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USGS2013

Mass-balance modeling of mineral weathering rates and CO2 consumption in the forested, metabasaltic Hauver Branch watershed, Catoctin Mountain, Maryland, USA

Mineral weathering rates and a forest macronutrient uptake stoichiometry were determined for the forested, metabasaltic Hauver Branch watershed in north-central Maryland, USA. Previous studies of Hauver Branch have had an insufficient number of analytes to permit determination of rates of all the minerals involved in chemical weathering, including biomass. More equations in the mass-balance matrix were added using existing mineralogic information. The stoichiometry of a deciduous biomass term was determined using multi-year weekly to biweekly stream-water chemistry for a nearby watershed, which drains relatively unreactive quartzite bedrock. At Hauver Branch, calcite hosts ~38 mol% of the calcium ion (Ca 2+ ) contained in weathering minerals, but its weathering provides ~90% of the stream water Ca 2+ . This occurs in a landscape with a regolith residence time of more than several Ka (kiloannum). Previous studies indicate that such old regolith does not typically contain dissolving calcite that affects stream Ca 2+ /Na + ratios. The relatively high calcite dissolution rate likely reflects dissolution of calcite in fractures of the deep critical zone. Of the carbon dioxide (CO 2 ) consumed by mineral weathering, calcite is responsible for approximately 27%, with the silicate weathering consumption rate far exceeding that of the global average. The chemical weathering of mafic terrains in decaying orogens thus may be capable of influencing global geochemical cycles, and therefore, climate, on geological timescales. Based on carbon-balance calculations, atmospheric-derived sulfuric acid is responsible for approximately 22% of the mineral weathering occurring in the watershed. Our results suggest that rising air temperatures, driven by global warming and resulting in higher precipitation, will cause the rate of chemical weathering in the Hauver Branch watershed to increase until a threshold temperature is reached. Beyond the threshold temperature, increased recharge would produce a shallower groundwater table and reduced chemical weathering rates.

Maryland↗

USGS1990

Hydrogeochemistry of rivers and lakes

This chapter has three principal objectives: (1) to summarize the present chemical composition of North American surface waters and point out any discernible trends with time; (2) to review chemical and biochemical principles and processes that control natural water composition, and the ways in which these may be involved in attaining the particular chemical compositions and trends that we can observe; and (3) to point out some of the more important factors that must be considered in collecting surface-water-quality data. This discussion is concerned principally with inorganic chemistry and geochemistry. However, biochemical processes in river and lake water influence their chemical composition extensively, and specific effects are pointed out. Aquatic biology is discussed in another chapter. The physical processes occurring in lakes also have very important effects on water chemistry; these aspects of limnology are covered more fully in a separate chapter. Data on which this chapter is based relate mostly to waters of Canada, the United States, and Mexico. For most of Central America, very little water-quality information is available. Tables 1 through 3 contain analytical data for river waters that illustrate some of the principles discussed, and summarize major features of the chemical composition of North American surface waters. To a certain extent, at least, one would expect the average concentrations of dissolved elements in surface fresh water to reflect the relative abundance of the elements in the crustal rocks exposed at and near the land surface.

Book chapter↗

USGS1980

United States Geological Survey Yearbook, fiscal year 1979

In March 1979, the U.S. Geological Survey celebrated its 100th year of service to the Nation and 10 decades of stewardship of the land and its resources. During this year, as in the previous 99, the Survey discharged its national trust by collecting, analyzing, and disseminating earth science information and by continuing its somewhat more recent responsibilities of supervising the development of energy and mineral resources on Federal lands. The basic mission of the Survey has changed over the years, and the scope of its activities and the power of analytic tools have also increased by several orders of magnitude from the early surveys of then "remote" western areas of the United States to surveying and mapping the mountains of the Moon and the polar caps of Mars and from the use of surveyor's transits, picks, the travelling chemistry kits to interpretation of Earth imagery. These representative advances illustrate important and continuing trends for at no previous time have our earth resources been so precious or our consciousness of their finiteness so acute. The Yearbook reports a broad range of the Survey's accomplishments during the past fiscal year and offers an overview of its future. Many of the topics touched on below will continue to be important resource issues in the coming decade.

Yearbook↗

USGS2005

External quality-assurance results for the National Atmospheric Deposition Program/National Trends Network, 2002-03

Six external quality-assurance programs were operated by the U.S. Geological Survey (USGS) External Quality-Assurance (QA) Project for the National Atmospheric Deposition Program/National Trends Network (NADP/NTN) from 2002 through 2003. Each program measured specific components of the overall error inherent in NADP/NTN wet-deposition measurements. The intersite-comparison program assessed the variability and bias of pH and specific conductance determinations made by NADP/NTN site operators twice per year with respect to accuracy goals. The percentage of site operators that met the pH accuracy goals decreased from 92.0 percent in spring 2002 to 86.3 percent in spring 2003. In these same four intersite-comparison studies, the percentage of site operators that met the accuracy goals for specific conductance ranged from 94.4 to 97.5 percent. The blind-audit program and the sample-handling evaluation (SHE) program evaluated the effects of routine sample handling, processing, and shipping on the chemistry of weekly NADP/NTN samples. The blind-audit program data indicated that the variability introduced by sample handling might be environmentally significant to data users for sodium, potassium, chloride, and hydrogen ion concentrations during 2002. In 2003, the blind-audit program was modified and replaced by the SHE program. The SHE program was designed to control the effects of laboratory-analysis variability. The 2003 SHE data had less overall variability than the 2002 blind-audit data. The SHE data indicated that sample handling buffers the pH of the precipitation samples and, in turn, results in slightly lower conductivity. Otherwise, the SHE data provided error estimates that were not environmentally significant to data users. The field-audit program was designed to evaluate the effects of onsite exposure, sample handling, and shipping on the chemistry of NADP/NTN precipitation samples. Field-audit results indicated that exposure of NADP/NTN wet-deposition samples to onsite conditions tended to neutralize the acidity of the samples by less than 1.0 microequivalent per liter. Onsite exposure of the sampling bucket appeared to slightly increase the concentration of most of the analytes but not to an extent that was environmentally significant to NADP data users. An interlaboratory-comparison program was used to estimate the analytical variability and bias of the NADP Central Analytical Laboratory (CAL) during 2002-03. Bias was identified in the CAL data for calcium, magnesium, sodium, potassium, ammonium, chloride, nitrate, sulfate, hydrogen ion, and specific conductance, but the absolute value of the bias was less than analytical minimum detection limits for all constituents except magnesium, nitrate, sulfate, and specific conductance. Control charts showed that CAL results were within statistical control approximately 90 percent of the time. Data for the analysis of ultrapure deionized-water samples indicated that CAL did not have problems with laboratory contamination. During 2002-03, the overall variability of data from the NADP/NTN precipitation-monitoring system was estimated using data from three collocated monitoring sites. Measurement differences of constituent concentration and deposition for paired samples from the collocated samplers were evaluated to compute error terms. The medians of the absolute percentage errors (MAEs) for the paired samples generally were larger for cations (approximately 8 to 50 percent) than for anions (approximately 3 to 33 percent). MAEs were approximately 16 to 30 percent for hydrogen-ion concentration, less than 10 percent for specific conductance, less than 5 percent for sample volume, and less than 8 percent for precipitation depth. The variability attributed to each component of the sample-collection and analysis processes, as estimated by USGS quality-assurance programs, varied among analytes. Laboratory analysis variability accounted for approximately 2 percent of the

Scientific Investigations Report↗

USGS2002

Rodent repellents, correlation between chemical structure and rodent repellency of benzoic acid derivatives

Sixty-five benzoic acid derivatives were either prepared or obtained from commercial concerns, tested for rat repellency, and their indices of repellency computed. The data from these tests were considered analytically for any correlation between chemical structure and rat repellency. The results suggest a qualitative relationship which is useful in deciding probability of repellency in other compounds.

Journal of Agricultural and Food Chemistry↗

USGS2023

Assessing contaminants of emerging concern in the Great Lakes Ecosystem: A decade of method development and practical application

Assessing the ecological risk of contaminants in the field typically involves consideration of a complex mixture of compounds which may or may not be detected via instrumental analyses. Further, there are insufficient data to predict the potential biological effects of many detected compounds, leading to their being characterized as contaminants of emerging concern (CECs). Over the past several years, advances in chemistry, toxicology, and bioinformatics have resulted in a variety of concepts and tools that can enhance the pragmatic assessment of the ecological risk of CECs. The present Focus article describes a 10+- year multiagency effort supported through the U.S. Great Lakes Restoration Initiative to assess the occurrence and implications of CECs in the North American Great Lakes. State-of-the-science methods and models were used to evaluate more than 700 sites in about approximately 200 tributaries across lakes Ontario, Erie, Huron, Michigan, and Superior, sometimes on multiple occasions. Studies featured measurement of up to 500 different target analytes in different environmental matrices, coupled with evaluation of biological effects in resident species, animals from in situ and laboratory exposures, and in vitro systems. Experimental taxa included birds, fish, and a variety of invertebrates, and measured endpoints ranged from molecular to apical responses. Data were integrated and evaluated using a diversity of curated knowledgebases and models with the goal of producing actionable insights for risk assessors and managers charged with evaluating and mitigating the effects of CECs in the Great Lakes. This overview is based on research and data captured in approximately about 90 peer-reviewed journal articles and reports, including approximately about 30 appearing in a virtual issue comprised of highlighted papers published in Environmental Toxicology and Chemistry or Integrated Environmental Assessment and Management . Environ Toxicol Chem 2023;42:2506–2518. © 2023 SETAC. This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA.

Environmental Toxicology and Chemistry↗

USGS2004

Herbicides and their transformation products in source-water aquifers tapped by public-supply wells in Illinois, 2001-02

During 2001-02, ground-water samples were collected from 117 public-supply wells distributed throughout Illinois to evaluate the occurrence of herbicides and their transformation products in the State?s source-water aquifers. Wells were selected using a stratified-random method to ensure representation of the major types of source-water aquifers in the State. Samples were analyzed for 18 herbicides and 18 transformation products, including 3 triazine and 14 chloroacetanilide products. Herbicide compounds (field-applied parent herbicides and their transformation products) were detected in 34 percent of samples. A subset of samples was collected unfiltered to determine if analytical results for herbicides in unfiltered samples are similar to those in paired filtered samples and, thus, can be considered equally representative of herbicide concentrations in ground water supplied to the public. The study by the U.S. Geological Survey was done in cooperation with the Illinois Environmental Protection Agency. Parent herbicides were detected in only 4 percent of all samples. The six most frequently detected herbicide compounds (from 5 to 28 percent of samples) were chloroacetanilide transformation products. The frequent occurrence of transformation products and their higher concentrations relative to those of most parent herbicides confirm the importance of obtaining information on transformation products to understand the mobility and fate of herbicides in ground-water systems. No sample concentrations determined during this study exceeded current (2003) Federal or State drinking-water standards; however, standards are established for only seven parent herbicides. Factors related to the occurrence of herbicide compounds in the State?s source-water aquifers include unconsolidated and unconfined conditions, various hydrogeologic characteristics and well-construction aspects at shallow depths, and proximity to streams. Generally, the closer an aquifer (or well location) is to a recharge area and (or) the stronger the hydraulic connection between an aquifer and a recharge area, the younger the ground water and the more vulnerable the aquifer will be to contamination by herbicide compounds. The weak relation between current (2001) statewide application rates of herbicides and current (2001-02) occurrence of herbicide compounds in source-water aquifers indicates that additional factors must be considered when relating herbicide-application rates to occurrence. These factors include historical application rates and the mobility and persistence of the various herbicide compounds in ground-water systems. Frequency of detection and concentrations of herbicides compounds in the State?s source-water aquifers are indicated to be highest during the spring, when crops are planted and herbicides primarily are applied. Excess nitrate (concentrations of nitrate, as nitrogen, higher than 3 milligrams per liter) in ground water strongly indicates the co-occurrence of herbicide compounds. However, nitrate concentrations are not a reliable indicator of herbicide-compound concentrations. The inverse relation found between current use of land for corn and soybean production and current occurrence of herbicide compounds in underlying aquifers indicates that various factors, along with current agricultural land use, contribute to herbicide occurrence. These factors include, among others, land-use history, ground-water age, ground-water-flow patterns, geology, soil microbiology, and chemistry and persistence of the herbicide compounds. Detection of agriculture-specific herbicide compounds in 71 percent of samples from urban areas with no current or recent agricultural land use near the sampled wells indicates that recharge to certain high-capacity supply wells may originate at considerable distances (up to about 10 miles) from the wells. Essentially no difference was found between the analytical results for herbicides in paired unfiltered and filtered samples,

Water-Resources Investigations Report↗

USGS2018

External quality assurance project report for the National Atmospheric Deposition Program’s National Trends Network and Mercury Deposition Network, 2015–16

The U.S. Geological Survey Precipitation Chemistry Quality Assurance project operated five distinct programs to provide external quality assurance monitoring for the National Atmospheric Deposition Program’s (NADP) National Trends Network and Mercury Deposition Network during 2015–16. The National Trends Network programs include (1) a field audit program to evaluate sample contamination and stability, (2) an interlaboratory comparison program to evaluate analytical laboratory performance, and (3) a colocated sampler program to evaluate bias and variability attributed to automated precipitation samplers. The Mercury Deposition Network programs include the (4) system blank program and (5) an interlaboratory comparison program. The results indicate that NADP data continue to be of sufficient quality for the analysis of spatial distributions and time trends for chemical constituents in wet deposition. The field audit program results indicate increased sample contamination for calcium, magnesium, and potassium relative to 2010 levels, and slight fluctuation in sodium contamination. Nitrate contamination levels dropped slightly during 2014–16, and chloride contamination leveled off between 2007 and 2016. Sulfate contamination is similar to the 2000 level. Hydrogen ion contamination has steadily decreased since 2012. Losses of ammonium and nitrate resulting from potential sample instability were negligible. The NADP Central Analytical Laboratory produced interlaboratory comparison results with low bias and variability compared to other domestic and international laboratories that support atmospheric deposition monitoring. Significant absolute bias above the magnitudes of the detection limits was observed for nitrate and sulfate concentrations, but no analyte determinations exceeded the detection limits for blanks. Colocated sampler program results from dissimilar colocated collectors indicate that the retrofit of the National Trends Network with N-CON Systems Company, Inc. precipitation collectors could cause substantial shifts in NADP annual deposition (concentration multiplied by depth) values. Median weekly relative percent differences for analyte concentrations ranged from -4 to +76 percent for cations, from 5 to 6 percent for ammonium, from +14 to +25 percent for anions, and from -21 to +8 percent for hydrogen ion contamination. By comparison, weekly absolute concentration differences for paired identical N-CON Systems Company, Inc., collectors ranged from 4–22 percent for cations; 2–9 percent for anions; 4–5 percent for ammonium; and 13–14 percent for hydrogen ion contamination. The N-CON Systems Company, Inc. collector caught more precipitation than the Aerochem Metrics Model 301 collector (ACM) at the WA99/99WA sites, but it typically caught slightly less precipitation than the ACM at ND11/11ND, sites which receive more wind and snow than WA99/99WA. Paired, identical OTT Pluvio-2 and ETI Noah IV precipitation gages were operated at the same sites. Median absolute percent differences for daily measured precipitation depths ranged from 0 to 7 percent. Annual absolute differences ranged from 0.08 percent (ETI Noah IV precipitation gages) to 11 percent (OTT Pluvio-2 precipitation gages). The Mercury Deposition Network programs include the system blank program and an interlaboratory comparison program. System blank results indicate that maximum total mercury contamination concentrations in samples were less than the third percentile of all Mercury Deposition Network sample concentrations (1.098 nanograms per liter; ng/L). The Mercury Analytical Laboratory produced chemical concentration results with low bias and variability compared with other domestic and international laboratories that support atmospheric-deposition monitoring. The laboratory’s performance results indicate a +1-ng/L shift in bias between 2015 (-0.4 ng/L) and 2016 (+0.5 ng/L).

Scientific Investigations Report↗

USGS2011

The Alaska Geochemical Database: v. 1.0 - Geologic Materials

What is the AGDB?: The Alaska Geochemical Database (AGDB) is a new, comprehensive compilation of geologic, spatial, descriptive, mineralogical, and analytical geochemical data for samples collected in Alaska and surrounding waters by the U.S. Geological Survey (USGS) from 1962 to 2009. Data for geologic materials (rocks, minerals and mineral separates, soils, lake sediments, bulk stream sediments, and a variety of heavy-mineral concentrates) will be released as a two-sided DVD (USGS Digital Data Series DS 637 v. 1.0) in October of 2011. Future data releases will include water, organic and leachate samples. The AGDB contains all Alaskan data from USGS legacy databases (for example, the RASS and PLUTO systems), and all results produced by USGS in-house and contract chemistry laboratories through December 2009. The database includes geochemical data resulting from the reanalysis of archived materials, such as those from the Alaska Mineral Resource Assessment (AMRAP) and National Uranium Resource Evaluation (NURE) programs, for additional elements and by newer methods. Reanalyses include samples collected statewide as part of the National Geochemical Survey, and samples from a project across the Alaska Range (data released in 2010). The AGDB also contains data for geologic materials from Alaska submitted by USGS researchers to non-USGS and non-contract labs, and a variety of other Alaskan geologic materials samples. Quality Control: Data in the AGDB have undergone extensive quality control screening including searching field notes and maps for accurate location information, verifying media and sample type, linking analytical data to geologic parameters recorded by the submitter, and documenting sample preparation and analytical methods. Data Files The AGDB v. 1.0 two-sided DVD includes: * a 4.3 GB Microsoft Access® 2007 relational database (as two linked .mdb files); * the same database in Microsoft Access® 2003; * Microsoft Excel® spreadsheet tables (.xls files) and ASCII text files that display the results of common queries to the database (for example, Ag-Cr values for concentrate samples; rock samples by quadrangle); * references for analytical methods; * references to published data; and * metadata in three file formats. Data Availability: * The Alaska Geochemical Database will be available in a searchable, spatially referenced, online format at http://mrdata.usgs.gov/; estimated availability early 2012. * A 2012 update (AGDB v. 2.0) will include water, organic, leachate, and miscellaneous sample media. For More Information: On sample media or analytical methods: http://minerals.cr.usgs.gov/projects/analytical_chem/references.html Text prepared by Jeanine M. Schmidt and Matt Granitto Figure prepared by Nora Shew; Layout by Jeanine Schmidt Artwork on page 1 by Daniel Granitto (used by permission) The USGS Mineral Resources Program is the sole Federal provider of research and information on nonfuel mineral resources.

Fact Sheet↗

USGS2024

Evaluating the reliability of environmental concentration data to characterize exposure in environmental risk assessments

Environmental risk assessments often rely on measured concentrations in environmental matrices to characterize exposure of the population of interest—typically, humans, aquatic biota, or other wildlife. Yet, there is limited guidance available on how to report and evaluate exposure datasets for reliability and relevance, despite their importance to regulatory decision-making. This paper is the second of a four-paper series detailing the outcomes of a Society of Environmental Toxicology and Chemistry Technical Workshop that has developed Criteria for Reporting and Evaluating Exposure Datasets (CREED). It presents specific criteria to systematically evaluate the reliability of environmental exposure datasets. These criteria can help risk assessors understand and characterize uncertainties when existing data are used in various types of assessments and can serve as guidance on best practice for the reporting of data for data generators (to maximize utility of their datasets). Although most reliability criteria are universal, some practices may need to be evaluated considering the purpose of the assessment. Reliability refers to the inherent quality of the dataset and evaluation criteria address the identification of analytes, study sites, environmental matrices, sampling dates, sample collection methods, analytical method performance, data handling or aggregation, treatment of censored data, and generation of summary statistics. Each criterion is evaluated as “fully met,” “partly met,” “not met or inappropriate,” “not reported,” or “not applicable” for the dataset being reviewed. The evaluation concludes with a scheme for scoring the dataset as reliable with or without restrictions, not reliable, or not assignable, and is demonstrated with three case studies representing both organic and inorganic constituents, and different study designs and assessment purposes. Reliability evaluation can be used in conjunction with relevance evaluation (assessed separately) to determine the extent to which environmental monitoring datasets are “fit for purpose,” that is, suitable for use in various types of assessments. Integr Environ Assess Manag 2024;00:1–23. © 2024 Society of Environmental Toxicology & Chemistry (SETAC). This article has been contributed to by U.S. Government employees and their work is in the public domain in the USA.

Integrated Environmental Assessment and Management↗

USGS2003

External quality-assurance results for the National Atmospheric Deposition Program/National Trends Network, 1997-99

Five external quality-assurance programs were operated by the U.S. Geological Survey for the National Atmospheric Deposition Program/ National Trends Network (NADP/NTN) during 1997 through 1999: the intersite-comparison program, the blind-audit program, the field- audit program, the interlaboratory-comparison program, and the collocated-sampler program. The intersite-comparison program assesses the accuracy of pH and specific-conductance determinations made by NADP/NTN site operators. In two 1997 intersite-comparison studies, 83.7 and 85.8 percent of the pH determinations met the NADP/NTN accuracy goals, whereas 97.3 and 92.4 percent of the specific-conductance determinations met the NADP/NTN accuracy goals. The percentage of pH and specific-conductance determinations that met the accuracy goals in 1998 were, for the most part, higher than in 1997. In two 1998 studies, 90.9 and 90.3 percent of the pH determinations met the accuracy goals compared to 94.7 and 96.0 percent of the specific- conductance measurements meeting the accuracy goals. In one 1999 intersite-comparison study, 89.5 percent and 99.4 percent of pH and specific- conductance determinations, respectively, met the NADP/NTN accuracy goals. The blind-audit program evaluates the effects of routine sample handling, processing, and shipping on the analytical bias and precision of weekly precipitation samples. A portion of the blind-audit sample subject to the normal onsite handling and processing of a weekly precipitation sample is referred to as the bucket portion, whereas the portion receiving only minimal handling is referred to as the bottle portion. Positive bias in regard to blind-audit results indicates that the bucket portion has a higher concentration than the bottle portion. The paired t-test for the 1997 through 1999 blind- audit data indicates that routine sample handling, processing, and shipping introduced a positive bias (a=0.05) for calcium and chloride and a negative bias (cz=0.05) for hydrogen ion. During 1997 through 1999, the median paired differences between the bucket and bottle portions ranged from 0.00 milligram per liter for nitrate and ammonium to +0.010 milligram per liter for both chloride and sulfate. The median paired difference between the bucket and bottle portions for hydrogen ion was -1.086 microequivalents per liter, whereas for specific conductance, the median paired difference between the bucket and bottle portions was -0.200 microsiemen per centimeter during 1997 through 1999. Surface-chemistry effects due to variable amounts of precipitation contacting prewashed sample-collection and shipping-container surfaces were studied in the blind-audit program by using three different sample volumes. The sample- collection and shipping containers used for the blind-audit study were obtained from the site operator's supply and could have been used for precipitation samples. Results of a Kruskal-Wallis analysis of variance test of the relation between paired blind-audit sample differences in units of concentration and sample volume were statistically significant for magnesium, chloride, sulfate, and hydrogen ion during 1997 through 1999. Before 1994, at least 5 of the 10 analytes displayed a statistically significant difference between paired blind-audit differences in units of concentration and sample volume, supporting the premise that chemical reactions between the 13-liter bucket shipping container (primarily the butadiene o-ring lid of the shipping container) and the sample, which resulted in an increasing loss of hydrogen ion with increasing volume, have been eliminated by the new l-liter bottle sample- shipping protocol. The field-audit program measures the effects of field exposure, handling, and processing on the chemistry of NADP/NTN precipitation samples. In the field-audit program, the site operator is instructed to process and submit a quality- control sample following a standard 7-day, Tuesday-to-Tuesday sampling period with no

Water-Resources Investigations Report↗

USGS2020

External quality assurance project report for the National Atmospheric Deposition Program’s National Trends Network and Mercury Deposition Network, 2017–18

The U.S. Geological Survey (USGS) Precipitation Chemistry Quality Assurance project (PCQA) operated five distinct programs to provide external quality-assurance monitoring for the National Atmospheric Deposition Program’s (NADP) National Trends Network and Mercury Deposition Network during 2017–18. The National Trends Network programs included (1) a field audit program to evaluate sample contamination and stability, (2) an interlaboratory comparison program to evaluate analytical laboratory performance, and (3) a colocated sampler program to evaluate variability attributed to automated precipitation samplers. The Mercury Deposition Network programs include the (4) system blank program and (5) an interlaboratory comparison program. The results indicate consistently low levels of sample contamination, generally strong analytical laboratory performance, and low overall variability in concentration data imparted by field equipment. The NADP operations moved from its 40-year home at the Illinois State Water Survey to the Wisconsin State Laboratory of Hygiene in June 2018. The PCQA programs were modified and (or) temporarily curtailed during the transition in 2018. Bias and variability of sample analysis results were evaluated for the two Central Analytical Laboratories, and ongoing monitoring will be helpful to differentiate true environmental signals from the effects of changing laboratory conditions and performance. Results of quality assurance sample analyses are provided to document that NADP data continue to be of sufficient quality for the analysis of spatial distributions and time trends for chemical constituents in wet deposition.

Scientific Investigations Report↗

USGS2024

External quality-assurance project report for the National Atmospheric Deposition Program National Trends Network and Mercury Deposition Network, 2021–22

The U.S. Geological Survey Precipitation Chemistry Quality Assurance project (PCQA) operated five distinct programs to provide external quality-assurance monitoring for the National Atmospheric Deposition Program (NADP) National Trends Network (NTN) and Mercury Deposition Network (MDN) during 2021–22. The NTN programs included (1) a field audit program to evaluate sample contamination and stability, (2) an interlaboratory-comparison program to evaluate analytical laboratory performance, and (3) a colocated sampler program to estimate overall variability of NTN wet-deposition measurements, and the MDN programs included the (4) system blank program to evaluate sample contamination and stability and (5) an interlaboratory-comparison program. The results indicated increased levels of sample contamination compared to previous years for NTN samples and decreased contamination in MDN samples. Strong analytical laboratory performance with low overall variability and bias in concentration data was indicated for the NTN Central Analytical Laboratory. Slight perturbations in contamination levels in NTN samples and in analytical performance for MDN are considered inconsequential. The colocated sampler program results indicated overall variability in NTN data to range from 0 to 30.3 percent for cations, 1.6 to 11.4 percent for ammonium, 0.8 to 20.2 percent for anions, 10.3 to 17.2 percent for hydrogen-ion concentration, and 1.5 to 12.2 percent for specific conductance. The PCQA results indicate that NADP data continue to be of sufficient quality for applications in independent research and NADP data products, including spatial interpolations and time trends for chemical constituents in wet deposition. Small shifts in data quality indicated by the 2021–22 PCQA results are included to be used for interpretation of the NADP data products.

Scientific Investigations Report↗

USGS1993

Application of mixed-mode, solid-phase extraction in environmental and clinical chemistry. Combining hydrogen-bonding, cation-exchange and Van der Waals interactions

Silica- and styrene-divinylbenzene-based mixed-mode resins that contain C8, C18 and sulphonated cation-exchange groups were compared for their efficiency in isolation of neutral triazine compounds from water and of the basic drug, benzoylecgonine, from urine. The triazine compounds were isolated by a combination of Van der Waals and hydrogen-bonding interactions, and benzoylecgonine was isolated by Van der Waals interactions and cation exchange. All analytes were eluted with a polar organic solvent contaning 2% ammonium hydroxide. Larger recoveries (95%) were achieved on copolymerized mixed-mode resins where C18 and sulfonic acid are in closer proximity than on 'blended' mixed-mode resins (60-70% recovery).

Journal of Chromatography A↗

USGS2023

External quality-assurance project report for the National Atmospheric Deposition Program’s National Trends Network and Mercury Deposition Network, 2019–20

The U.S. Geological Survey Precipitation Chemistry Quality Assurance project (PCQA) operated four distinct programs to provide external quality-assurance monitoring for the National Atmospheric Deposition Program’s (NADP) National Trends Network (NTN) and Mercury Deposition Network (MDN) during 2019–20. The NTN programs included (1) a field audit program to evaluate sample contamination and stability, and (2) an interlaboratory comparison program to evaluate analytical laboratory performance. The MDN programs included the (3) system blank program to evaluate sample contamination and stability, and (4) an interlaboratory comparison program. The results indicated increased levels of sample contamination compared to previous years for NTN samples and decreased contamination in MDN samples. Strong analytical laboratory performance with low overall variability and bias in concentration data were indicated for the NTN’s Central Analytical Laboratory. A positive bias in the hydrogen ion concentrations in NTN samples during 2019 was eliminated by correction of a pH calibration protocol during 2020. The MDN’s Mercury Analytical Laboratory performance declined in 2020 compared to 2019 as indicated by increased variability in analytical results and a negative bias of approximately -1 nanogram per liter in the concentrations of total mercury. Slight perturbations in contamination levels in NTN samples and in analytical performance for MDN are considered small. The PCQA results indicate that NADP data continue to be of sufficient quality for applications in independent research and NADP data products, including spatial interpolations and time trends for chemical constituents in wet deposition. Small shifts in data quality indicated by the 2019–20 PCQA results are intended to be used for interpretation of the NADP data products.

Scientific Investigations Report↗

USGS2021

Evaluation and application of the Purge Analyzer Tool (PAT) to determine in-well flow and purge criteria for sampling monitoring wells at the Stringfellow Superfund site in Jurupa Valley, California, in 2017

The U.S. Geological Survey and U.S. Environmental Protection Agency are developing analytical tools to assess the representativeness of groundwater samples from fractured-rock aquifers. As part of this effort, monitoring wells from the Stringfellow Superfund site in Jurupa Valley in Riverside County, California, approximately 50 miles east of Los Angeles, were field tested to collect information to assist in the evaluation and application of in-well flow as computed by the analytical model called the Purge Analyzer Tool, which computes in-well groundwater travel times for simple piston transport of inflowing groundwater from open intervals of a monitoring well to the pump intake and can provide insight into optimal purging parameters (duration, rate, and pump position) needed for the collection of representative groundwater samples. Field testing of wells included hydraulic, chemistry, and dye tracer analysis to investigate travel times in wells under pumping conditions. The Purge Analyzer Tool was able to replicate dye velocities (travel times) for one of three wells that had appreciable inflow from the aquifer but not the other two wells, which are screened in low-permeability sediments and rock, where flow was dominated by borehole storage. A set of criteria was established to help assess the ability to collect representative groundwater chemistry from monitoring wells; criteria included understanding the height of the static well water column and relative exchange rate between the aquifer and the well.

California↗

USGS2010

Nonparametric statistical methods for comparing two sites based on data with multiple nondetect limits

As concern over the effects of trace amounts of pollutants has increased, so has the need for statistical methods that deal appropriately with data that include values reported as “less than” the detection limit. It has become increasingly common for water quality data to include censored values that reflect more than one detection limit for a single analyte. For such multiply censored data sets, standard statistical methods (for example, to compare analyte concentration in two areas) are not valid. In such cases, methods from the biostatistical field of survival analysis are applicable. Several common two‐sample censored data rank tests are explained, and their behaviors are studied via a Monte Carlo simulation in which sample sizes and censoring mechanisms are varied under an assumed lognormal distribution. These tests are applied to shallow groundwater chemistry data from two sites in the San Joaquin Valley, California. The best overall test, in terms of maintained α level, is the normal scores test based on a permutation variance. In cases where the α level is maintained, however, the Peto‐Prentice statistic based on an asymptotic variance performs as well or better.

California↗

USGS2002

Compilation of minimum and maximum isotope ratios of selected elements in naturally occurring terrestrial materials and reagents

Documented variations in the isotopic compositions of some chemical elements are responsible for expanded uncertainties in the standard atomic weights published by the Commission on Atomic Weights and Isotopic Abundances of the International Union of Pure and Applied Chemistry. This report summarizes reported variations in the isotopic compositions of 20 elements that are due to physical and chemical fractionation processes (not due to radioactive decay) and their effects on the standard atomic weight uncertainties. For 11 of those elements (hydrogen, lithium, boron, carbon, nitrogen, oxygen, silicon, sulfur, chlorine, copper, and selenium), standard atomic weight uncertainties have been assigned values that are substantially larger than analytical uncertainties because of common isotope abundance variations in materials of natural terrestrial origin. For 2 elements (chromium and thallium), recently reported isotope abundance variations potentially are large enough to result in future expansion of their atomic weight uncertainties. For 7 elements (magnesium, calcium, iron, zinc, molybdenum, palladium, and tellurium), documented isotope-abundance variations in materials of natural terrestrial origin are too small to have a significant effect on their standard atomic weight uncertainties. This compilation indicates the extent to which the atomic weight of an element in a given material may differ from the standard atomic weight of the element. For most elements given above, data are graphically illustrated by a diagram in which the materials are specified in the ordinate and the compositional ranges are plotted along the abscissa in scales of (1) atomic weight, (2) mole fraction of a selected isotope, and (3) delta value of a selected isotope ratio. There are no internationally distributed isotopic reference materials for the elements zinc, selenium, molybdenum, palladium, and tellurium. Preparation of such materials will help to make isotope ratio measurements among laboratories comparable. The minimum and maximum concentrations of a selected isotope in naturally occurring terrestrial materials for selected chemical elements reviewed in this report are given below: Isotope Minimum mole fraction Maximum mole fraction -------------------------------------------------------------------------------- 2H 0 .000 0255 0 .000 1838 7Li 0 .9227 0 .9278 11B 0 .7961 0 .8107 13C 0 .009 629 0 .011 466 15N 0 .003 462 0 .004 210 18O 0 .001 875 0 .002 218 26Mg 0 .1099 0 .1103 30Si 0 .030 816 0 .031 023 34S 0 .0398 0 .0473 37Cl 0 .240 77 0 .243 56 44Ca 0 .020 82 0 .020 92 53Cr 0 .095 01 0 .095 53 56Fe 0 .917 42 0 .917 60 65Cu 0 .3066 0 .3102 205Tl 0 .704 72 0 .705 06 The numerical values above have uncertainties that depend upon the uncertainties of the determinations of the absolute isotope-abundance variations of reference materials of the elements. Because reference materials used for absolute isotope-abundance measurements have not been included in relative isotope abundance investigations of zinc, selenium, molybdenum, palladium, and tellurium, ranges in isotopic composition are not listed for these elements, although such ranges may be measurable with state-of-the-art mass spectrometry. This report is available at the url: http://pubs.water.usgs.gov/wri014222.

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