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USGS2015

Inter-laboratory variation in the chemical analysis of acidic forest soil reference samples from eastern North America

Long-term forest soil monitoring and research often requires a comparison of laboratory data generated at different times and in different laboratories. Quantifying the uncertainty associated with these analyses is necessary to assess temporal changes in soil properties. Forest soil chemical properties, and methods to measure these properties, often differ from agronomic and horticultural soils. Soil proficiency programs do not generally include forest soil samples that are highly acidic, high in extractable Al, low in extractable Ca and often high in carbon. To determine the uncertainty associated with specific analytical methods for forest soils, we collected and distributed samples from two soil horizons (Oa and Bs) to 15 laboratories in the eastern United States and Canada. Soil properties measured included total organic carbon and nitrogen, pH and exchangeable cations. Overall, results were consistent despite some differences in methodology. We calculated the median absolute deviation (MAD) for each measurement and considered the acceptable range to be the median 6 2.5 3 MAD. Variability among laboratories was usually as low as the typical variability within a laboratory. A few areas of concern include a lack of consistency in the measurement and expression of results on a dry weight basis, relatively high variability in the C/N ratio in the Bs horizon, challenges associated with determining exchangeable cations at concentrations near the lower reporting range of some laboratories and the operationally defined nature of aluminum extractability. Recommendations include a continuation of reference forest soil exchange programs to quantify the uncertainty associated with these analyses in conjunction with ongoing efforts to review and standardize laboratory methods.

Ecosphere↗

USGS2024

A universal method for the simultaneous determination of environmental pollutants in marine biological samples: Per- and polyfluoroalkyl substances and antibiotics as a case study

Conventional detection technologies for environmental contaminants have primarily focused on providing accurate qualitative and quantitative evaluations for single pollutant types, leading to increased costs and an inability to satisfy the growing demand for detecting a broader spectrum of pollutants. Here, we introduced a novel analytical method to simultaneously measure the concentration levels of diverse environmental pollutants, characterized by their distinct properties, across complex biological samples. Per- and polyfluoroalkyl substances (PFAS) and antibiotics were used as a case study due to their frequency of detection in the environment and known impacts Our method harnesses the salting-out effect of sodium chloride on proteins within the muscle tissues of 178 marine species, which significantly reduces the addition of extraneous substances, mitigates matrix interference, and avoids reliance on solid-phase extraction or dispersive extraction agents. The method provides a simultaneous pretreatment for the detection of several compounds, with detection limits from 0.002 to 0.41 ng/g dry weight, which are substantially lower than conventional methods. Overall, this method streamlines efficiency, decreases costs, lessens matrix effects, and sets a solid groundwork for future applications in the concurrent detection of a broader spectrum of environmentally pertinent pollutants with varied characteristics.

ACS ES&T Water↗

USGS2021

A simplified method for rapid estimation of emergency water supply needs after earthquakes

Researchers are investigating the problem of estimating households with potable water service outages soon after an earthquake. Most of these modeling approaches are computationally intensive, have large proprietary data collection requirements or lack precision, making them unfeasible for rapid assessment, prioritization, and allocation of emergency water resources in large, complex disasters. This study proposes a new simplified analytical method—performed without proprietary water pipeline data—to estimate water supply needs after earthquakes, and a case study of its application in the HayWired earthquake scenario. In the HayWired scenario—a moment magnitude (M w ) 7.0 Hayward Fault earthquake in the San Francisco Bay Area, California (USA)—an analysis of potable water supply in two water utility districts was performed using the University of Colorado Water Network (CUWNet) model. In the case study, application of the simplified method extends these estimates of household water service outage to the nine counties adjacent to the San Francisco Bay, aggregated by a ~250 m 2 (nine-arcsecond) grid. The study estimates about 1.38 million households (3.7 million residents) out of 7.6 million residents (2017, ambient, nighttime population) with potable water service outage soon after the earthquake—about an 8% increase from the HayWired scenario estimates.

California↗

USGS2009

Using indirect methods to constrain symbiotic nitrogen fixation rates: A case study from an Amazonian rain forest

Human activities have profoundly altered the global nitrogen (N) cycle. Increases in anthropogenic N have had multiple effects on the atmosphere, on terrestrial, freshwater and marine ecosystems, and even on human health. Unfortunately, methodological limitations challenge our ability to directly measure natural N inputs via biological N fixation (BNF)-the largest natural source of new N to ecosystems. This confounds efforts to quantify the extent of anthropogenic perturbation to the N cycle. To address this gap, we used a pair of indirect methods -analytical modeling and N balance-to generate independent estimates of BNF in a presumed hotspot of N fixation , a tropical rain forest site in central Rondônia in the Brazilian Amazon Basin. Our objectives were to attempt to constrain symbiotic N fixation rates in this site using indirect methods , and to assess strengths and weaknesses of this approach by looking for areas of convergence and disagreement between the estimates. This approach yielded two remarkably similar estimates of N fixation . However, when compared to a previously published bottom-up estimate, our analysis indicated much lower N inputs via symbiotic BNF in the Rondônia site than has been suggested for the tropics as a whole. This discrepancy may reflect errors associated with extrapolating bottom-up fluxes from plot-scale measures, those resulting from the indirect analyses, and/or the relatively low abundance of legumes at the Rondônia site. While indirect methods have some limitations, we suggest that until the technological challenges of directly measuring N fixation are overcome, integrated approaches that employ a combination of model-generated and empirically-derived data offer a promising way of constraining N inputs via BNF in natural ecosystems.

Biogeochemistry↗

USGS2022

Pharmaceutical pollution of the world’s rivers

Environmental exposure to active pharmaceutical ingredients (APIs) can have negative effects on the health of ecosystems and humans. While numerous studies have monitored APIs in rivers, these employ different analytical methods, measure different APIs, and have ignored many of the countries of the world. This makes it difficult to quantify the scale of the problem from a global perspective. Furthermore, comparison of the existing data, generated for different studies/regions/continents, is challenging due to the vast differences between the analytical methodologies employed. Here, we present a global-scale study of API pollution in 258 of the world’s rivers, representing the environmental influence of 471.4 million people across 137 geographic regions. Samples were obtained from 1,052 locations in 104 countries (representing all continents and 36 countries not previously studied for API contamination) and analyzed for 61 APIs. Highest cumulative API concentrations were observed in sub-Saharan Africa, south Asia, and South America. The most contaminated sites were in low- to middle-income countries and were associated with areas with poor wastewater and waste management infrastructure and pharmaceutical manufacturing. The most frequently detected APIs were carbamazepine, metformin, and caffeine (a compound also arising from lifestyle use), which were detected at over half of the sites monitored. Concentrations of at least one API at 25.7% of the sampling sites were greater than concentrations considered safe for aquatic organisms, or which are of concern in terms of selection for antimicrobial resistance. Therefore, pharmaceutical pollution poses a global threat to environmental and human health, as well as to delivery of the United Nations Sustainable Development Goals.

Proceedings of the National Academy of Sciences↗

USGS2010

Method description, quality assurance, environmental data, and other Information for analysis of pharmaceuticals in wastewater-treatment-plant effluents, streamwater, and reservoirs, 2004-2009

Abstract Wastewater-treatment-plant (WWTP) effluents are a demonstrated source of pharmaceuticals to the environment. During 2004-09, a study was conducted to identify pharmaceutical compounds in effluents from WWTPs (including two that receive substantial discharges from pharmaceutical formulation facilities), streamwater, and reservoirs. The methods used to determine and quantify concentrations of seven pharmaceuticals are described. In addition, the report includes information on pharmaceuticals formulated or potentially formulated at the two pharmaceutical formulation facilities that provide substantial discharge to two of the WWTPs, and potential limitations to these data are discussed. The analytical methods used to provide data on the seven pharmaceuticals (including opioids, muscle relaxants, and other pharmaceuticals) in filtered water samples also are described. Data are provided on method performance, including spike data, method detection limit results, and an estimation of precision. Quality-assurance data for sample collection and handling are included. Quantitative data are presented for the seven pharmaceuticals in water samples collected at WWTP discharge points, from streams, and at reservoirs. Occurrence data also are provided for 19 pharmaceuticals that were qualitatively identified. Flow data at selected WWTP and streams are presented. Between 2004-09, 35-38 effluent samples were collected from each of three WWTPs in New York and analyzed for seven pharmaceuticals. Two WWTPs (NY2 and NY3) receive substantial inflows (greater than 20 percent of plant flow) from pharmaceutical formulation facilities (PFF) and one (NY1) receives no PFF flow. Samples of effluents from 23 WWTPs across the United States were analyzed once for these pharmaceuticals as part of a national survey. Maximum pharmaceutical effluent concentrations for the national survey and NY1 effluent samples were generally less than 1 ug/L. Four pharmaceuticals (methadone, oxycodone, butalbital and metaxalone) in samples of NY3 effluent had median concentrations ranging from 3.4 to greater than 400 ug/L. Maximum concentrations of oxycodone (1,700 ug/L) and metaxalone (3,800 ug/L) in samples from NY3 effluent exceeded 1,000 ug/L. Three pharmaceuticals (butalbital, carisoprodol, and oxycodone) in samples of NY2 effluent had median concentrations ranging from 2 to 11 ug/L. These findings suggest that current 2 manufacturing practices at these PFFs can result in pharmaceutical concentrations from 10 to 1,000 times higher than those typically found in WWTP effluents.

Open-File Report↗

USGS2019

Understanding organic matter heterogeneity and maturation rate by Raman spectroscopy

Solid organic matter (OM) in sedimentary rocks produces petroleum and solid bitumen when it undergoes thermal maturation. The solid OM is a ‘geomacromolecule’, usually representing a mixture of various organisms with distinct biogenic origins, and can have high heterogeneity in composition. Programmed pyrolysis is a common method to reveal bulk geochemical characteristics of the dominant OM, while detailed organic petrography is required to reveal information about the biogenic origin of contributing macerals. Despite the advantages of programmed pyrolysis, it cannot provide information about the heterogeneity of chemical compositions present in the individual OM types. Therefore, other analytical techniques such as Raman spectroscopy are necessary. In this study, we compared geochemical characteristics and Raman spectra of two sets of naturally and artificially matured Bakken source rock samples. A continuous Raman spectral map on solid bitumen particles was created from the artificially matured hydrous pyrolysis residues, in particular, to show the systematic chemical modifications in microscale. Spectroscopic data was plotted for both sets against thermal maturity to compare maturation rate/path for these two separate groups. The outcome showed that artificial maturation through hydrous pyrolysis does not follow the same trend as naturally-matured samples although having similar solid bitumen reflectance values (%SBRo). Furthermore, Raman spectroscopy of solid bitumen from artificially matured samples indicated the heterogeneity of OM decreases as maturity increases. This may represent an alteration in chemical structure towards more uniform compounds at higher maturity. This study may emphasize the necessity of using analytical methods such as Raman spectroscopy along with conventional geochemical methods to better reveal the underlying chemical structure of OM. Finally, observation by Raman spectroscopy of chemical alteration of OM during artificial maturation may assist in the proposal of improved pyrolysis protocols to better resemble natural geologic processes.

North Dakota↗

USGS2020

Liquid chromatographic method for determining the concentration of bisazir in water

Barrier dams, traps, and lampricides are the techniques currently used by the Great Lakes Fishery Commission to control sea lampreys {Petromyzon marinug) in the Great Lakes. To augment these control techniques, a sterile-male-release research program was initiated at the Lake Huron Biological Station. Male sea lampreys were sterilized by intraperitoneal injection of the chemical sterilant P,P-bis(1-aziridinyl)- N methylphosphinothioic amide (bisazir). An analytical method was needed to quantitate the concentration of bisazir in water and to routinely verify that bisazir (>25 μg/L) does not persist in the treated effluent discharged from the sterilization facility to Lake Huron. A rapid, accurate, and sensitive liquid chromatographic (LC) method was developed for determining bisazir in water. Bisazir was dissolved in Lake Huron water; extracted and concentrated on a C 18 solid-phase extraction column; eluted with methanol; and quantitated by reversed-phase LC using a Cis column, amobile phase of 70% water and 30% methanol (v/v), and UV detection (205 nm). Bisazir retention time was 7-8 min; total run time was about 20 min. Method detection limit for bisazir dissolved in Lake Huron water was about 15 μg/L. Recovery from Lake Huron water fortified with bisazir at 100 μg/L was 94% (95% confidence interval, 90.2-98.2%).

Journal of AOAC International↗

USGS2026

Appendix 6: Overview of iPOM 2.0: Updates to wolf abundance estimation in Montana

Montana Fish, Wildlife and Parks (MFWP) uses the integrated Patch Occupancy Model (iPOM) to estimate statewide and regional wolf abundance. During the early years of recovery, wolf abundance was tracked using minimum counts. As the population increased, limitations of this method became apparent, motivating development of a model-based approach for estimating abundance. iPOM development began in 2006, was operationalized in 2013, and has been used in its current form (iPOM 1.0) since 2021. Since its inception, iPOM has been developed and presented as an adaptive modeling framework intended to evolve as new data and analytical methods become available1. Here, we briefly present ongoing work to produce the next iteration of iPOM, hereafter iPOM 2.0, and summarize major model updates and resulting preliminary wolf abundance estimates. iPOM uses models for occupancy, territory size, and pack size, along with monitoring data collected by MFWP wolf specialists and potential wolf sightings reported by deer and elk hunters during the 5-week general rifle season each Nov-Dec. These monitoring data, wolf sightings, and covariates for habitat and survey effort are used to model occupancy of packs on a statewide grid of 600-km 2 cells. The area used by wolves is then estimated as each cell’s occupancy estimate multiplied by grid cell area. iPOM estimates pack abundance by dividing this area by predicted territory sizes, and in-pack wolf abundance by multiplying pack abundance by estimated group size. This is combined with a lone wolf rate to estimate total wolf abundance (see Sells et al. 1 for a full description of iPOM 1.0). This technical summary provides a high-level overview of the proposed iPOM updates and their implications for wolf abundance estimates. The estimates presented here represent results as of June 2026 and are provided to inform upcoming discussions surrounding harvest management and regulations (e.g., season dates, quotas, methods). Results are preliminary and remain subject to final model refinement and peer review.

Montana↗

USGS2023

Centurial persistence of forever chemicals at military fire training sites

Drinking water contamination by per- and polyfluoroalkyl substances (PFAS) is widespread near more than 300 United States (U.S.) military bases that used aqueous film-forming foams (AFFF) for fire training and firefighting activities. Much of the PFAS at these sites consist of precursors that can transform into terminal compounds of known health concern but are omitted from standard analytical methods. Here, we estimate the expected duration and contribution of precursor biotransformation to groundwater PFAS contamination at an AFFF-contaminated military base on Cape Cod, Massachusetts, United States, by optimizing a geochemical box model using measured PFAS concentrations from a multidecadal time series of groundwater and a soil survey in the source zone. A toolbox of analytical techniques used to reconstruct the mass budget of PFAS showed that precursors accounted for 46 ± 8% of the extractable organofluorine (a proxy for total PFAS) across years. Terminal PFAS still exceed regulatory limits by 2000-fold decades after AFFF use ceased. Measurements and numerical modeling show that sulfonamido precursors are retained in the vadose zone and their slow biotransformation into perfluoroalkyl sulfonates (half-life > 66 yr) sustains groundwater concentrations of perfluorobutane sulfonate (PFBS) and perfluorohexane sulfonate (PFHxS). The estimated PFAS reservoir in the vadose zone and modeled flux into groundwater suggest PFAS contamination above regulatory guidelines will persist for centuries without remediation.

Massachusetts↗

USGS2019

Determination of study reporting limits for pesticide constituent data for the California Groundwater Ambient Monitoring and Assessment Program Priority Basin Project, 2004–2018—Part 1: National Water Quality Schedules 2003, 2032, or 2033, and 2060

The California Groundwater Ambient Monitoring and Assessment Program Priority Basin Project (GAMA-PBP) is a long-term cooperative project designed to assess the quality of groundwater resources used for public and domestic drinking water supplies in the State of California, to monitor and evaluate changes to that quality, to investigate the human and natural factors controlling water quality, and to improve the availability of comprehensive groundwater quality data and information. Between May 18, 2004, and May 3, 2018, the GAMA-PBP collected 3001 groundwater samples for analysis of pesticide constituents by the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL)(note that ‘pesticide constituents’ includes parent compounds and degradates). Of these samples, 2994 were analyzed for pesticide constituents on schedules 2003, 2032, or 2033 (65 to 84 constituents), and 840 were analyzed for pesticide constituents on schedule 2060 (58 constituents). The original dataset reported by the NWQL to the USGS National Water Information System (NWIS) database contained a total of 2,688 detections of 78 pesticide constituents and 253,825 non-detections. In this original dataset, 33 percent of the 3,001 samples analyzed had reported detections of one or more pesticide constituents. This report describes the GAMA-PBP data-quality objectives for pesticide data, the procedures used to establish study reporting limits, and use of those reporting limits to censor the data from the NWQL so that the final data published by the GAMA-PBP meet these data-quality objectives. The final GAMA-PBP dataset for samples collected from May 2004 to May 2018, after censoring, had a total of 1,632 detections of 37 pesticide constituents. In the final GAMA-PBP dataset, 25 percent of the 3,001 samples analyzed had detections of one or more pesticide constituents. The presence of pesticides in groundwater is commonly evaluated by calculating detection frequencies. Detection frequencies for pesticides are sensitive to detection limits and method performance for concentrations near those limits; therefore, the two primary data quality issues addressed in the GAMA-PBP data-quality objectives for pesticides are (1) establishing criteria for classifying data from the laboratory as detections or non-detections for the purpose of data reporting by the project and (2) accounting for changes in analytical methods or method performance over time. The GAMA-PBP addresses these issues by developing study reporting limits that are used as the boundary between detections and non-detections for the reporting of GAMA-PBP results. These reporting limits are defined from method detection limits (MDLs) provided by the NWQL, unless examination of results from laboratory set blanks (LSBs) and GAMA-PBP field blanks indicates that a higher concentration censoring limit is warranted. The GAMA-PBP selected the MDL as the primary choice for defining study reporting limits for consistency with U.S. Environmental Protection Agency (EPA) guidelines for reporting detections of pesticides and other organic constituents. A five-step procedure is used to develop study reporting limits and censor the GAMA-PBP dataset accordingly. The effect of the censoring at each step is described to provide information about the relative effect of each step on the overall censoring of the dataset. Steps 1 and 2 can be implemented at the time the data are received, whereas steps 3−5 require information accumulated over an extended period. Step 1: Reject results that were most likely the result of specific contamination instances attributable to unusual field or laboratory conditions during sample collection or processing. Two such instances were identified, leading to rejection of 25 detections, which were assigned a data-quality indicator code of “Q” for “reviewed and rejected” in the NWIS database. Step 2: Use the NWQL MDLs in effect at the time each sample was analyzed as the reporting limit. A total of 506 detections were censored on this basis. Step 3: Use the maximum MDL established by the NWQL during July 2004–August 2018 (MDLmax) as the reporting limit. The rationale for using the MDLmax as the reporting limit is based primarily on the observation that the concentrations of MDLs generally increased over time. A total of 438 detections were censored on this basis. Step 4: Use the LSBs to identify periods of greater potential laboratory contamination bias and define raised reporting limits to be used during those periods. These periods were defined by using a moving average detection frequency approach. For consistency with the NWQL procedures for defining raised reporting limits on the basis of detections in LSBs, the raised reporting limits were defined as equal to three times the highest concentration measured in an LSB during the period. A total of 25 detections in groundwater samples analyzed during periods of increased laboratory contamination bias were censored. Step 5: Use the LSBs and field blanks to identify potential contamination bias from field or laboratory processes outside of the time periods identified in step 4. The NWQL protocols were used to define the MDLs from blanks analyzed outside of the periods identified in step 4. If an MDL defined from blanks was greater than the MDLmax, the MDL defined from blanks was used to censor the data. One constituent had a study reporting limit defined on this basis, and a total of 62 detections in groundwater samples were censored. As of 2019, the USGS NWIS database does not have the capability to store both the original value reported by the NWQL and the final value published by the GAMA-PBP that reflects application of the quality-control censoring described in this report. In the interim, while this capability is developed, the 1,031 results censored in steps 2−5 are blocked from public release in NWIS, and the GAMA-PBP has published the original and final values in a USGS data release accompanying this report. The entire GAMA-PBP final dataset for pesticide constituents on schedules 2003, 2032, or 2033, or on schedule 2060 is publicly available in that USGS data release, through the USGS GAMA-PBP public web portal, and through the California State Water Resources Control Board GAMA public groundwater information system.

California↗

USGS1995

Interlaboratory study of a method for determining nonvolatile organic carbon in aquifer materials

The organic carbon fraction in aquifer materials exerts a major influence on the subsurface mobilities of organic and organic-associated contaminants. The spatial distribution of total organic carbon (TOC) in aquifer materials must be determined before the transport of hydrophobic organic pollutants in aquifers can be modeled accurately. Previous interlaboratory studies showed that it is difficult to measure TOC concentrations <0.1% in aquifer materials, when total inorganic carbon (TIC) concentrations are >1%. We have tested a new analytical method designed to improve the accuracy and precision of nonvolatile TOC quantitation in geologic materials that also contain carbonate minerals. Four authentic aquifer materials and one NIST standard reference material were selected as test materials for a blind collaborative study. Nonvolatile TOC in these materials ranged from 0.05 to 1.4%, while TIC ranged from 0.46 to 12.6%. Sample replicates were digested with sulfurous acid, dried at 40??C, and then combusted at 950??C using LECO or UIC instruments. For the three test materials that contained >2% TIC, incomplete acidification resulted in a systematic positive bias of TOC values reported by five of the six laboratories that used the test method. Participants did not have enough time to become proficient with the new method before they analyzed the test materials. A seventh laboratory successfully used an alternative method that analyzed separate liquid and solid fractions of the acidified sample residues. ?? 1995 Springer-Verlag.

Environmental Geology↗

USGS2003

Stream Bank Stability in Eastern Nebraska

Dredged and straightened channels in eastern Nebraska have experienced degradation leading to channel widening by bank failure. Degradation has progressed headward and affected the drainage systems upstream from the modified reaches. This report describes a study that was undertaken to analyze bank stability at selected sites in eastern Nebraska and develop a simplified method for estimating the stability of banks at future study sites. Bank cross sections along straight reaches of channel and geotechnical data were collected at approximately 150 sites in 26 counties of eastern Nebraska. The sites were categorized into three groups based on mapped soil permeability. With increasing permeability of the soil groups, the median cohesion values decreased and the median friction angles increased. Three analytical methods were used to determine if banks were stable (should not fail even when saturated), at risk (should not fail unless saturated), or unstable (should have already failed). The Culmann and Agricultural Research Service methods were based on the Coulomb equation and planar failure; an indirect method was developed that was based on Bishop's simplified method of slices and rotational failure. The maximum angle from horizontal at which the bank would be stable for the given soil and bank height conditions also was computed with the indirect method. Because of few soil shear-strength data, all analyses were based on the assumption of homogeneous banks, which was later shown to be atypical, at least for some banks. Using the Culmann method and assuming no soil tension cracks, 67 percent of all 908 bank sections were identified as stable, 32 percent were at risk, and 1 percent were unstable; when tension cracks were assumed, the results changed to 58 percent stable, 40 percent at risk, and 1 percent unstable. Using the Agricultural Research Service method, 67 percent of all bank sections were identified as stable and 33 percent were at risk. Using the indirect method, 62 percent of all bank sections were identified as stable and 31 percent were at risk; 3 percent were unstable, and 3 percent were outside of the range of the tables developed for the method. For each of the methods that were used, the largest percentage of stable banks and the smallest percentage of at risk banks was for the soil group with the lowest soil permeability and highest median cohesion values. A comparison of the expected stable bank angles for saturated conditions and the surveyed bank angles indicated that many of the surveyed bank angles were considerably less than the maximum expected stable bank angles despite the banks being classified as at risk or unstable. For severely degraded channels along straight reaches this was not expected. It was expected that they would have angles close to the maximum stable angle as they should have been failing from an oversteepened condition. Several explanations are possible. The channel reaches of some study sites have not yet been affected to a significant degree by degradation; study sites were selected throughout individual basins and severe degradation has not yet extended to some sites along upper reaches; and some reaches have experienced aggradation as degradation progresses upstream. Another possibility is that some bank sections have been affected by lateral migration processes, which typically result in shallow bank angles on the inside bend of the channel. Another possibility is that the maximum expected stable bank angles are too steep. The stability methods used were well established and in essential agreement with each other, and there was no reason to question the geometry data. This left non-representative soil data as a probable reason for computed stable bank angles that, at least in some cases, are overly steep. Based on an examination of the cohesion data, to which the stable bank-angle calculations were most sensitive, both vertical and horizontal variability in soil properti

Water-Resources Investigations Report↗

USGS2017

Evaluation of laser ablation double-focusing SC-ICPMS for “common” lead isotopic measurements in silicate glasses and mineral

An analytical method for the in situ measurement of “common” Pb isotope ratios in silicate glasses and minerals using a 193-nm excimer laser ablation (LA) system with a double-focusing single-collector (SC)-ICPMS is presented and evaluated as a possible alternative to multiple-collector (MC)-ICPMS. This LA-SC-ICPMS technique employs fast-scanning ion deflectors to sequentially place a series of flat-topped isotope peaks into a single ion-counting detector at a fixed accelerating voltage and magnetic field strength. Reference materials (including NIST, MPI-DING, and USGS glasses) are used to identify two analytical artifacts on the Pb isotope ratios (expressed here as heavier/lighter isotopes) when corrected for mass bias relative to NIST SRM610. The first artifact is characterized by anomalously low Pb isotope ratios (~0.1%/AMU) when SRM610 is analyzed in raster mode as an unknown at small spot sizes (<25 µm), which may indicate that (1) SRM610 is isotopically heterogeneous on a small length scale and/or (2) there is a non-spectral matrix effect on the Pb isotope ratios related to differences in spot size. The second artifact is characterized by anomalously high Pb isotope ratios (<0.1%/AMU) for NIST SRM612 (in raster mode) and some Fe-rich glass reference materials (BCR-2G, GOR132-G, and T1-G). These offsets are thought to be caused by one or more non-spectral matrix effects related to differences in the ablation behavior, composition, or physical properties of these reference materials compared to the bracketing SRM610 standard. The precision (±2SD) of our LA-SC-ICPMS Pb isotopic measurements is similar to ( 207 Pb/ 206 Pb and 208 Pb/ 206 Pb, or 20X Pb/ 206 Pb) or better than ( 206 Pb/ 204 Pb, 207 Pb/ 204 Pb, and 208 Pb/ 204 Pb, or 20X Pb/ 204 Pb) a series of published studies that used a different type of SC-ICPMS and obtained a factor of ~3-4 higher sensitivity for Pb. An increase in the sensitivity of our LA-SC-ICPMS would likely improve the precision of the 20X Pb/ 206 Pb and 20X Pb/ 204P b ratios for low-Pb materials (<5 ppm), possibly making the technique broadly similar to LA-MC-ICPMS (particularly compared to methods that rely upon at least one ion-counting detector). Further improvement in the precision of the 20X Pb/ 206 Pb and 20X Pb/ 204 Pb ratios for high-Pb materials (>5 ppm) by LA-SC-ICPMS is unlikely, and in this case, LA-MC-ICPMS remains the preferable analytical technique.

Journal of Analytical Atomic Spectrometry↗

USGS2003

Ground-Water Levels and Water-Quality Data for Wells in the Crumpton Creek Area near Arnold Air Force Base, Tennessee, November 2001 to January 2002

From November 2001 to January 2002, a study of the ground-water resources in the Crumpton Creek area of Middle Tennessee was conducted to determine whether volatile organic compounds (VOCs) from Arnold Air Force Base (AAFB) have affected local private water supplies and to advance understanding of the ground-water-flow system in this area. VOC samples were collected from private wells that were not included in previous sampling efforts conducted in the Crumpton Creek area near AAFB. Ground-water-flow directions were investigated by measuring water levels in wells and constructing a potentiometric-surface map of the Manchester aquifer in the study area. Data were collected from a total of 68 private wells, 82 monitoring wells, and 1 cave during the period of study. Ground-water levels were determined for 42 of the private wells and for all 82 monitoring wells. Of the 82 monitoring wells, 81 withdraw water from the Manchester aquifer and 1 well withdraws water from the overlying shallow aquifer. The Manchester aquifer wells range in depth from 20 to 150 feet. Water-level altitudes for the Manchester aquifer ranged from 956 to 1,064 feet above the National Geodetic Vertical Datum of 1929. Water levels ranged from approximately 6 feet above land surface to 94 feet below land surface. Water-quality samples were collected from all 68 private wells, 8 of the monitoring wells, and the 1 cave. Of the 55 VOCs analyzed, 42 were not detected. Thirteen VOCs were detected; however, only tetrachloroethylene (PCE), methylene chloride, and toluene were detected at concentrations equal to or above reporting levels for the analytical method used. PCE was detected in water samples from 15 private wells and was the only VOC that exceeded drinking water maximum contaminant levels for public water systems. PCE concentrations in samples from five of the wells were below the reporting level and ranged from estimated concentrations of 0.46 to 0.80 microgram per liter (?g/L). Samples from 10 wells contained concentrations equal to or greater than the analytical reporting level of 1 ?g/L for PCE. Samples from one of these wells contained PCE concentrations (12 ?g/L and 11 ?g/L) exceeding the drinking water maximum contaminant level of 5 ?g/L for PCE. The spatial distribution of PCE detections and the relative concentrations of PCE and trichloroethylene suggest that the PCE detections are associated with a small and localized ground-water contamination plume unrelated to AAFB ground-water contamination.

Water-Resources Investigations Report↗

USGS2025

Earth Mapping Resources Initiative protocols—Sampling hard-rock mine waste and perpetual mine water sources

Supporting the overarching goal to evaluate critical minerals nationwide, the mine waste characterization effort in the U.S. Geological Survey (USGS) Earth Mapping Resources Initiative has created a series of protocols to standardize sampling carried out under this effort by the participating State geological surveys and their cooperators. The protocols are based on published, reviewed methods that can be deployed in the field. The protocols include (1) collecting and processing composite samples of mine and mill waste, including tailings, waste rock, gangue, heap leach piles, ore stockpiles, slag, or other mineralized and processed materials and (2) collecting and preserving water samples from perpetual or long-term mine water sources. The protocols also specify information to document on field sheets and detail the collection of geospatial data. The analytical methods used by the USGS and USGS contract laboratories are described in this report, including the data delivery pathway for USGS-derived data.

Scientific Investigations Report↗

USGS2021

Cyprosulfamide: Analysis of the herbicide safener and two of its degradates in surface water and groundwater from the Midwestern United States

Herbicide safeners are commonly included in herbicide formulations to selectively protect crops from herbicide toxicity but are poorly understood in terms of their environmental occurrence and fate. This study established an analytical method for a newer safener, cyprosulfamide, and two of its degradates, cyprosulfamide desmethyl and N -cyclopropyl-4-sulfamoylbenzamide, in water via solid-phase extraction and liquid chromatography with tandem mass spectroscopy. To evaluate the potential for off-field transport and transformation of cyprosulfamide, the method was used to analyze groundwater and surface water samples collected near cornfields in the midwestern United States where cyprosulfamide had been applied. All three compounds were detected in surface water samples ( N = 34); N -cyclopropyl-4-sulfamoylbenzamide was most frequently detected (56%), followed by cyprosulfamide (25%) and cyprosulfamide desmethyl (19%). Maximum concentrations ranged from 22.0 to 5185.9 ng/L, with the highest concentrations and detection rates during the growing season. None of our target analytes were detected in groundwater.

ACS Agricultural Science and Technology↗

USGS2004

The National Geochemical Survey: Database and documentation

The USGS, in collaboration with other federal and state government agencies, industry, and academia, is conducting the National Geochemical Survey (NGS) to produce a body of geochemical data for the United States based primarily on stream sediments, analyzed using a consistent set of methods. These data will compose a complete, national-scale geochemical coverage of the US, and will enable construction of geochemical maps, refine estimates of baseline concentrations of chemical elements in the sampled media, and provide context for a wide variety of studies in the geological and environmental sciences. The goal of the NGS is to analyze at least one stream-sediment sample in every 289 km2 area by a single set of analytical methods across the entire nation, with other solid sample media substituted where necessary. The NGS incorporates geochemical data from a variety of sources, including existing analyses in USGS databases, reanalyses of samples in USGS archives, and analyses of newly collected samples. At the present time, the NGS includes data covering ~71% of the land area of the US, including samples in all 50 states. This version of the online report provides complete access to NGS data, describes the history of the project, the methodology used, and presents preliminary geochemical maps for all analyzed elements. Future editions of this and other related reports will include the results of analysis of variance studies, as well as interpretive products related to the NGS data.

Open-File Report↗