1‰. δ202MeHg values were unvarying within each bird regardless of Hg(Sec)4 abundance, indicating fast internal cycling or replenishment of MeHg relative to demethylation. Our findings document a universal selenium-dependent demethylation reaction in birds, provide new insights on the internal transformations and cycling of MeHg and Hg(Sec)4, and allow for mathematical correction of δ202THg values due to the MeHg  Hg(Sec)4 reaction.

ACS Earth and Space Chemistry↗

USGS2006

Hydrogeologic framework refinement, ground-water flow and storage, water-chemistry analyses, and water-budget components of the Yuma area, southwestern Arizona and southeastern California

The ground-water and surface-water system in the Yuma area in southwestern Arizona and southeastern California is managed intensely to meet water-delivery requirements of customers in the United States, to manage high ground-water levels in the valleys, and to maintain treaty-mandated water-quality and quantity requirements of Mexico. The following components in this report, which were identified to be useful in the development of a ground-water management model, are: (1) refinement of the hydrogeologic framework; (2) updated water-level maps, general ground-water flow patterns, and an estimate of the amount of ground water stored in the mound under Yuma Mesa; (3) review and documentation of the ground-water budget calculated by the Bureau of Reclamation, U.S. Department of the Interior (Reclamation); and (4) water-chemistry characterization to identify the spatial distribution of water quality, information on sources and ages of ground water, and information about the productive-interval depths of the aquifer. A refined three-dimensional digital hydrogeologic framework model includes the following hydrogeologic units from bottom to top: (1) the effective hydrologic basement of the basin aquifer, which includes the Pliocene Bouse Formation, Tertiary volcanic and sedimentary rocks, and pre-Tertiary metamorphic and plutonic rocks; (2) undifferentiated lower units to represent the Pliocene transition zone and wedge zone; (3) coarse-gravel unit; (4) lower, middle, and upper basin fill to represent the upper, fine-grained zone between the top of the coarse-gravel unit and the land surface; and (5) clay A and clay B. Data for the refined model includes digital elevation models, borehole lithology data, geophysical data, and structural data to represent the geometry of the hydrogeologic units. The top surface of the coarse-gravel unit, defined by using borehole and geophysical data, varies similarly to terraces resulting from the down cutting of the Colorado River. Clay A is nearly the same as the previous conceptual hydrogeologic model definition (Olmsted and others, 1973), except for a minor westward extension from the city of Yuma. Clay B is extended to the southerly international boundary and increased in areal extent by about two-thirds of the original extent (Olmsted and others, 1973). The other hydrogeologic units generally are the same as in the previous conceptual hydrogeologic model. Before development, the Colorado and Gila Rivers were the sources of nearly all the ground water in the Yuma area through direct infiltration of water from river channels and annual overbank flooding. After construction of upstream reservoirs and clearing and irrigation of the floodplains, the rivers now act as drains for the ground water. Ground-water levels in most of the Yuma area are higher now than they were in predevelopment time. A general gradient of ground-water flow toward the natural discharge area south of the Yuma area still exists, but many other changes in flow are evident. Ground water in Yuma Valley once flowed away from the Colorado River, but now has a component of flow towards the river and Mexicali Valley. A ground-water mound has formed under Yuma Mesa from long-term surface-water irrigation; about 600,000 to 800,000 acre-ft of water are stored in the mound. Ground-water withdrawals adjacent to the southerly international boundary have resulted in water-level declines in that area. The reviewed and documented water budget includes the following components: (1) recharge in irrigated areas, (2) evapotranspiration by irrigated crops and phreatophytes, (3) ground-water return flow to the Colorado River, and (4) ground-water withdrawals (including those in Mexicali Valley). Recharge components were calculated by subtracting the amount of water used by crops from the amount of water delivered. Evapotranspiration rates were calculated on the basis of established methods, thus were appropriate for input to the ground-water flow model developed by the Bureau of Reclamation (William Greer, hydrologist, Bureau of Reclamation, written commun., 2005). Evapotranspiration by crops and phreatophytes were calculated by using crop coefficient methods and meteorological data. Other methods of calculating evapotranspiration rates by using combinations of satellite imagery and ground-based data could be used for higher spatial and temporal resolution. Ground-water return flow during years of low flow on the Colorado River (1972–82, 1987–92, and 1994–96) averaged 79,000 acre-ft per year. Ground-water withdrawal data for 1970–99 were similar to other estimates made by the U.S. Geological Survey for the Yuma area. New water-chemistry data were collected in 12 wells and 8 canals/drains to characterize spatial patterns in chemical constituents, determine isotopic ages of water, infer possible sources of ground water, and locate the vertical intervals of the aquifer that contribute most water to wells. Depth-dependent samples were collected at one of the wells (YM-10). A large quantity of water-quality data were compiled from Bureau of Reclamation and U.S. Geological Survey records and merged into the U.S. Geological Survey National Water Information System database. New samples were analyzed for major ions, nutrients, stable isotopes of oxygen and hydrogen, tritium ( 3 H), and carbon-14 ( 14 C) (along with C 13 /C 12 ratios). Light values of oxygen-18 ( 18 O) and deuterium ( 2 H, D) in well 242-2 indicate recharge from the Colorado River. Heavy water samples from wells 242-22, CADC, and Mesa del Sol indicate local recharge sources. Tritium data indicate there is young water in wells in the valleys and near the edge of Yuma Mesa, while older water is found far from the Colorado River. 14 C data indicate that water from wells near the southerly international boundary is at least several thousand years old.

Arizona, California↗

USGS2002

Apparatus for continuous extraction of nonpolar compounds from water applied to determination of chlorinated pesticides and intermediates

A continuous, multichamber liquid-liquid extractor, with internal solvent recycle, for the extraction of nonpolar contaminants from natural waters is described. The multichamber arrangement makes it possible to judge the completeness of extraction of a given component from the aqueous stream. Recoveries as high as 100% are obtained by applying the apparatus to the extraction of the pesticides aldrin, dieldrin, and endrin and their manufacturing intermediates.

Analytical Chemistry↗

USGS1953

Method for determination of small amounts of rare earths and thorium in phosphate rocks

In laboratory investigations, interest developed in the possible rare-earth content of phosphate samples from Florida and the northwestern United States. Because of the difficulty of making chemical determinations of traces of individual rare earths, a combined chemical-spectrographic method was investigated. After removal of iron by the extraction of the chloride with ether, the rare earths and thorium are concentrated by double oxalate precipitation, using calcium as a carrier. The rare earths are freed from calcium by an ammonium hydroxide precipitation with a fixed amount of aluminum as a carrier. The aluminum also serves as an internal standard in the final spectrographic analysis. The method will determine from 0.02 to 2 mg. of each rare earth with an error no greater than 10%. The investigation has resulted in a fairly rapid and precise procedure, involving no special spectrographic setup. The method could be applied to other types of geologic materials with the same expected accuracy.

Analytical Chemistry↗

USGS2019

Columbia Environmental Research Center

The U.S. Geological Survey Columbia Environmental Research Center performs research to solve challenging environmental problems related to contaminants and habitat alterations in aquatic and terrestrial ecosystems. The research is interdisciplinary and pursued through partnerships within the U.S. Geological Survey and with national, international, state, and local agencies; nongovernmental organizations; and universities. Research is prioritized to provide science to the U.S. Department of the Interior and other natural resource management agencies to inform rehabilitation of degraded habitats and imperiled fish and wildlife populations. The Columbia Environmental Research Center was established in 1966 in Columbia, Missouri, as the U.S. Fish and Wildlife Service’s Fish Pesticide Research Laboratory; the Columbia Environmental Research Center was incorporated into the U.S. Geological Survey in 1996. The U.S. Geological Survey’s staff of 130 includes 90 scientists of which one-half have advanced degrees in ecology, toxicology, biology, biochemistry, chemistry, hydrology, geology, and information technology.

Missouri↗

USGS2003

Methodological refinements in the determination of 146 polychlorinated biphenyls, including non-ortho- and mono-ortho-substituted PCBs, and 26 organochlorine pesticides as demonstrated in heron eggs

A method for the determination of 146 polychlorinated biphenyls (PCBs), including four non-ortho- and eight mono-ortho-substituted congeners, and 26 chlorinated pesticides is described. The method consists of ultrasonic extraction, Florisil cleanup, HPLC fractionation over porous graphitic carbon (PGC), and final determination with GC/ECD, GC/MS, or both. Two PCB congeners (PCB 30 and PCB 161) and two polybromobiphenyls (2,4‘,5-tribromobiphenyl and 3,3‘,4,4‘-tetrabromobiphenyl) were used as surrogate standards to evaluate the analytical efficiency. Four PCB congeners, PCB 14 and PCB 159 for the first fraction, PCB 61 for the second fraction, and PCB 204 for the third fraction, were used as internal standards to monitor the GC performance. The retention behavior of PCBs and pesticides on the PGC column are discussed. The method was found to be reproducible, effective, and reliable under the operational conditions proposed and was applied successfully to the analysis of individual PCBs and chlorinated pesticides in black-crowned night heron ( Nycticorax nycticorax ) egg samples.

Maryland↗

USGS2007

Aquifer susceptibility to perchlorate contamination in a highly urbanized environment

Perchlorate contamination from anthropogenic sources has been released into the Rialto-Colton, California, USA, groundwater flow system since the 1940s during its production, distribution, storage, and use. Preliminary analysis of lithological, geophysical, and water-chemistry data provided new understanding of the pathways of perchlorate migration that aid in assessing the susceptibility of drinking-water supplies to contamination within the Rialto-Colton basin. Vertical migration of perchlorate into the main water-producing aquifers is restricted by an areally extensive old soil surface; however, perchlorate data indicate contamination below this soil surface. Possible pathways for the downward migration of the contaminated water include wellbore flow and discontinuities in the old soil surface. Horizontal migration of perchlorate is influenced by lithology and faults within the basin. The basin fill is a heterogeneous mixture of boulders, gravel, sand, silt, and clay, and internal faults may restrict perchlorate migration in some areas.

California↗

USGS2013

Wetlands serve as natural sources for improvement of stream ecosystem health in regions affected by acid deposition

For over 40 years, acid deposition has been recognized as a serious international environmental problem, but efforts to restore acidified streams and biota have had limited success. The need to better understand the effects of different sources of acidity on streams has become more pressing with the recent increases in surface water organic acids, or 'brownification' associated with climate change and decreased inorganic acid deposition. Here, we carried out a large scale multi-seasonal investigation in the Adirondacks, one of the most acid-impacted regions in the United States, to assess how acid stream producers respond to local and watershed influences and whether these influences can be used in acidification remediation. We explored the pathways of wetland control on aluminum chemistry and diatom taxonomic and functional composition. We demonstrate that streams with larger watershed wetlands have higher organic content, lower concentrations of acidic anions, and lower ratios of inorganic to organic monomeric aluminum, all beneficial for diatom biodiversity and guilds producing high biomass. Although brownification has been viewed as a form of pollution, our results indicate that it may be a stimulating force for biofilm producers with potentially positive consequences for higher trophic levels. Our research also reveals that the mechanism of watershed control of local stream diatom biodiversity through wetland export of organic matter is universal in running waters, operating not only in hard streams, as previously reported, but also in acid streams. Our findings that the negative impacts of acid deposition on Adirondack stream chemistry and biota can be mitigated by wetlands have important implications for biodiversity conservation and stream ecosystem management. Future acidification research should focus on the potential for wetlands to improve stream ecosystem health in acid-impacted regions and their direct use in stream restoration, for example, through stream rechanneling or wetland construction in appropriate hydrologic settings.

Global Change Biology↗

USGS2025

Targeted quantitation of 6ppd-quinone in fish tissue samples with liquid chromatography-tandem mass spectrometry

The tire additive transformation product N -(1,3-dimethylbutyl)- N’ -phenyl- p -phenylenediamine-quinone (6PPD-quinone) has recently garnered global attention due to its acute toxicity to some salmonids, such as coho salmon ( Oncorhynchus kisutch ), and its ubiquitous presence in urban stormwater systems. In the present study, we developed and compared the extraction efficiency of two sample preparation methodologies for quantification of 6PPD-quinone among two fish tissue sample types that included fillet of smallmouth bass ( Micropterus dolomieu ) and whole-body samples of O. kisutch fry subjected to in vivo exposure tests with 6PPD-quinone. The two sample preparation methods tested included an accelerated solvent extraction (ASE) approach and a sonication extraction approach. Both sample preparation methods included identical purification steps for the crude sample extracts with enhanced matrix removal cartridges. The purified sample extracts were subjected to targeted analysis of 6PPD-quinone using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The results showed that extractions made with the reported ASE method demonstrated significantly higher absolute recovery (80–96%) of the extracted internal standard, [ 13 C 6 ]-6PPD-quinone, than sonication-based extractions (74–80%) in both fish tissue sample types. The proposed ASE method shows acceptable limits of quantification (0.37–0.67 ng g −1 ), linearity (R 2 > 0.996), and repeatability (RSD ≤ 9%). This work advances research capabilities for investigations on the toxicokinetic processes of 6PPD-quinone in biological samples.

Environmental Toxicology and Chemistry↗

USGS1977

Application of epithermal neutron activation in multielement analysis of silicate rocks employing both coaxial Ge(Li) and low energy photon detector systems

The instrumental activation analysis of silicate rocks using epithermal neutrons has been studied using both high resolution coaxial Ge(Li) detectors and low energy photon detectors, and applied to the determination of 23 elements in eight new U.S.G.S. standard rocks. The analytical use X-ray peaks associated with electron capture or internal conversion processes has been evaluated. Of 28 elements which can be considered to be determinable by instrumental means, the epithermal activation approach is capable of giving improved sensitivity and precision in 16 cases, over the normal INAA procedure. In eleven cases the use of the low energy photon detector is thought to show advantages over convertional coaxial Ge(Li) spectroscopy. ?? 1977 Akade??miai Kiado??.

Journal of Radioanalytical Chemistry↗

USGS2012

Interactions of tissue and fertilizer nitrogen on decomposition dynamics of lignin-rich conifer litter

High tissue nitrogen (N) accelerates decomposition of high-quality leaf litter in the early phases of mass loss, but the influence of initial tissue N variation on the decomposition of lignin-rich litter is less resolved. Because environmental changes such as atmospheric N deposition and elevated CO 2 can alter tissue N levels within species more rapidly than they alter the species composition of ecosystems, it is important to consider how within-species variation in tissue N may shape litter decomposition and associated N dynamics. Douglas-fir (Pseudotsuga menziesii ) is a widespread lignin-rich conifer that dominates forests of high carbon (C) storage across western North America, and displays wide variation in tissue and litter N that reflects landscape variation in soil N. We collected eight unique Douglas-fir litter sources that spanned a two-fold range in initial N concentrations (0.67–1.31%) with a narrow range of lignin (29–35%), and examined relationships between initial litter chemistry, decomposition, and N dynamics in both ambient and N fertilized plots at four sites over 3 yr. High initial litter N slowed decomposition rates in both early (0.67 yr) and late (3 yr) stages in unfertilized plots. Applications of N fertilizer to litters accelerated early-stage decomposition, but slowed late-stage decomposition, and most strongly affected low-N litters, which equalized decomposition rates across litters regardless of initial N concentrations. Decomposition of N-fertilized litters correlated positively with initial litter manganese (Mn) concentrations, with litter Mn variation reflecting faster turnover of canopy foliage in high N sites, producing younger litterfall with high N and low Mn. Although both internal and external N inhibited decomposition at 3 yr, most litters exhibited net N immobilization, with strongest immobilization in low-N litter and in N-fertilized plots. Our observation for lignin-rich litter that high initial N can slow decomposition yet accelerate N release differs from findings where litter quality variation across species promotes coupled C and N release during decomposition. We suggest reevaluation of ecosystem models and projected global change effects to account for a potential decoupling of ecosystem C and N feedbacks through litter decomposition in lignin-rich conifer forests.

Ecosphere↗

USGS2024

Monitoring marine eruptions

Introduction Submarine volcanoes produce much of the same seismicity and eruptive activity as subaerial volcanoes and can pose hazards to society. Although they can be monitored with similar techniques and methods as described in other chapters of this volume, their submerged location brings unique challenges. This chapter addresses these challenges and provides recommendations for monitoring volcanoes fully or partly in marine environments to meet the capabilities described in other chapters of this volume. The United States and its territories host dozens of submarine volcanoes with most (around 60) in the Commonwealth of the Northern Mariana Islands. Approximately 20 of the Northern Mariana Islands submarine volcanoes are known to be hydrothermally active, and 10 have confirmed eruptions since the 1950s (for example, Baker and others, 2008; Tepp and others, 2019a). Nine of those volcanoes were considered by the National Volcanic Threat Assessment (Ewert and others, 2018) to have a combination of eruptive type and summit depth that poses a higher risk of hazardous eruptions, although only one was listed as a moderate (level 3) threat. Other notable submarine volcanoes of interest to the United States that have historically erupted are Axial Seamount off the Washington State coast, Kamaʻehuakanaloa in Hawaiʻi, and Vailuluʻu seamount in American Samoa. All of these, however, have a low risk of hazards because of their depth (greater than 600 meters below sea level) and eruptive type and so are not included in the National Volcanic Threat Assessment. In addition to submarine volcanoes, the submerged flanks of island volcanoes can also be a source of hazardous submarine eruptions—for example, the 1877 eruption of Mauna Loa, Hawai‘i, in Kealakekua Bay (Wanless and others, 2006). The most notable submarine eruption in recent times was the 2022 eruption of Hunga Tonga–Hunga Haʻapai in Tonga, which was one of the largest eruptions on Earth in the past 100 years. It created a massive volcanic plume, unprecedented shock waves, and far-reaching tsunami (Lynett and others, 2022). Other recent submarine eruptions in the Pacific Ocean Basin have produced subaerial plumes that reached aircraft heights (Carey and others, 2014) and large pumice rafts that can affect marine traffic and harbors (for example, Jutzeler and others, 2014; Kornei, 2019). These examples illustrate the potential hazards of major submarine eruptions. Yet, submarine volcanoes are largely unmonitored, and many eruptions occur that are unnoticed or only identified hours or days afterward. Within U.S. territory, submarine volcanoes in the Northern Mariana Islands have been known to produce eruptive activity that can affect society. Reports from fishermen and other marine vessels in the Northern Mariana Islands have noted underwater explosions, sea-surface discoloration, and bubbling water, all of which are known to be signs of submarine volcanic activity. South Sarigan seamount, located about 160 kilometers (km) north of Saipan, erupted in 2010 from greater than 150 meters below the sea surface, resulting in a gas and ash plume that reached more than 11.9 km into the atmosphere (for example, Searcy, 2013; Embley and others, 2014), high enough to affect international air traffic. Precursory and co-eruptive seismicity was detected on the regional Northern Mariana Islands seismic network (Searcy, 2013) and on global monitoring instruments (Green and others, 2013). Monitoring of submarine volcanoes is best accomplished with marine-based instrumentation, which is also useful for monitoring small island volcanoes that may not have the land area necessary for comprehensive subaerial monitoring. The primary marine-based instrumentation used for submarine volcanoes includes ocean-bottom pressure sensors to assess sea-floor deformation, ocean-bottom seismometers (OBSs) to detect seismicity, and both moored and ocean-bottom hydrophones to detect submarine explosions. Other sensors offer important monitoring data, such as turbidity, temperature, and chemistry of hydrothermal emissions. Marine-based instruments are typically deployed in campaign-style networks with no real-time telemetry owing to cost considerations and technical limitations. However, when necessary, marine instruments can be operated in real time using cables to transmit data to land-based facilities; other technologies for this purpose are in use or in development, such as acoustic transmission from the instrument to a moored buoy (Matsumoto and others, 2016) and a winch-based system with a satellite antenna that is part of the instrument mooring (Matsumoto and others, 2019). Emerging technologies for marine-based monitoring may be considered as part of a future monitoring plan. These technologies include ocean gliders and floats with on-board hydrophones that have been used to record earthquakes and submarine eruptions (for example, Matsumoto and others, 2013; Sukhovich and others, 2015) and fiber-optic cables that have been used as strainmeters to detect earthquakes (for example, Marra and others, 2018; Lindsey and others, 2019). Land-based instruments and satellites can also provide some capability for monitoring submarine volcanoes, but they provide more limited observations than marine-based instrumentation.

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