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At least 235 records · Page 13Linked to original sources

Quality-assurance results for routine water analysis in US Geological Survey laboratories, water year 1991

The US. Geological Survey operates a quality- assurance program based on the analyses of reference samples for the National Water Quality Laboratory in Arvada, Colorado, and the Quality of Water Service Unit in Ocala, Florida. Reference samples containing selected inorganic, nutrient, and low ionic-strength constituents are prepared and disguised as routine samples. The program goal is to determine precision and bias for as many analytical methods offered by the participating laboratories as possible. The samples typically are submitted at a rate of approximately 5 percent of the annual environmental sample load for each constituent. The samples are distributed to the laboratories throughout the year. Analytical data for these reference samples reflect the quality of environmental sample data produced by the laboratories because the samples are processed in the same manner for all steps from sample login through data release. The results are stored permanently in the National Water Data Storage and Retrieval System. During water year 1991, 86 analytical procedures were evaluated at the National Water Quality Laboratory and 37 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic (major ion and trace metal) constituent data for water year 1991 indicated analytical imprecision in the National Water Quality Laboratory for 5 of 67 analytical procedures: aluminum (whole-water recoverable, atomic emission spectrometric, direct-current plasma); calcium (atomic emission spectrometric, direct); fluoride (ion-exchange chromatographic); iron (whole-water recoverable, atomic absorption spectrometric, direct); and sulfate (ion-exchange chromatographic). The results for 11 of 67 analytical procedures had positive or negative bias during water year 1991. Analytical imprecision was indicated in the determination of two of the five National Water Quality Laboratory nutrient constituents: orthophosphate as phosphorus and phosphorus. A negative or positive bias condition was indicated in three of five nutrient constituents. There was acceptable precision and no indication of bias for the 14 low ionic-strength analytical procedures tested in the National Water Quality Laboratory program and for the 32 inorganic and 5 nutrient analytical procedures tested in the Quality of Water Service Unit during water year 1991.

Water-Resources Investigations Report↗

Steroid determination in fish plasma using capillary electrophoresis

A capillary separation method that incorporates pH-mediated stacking is employed for the simultaneous determination of circulating steroid hormones in plasma from Perca flavescens (yellow perch) collected from natural aquatic environments. The method can be applied to separate eight steroid standards: progesterone, 17α,20β-dihydroxypregn-4-en-3-one, 17α-hydroxyprogesterone, testosterone, estrone, 11-ketotestosterone, ethynyl estradiol, and 17β-estradiol. Based on screening of plasma, the performance of the analytical method was determined for 17α,20β-dihydroxypregn-4-en-3-one, testosterone, 11-ketotestosterone, and 17β-estradiol. The within-day reproducibility in migration time for these four steroids in aqueous samples was ≤2%. Steroid quantification was accomplished using a calibration curve obtained with external standards. Plasma samples from fish collected from the Choptank and Severn Rivers, Maryland, USA, stored for up to one year were extracted with ethyl acetate and then further processed with anion exchange and hydrophobic solid phase extraction cartridges. The recovery of testosterone and 17β-estradiol from yellow perch plasma was 84 and 85%, respectively. Endogenous levels of testosterone ranged from 0.9 to 44 ng/ml, and when detected 17α,20β-dihydroxypregn-4-en-3-one ranged from 5 to 34 ng/ml. The reported values for testosterone correlated well with the immunoassay technique. Endogenous concentrations of 17β-estradiol were ≤1.7 ng/ml. 11-Ketotestosterone was not quantified because of a suspected interferant. Higher levels of 17α,20β-dihydroxypregn-4-en-3-one were found in male and female fish in which 17β-estradiol was not detected. Monitoring multiple steroids can provide insight into hormonal fluctuations in fish.

Maryland↗

Strategic Plan for the North American Breeding Bird Survey: 2006-2010

Executive Summary The mission of the North American Breeding Bird Survey (BBS) is to provide scientifically credible measures of the status and trends of North American bird populations at continental and regional scales to inform biologically sound conservation and management actions. Determining population trends, relative abundance, and distributions of North American avifauna is critical for identifying conservation priorities, determining appropriate conservation actions, and evaluating those actions. The BBS program, jointly coordinated by the U.S. Geological Survey and Environment Canada’s Canadian Wildlife Service, provides the U.S. and Canadian Federal governments, state and provincial agencies, other conservation practitioners, and the general public with science-based avian population trend estimates and other information for regional and national species’ population assessments. Despite the demonstrated value of the BBS for furthering avian conservation across North America, its importance is often underappreciated, and it is underfunded compared with many other government-supported programs that report on status of the environment. Today, BBS resources, adjusted for inflation, are below the amount allocated in the 1970s and are still only sufficient to support two biologists. Yet the number of routes, participants, data, and data requests has quadrupled. Data and information management and delivery requirements and security concerns, non-existent in 1966, impose further demands on BBS resources. In addition, the Mexican expansion of the BBS offers new hope for a truly continental approach to avian conservation, but also brings additional challenges. Meeting the goals of this plan will take cooperation among myriad stakeholders; yet, even with collaboration, most objectives of this plan will be unattainable if BBS program support is not increased. The BBS developed this strategic plan to help set priorities and identify resources required for the program to continue to meet the evolving needs of the conservation community for information on bird population change. By setting clear goals, strategies, and measures of success, this plan provides a cohesive framework and vision for maintenance and development of the BBS. The plan identifies two major goals for the BBS, with a number of strategies and objectives to achieve these goals. Over the next 5 years, progress made in addressing each long-term goal and its associated 5-year strategies and objectives will gage the plan’s success. Specific actions, projected outcomes, and measures of success related to accomplishing these are outlined in Table 1, with a timeline in Table 2. The two main goals for the program, with a summary of the strategies to achieve them, are: Goal 1: Collect scientifically credible measures of the status and trends of North American bird populations at continental and regional scales. The North American Breeding Bird Survey will continue to support North American natural resource conservation through the collection of scientifically credible measures of the status and trends of continental bird populations. While doing this, the BBS will work to improve the science behind the program to better meet its mission and the changing needs of the avian conservation community. In partnership with collaborators, the BBS will address detection probability bias and habitat bias, improve analytical methods, and more fully assess and account for observer quality. Moreover, the BBS will improve the quality and breadth of avian population data through strategic increases in route density and the establishment of a Mexican BBS program. Goal 2: Ensure BBS data and analytical results are widely available and easily accessible for use by the avian conservation and management communities. At the heart of the BBS lies a four-million-record database containing more than 40 years of data on more than 600 bird species. These data are of no value if not well maintained, appropriately analyzed, and widely and easily accessible. The USGS has greatly improved data management and accessibility in recent years. Trend estimates were first made available via the Internet in the mid-1990s, followed closely by the raw data with baseline metadata and standard operating procedures. Nevertheless, numerous enhancements to data management and the usability of BBS results will greatly improve the ability of the BBS to serve avian conservation goals. The BBS needs to ensure that BBS data and results presented on the web site use the best data-management practices and statistical methods, with adequate documentation for users to understand them and any differences between different trend estimates. Moreover, the BBS needs to increase communication with BBS partners and stakeholders to ensure that it continues to meet the avian population status and trends needs of the conservation community and to encourage the development of new products. Working with collaborators, the BBS will develop tools for integrating environmental parameters like habitat change into the analyses, and for integrating BBS data with other avian survey results. In addition, the BBS will continue to improve data and database management through the incorporation of additional data and data fields, such as georeferenced stop locations and more complete metadata for the raw data and results, thus enhancing the uses that can be made of the data.

Circular↗

Measurements of HFC-134a and HCFC-22 in groundwater and unsaturated-zone air: implications for HFCs and HCFCs as dating tracers

A new analytical method using gas chromatography with an atomic emission detector (GC–AED) was developed for measurement of ambient concentrations of hydrochlorofluorocarbons (HCFCs) and hydrofluorocarbons (HFCs) in soil, air, and groundwater, with the goal of determining their utility as groundwater age tracers. The analytical detection limits of HCFC-22 (difluorochloromethane, CHClF 2 ) and HFC-134a (1,2,2,2-tetrafluoroethane, C 2 H 2 F 4 ) in 1 L groundwater samples are 4.3 × 10 − 1 and 2.1 × 10 − 1 pmol kg − 1 , respectively, corresponding to equilibrium gas-phase mixing ratios of approximately 5–6 parts per trillion by volume (pptv). Under optimal conditions, post-1960 (HCFC-22) and post-1995 (HFC-134a) recharge could be identified using these tracers in stable, unmixed groundwater samples. Ambient concentrations of HCFC-22 and HFC-134a were measured in 50 groundwater samples from 27 locations in northern and western parts of Virginia, Tennessee, and North Carolina (USA), and 3 unsaturated-zone profiles were collected in northern Virginia. Mixing ratios of both HCFC-22 and HFC-134a decrease with depth in unsaturated-zone gas profiles with an accompanying increase in CO 2 and loss of O 2 . Apparently, ambient concentrations of HCFC-22 and HFC-134a are readily consumed by methanotrophic bacteria under aerobic conditions in the unsaturated zone. The results of this study indicate that soils are a sink for these two greenhouse gases. These observations contradict the previously reported results from microcosm experiments that found that degradation was limited above-ambient HFC-134a. The groundwater HFC and HCFC concentrations were compared with concentrations of chlorofluorocarbons (CFCs, CFC-11, CFC-12, CFC-113) and sulfur hexafluoride (SF 6 ). Nearly all samples had measured HCFC-22 or HFC-134a that were below concentrations predicted by the CFCs and SF6, with many samples showing a complete loss of HCFC-22 and HFC-134a. This study indicates that HCFC-22 and HFC-134a are not conservative as environmental tracers and leaves in question the usefulness of other HCFCs and HFCs as candidate age tracers.

North Carolina, Tennessee, Virginia↗

Catalog of Mount St. Helens 2004-2007 dome samples with major- and trace-element chemistry

Sampling and analysis of eruptive products at Mount St. Helens is an integral part of volcano monitoring efforts conducted by the U.S. Geological Survey?s Cascades Volcano Observatory (CVO). The objective of our eruption sampling program is to enable petrological assessments of pre-eruptive magmatic conditions, critical for ascertaining mechanisms for eruption triggering and forecasting potential changes in eruption behavior. This report provides a catalog of near-vent lithic debris and new dome-lava collected during 34 intra-crater sampling forays throughout the October 2004 to October 2007 (2004-7) eruptive interval at Mount St. Helens. In addition, we present comprehensive bulk-rock geochemistry for a time-series of representative (2004-7) eruption products. This data, along with that in a companion report on Mount St. Helens 2004 to 2006 tephra by Rowe and others (2008), are presented in support of the contents of the U.S. Geological Survey Professional Paper 1750 (Sherrod and others, eds., 2008). Readers are referred to appropriate chapters in USGS Professional Paper 1750 for detailed narratives of eruptive activity during this time period and for interpretations of sample characteristics and geochemical data. The suite of rock samples related to the 2004-7 eruption of Mount St. Helens and presented in this catalog are archived at the David A. Johnson Cascades Volcano Observatory, Vancouver, Wash. The Mount St. Helens 2004-7 Dome Sample Catalogue with major- and trace-element geochemistry is tabulated in 3 worksheets of the accompanying Microsoft Excel file, of2008-1130.xls. Table 1 provides location and sampling information. Table 2 presents sample descriptions. In table 3, bulk-rock major and trace-element geochemistry is listed for 44 eruption-related samples with intra-laboratory replicate analyses of 19 dacite lava samples. A brief overview of the collection methods and lithology of dome samples is given below as an aid to deciphering the dome sample catalog. This is followed by an explanation of the categories of sample information (column headers) in Tables 1 and 2. A summary of the analytical methods used to obtain the geochemical data in this report introduces the presentation of major- and trace-element geochemistry of 2004-7 Mount St. Helens dome samples in table 3. Intra-laboratory results for the USGS AGV-2 standard are presented (tables 4 and 5), which demonstrate the compatibility of chemical data from different sources.

Open-File Report↗

Palynological assessment of organic tissues and metallic minerals in the Jerritt Canyon gold deposit, Nevada (U.S.A.)

Organic tissues and metallic minerals were studied in acid residues and thin section of the Jerritt Canyon (Bell Mine) gold deposit. The purpose was to compare gold-bearing and gold-free rocks, characterize their differences, and assess a possible relationship between the invisible gold and the organic tissues in these early Paleozoic, carbonaceous limestones, dolomites, and claystones. The most visually abundant acid-resistant component in the sooty, unoxidized, gold-bearing rocks is a black, rectangular, carbon-bearing mineraloid. In X-ray diffraction, it is poorly crystalline; in nuclear magnetic resonance, it is a highly aromatized structure. The increase in gold content that accompanies the increase in content of this protographite suggests that it may be the major gold-bearing compound. Less abundant among the acid-resistant residues are uncarbonized organic tissues that are typical of marine settings. The tissues not in the vicinity of silicified veins are medium to dark brown. The dominant tissues are the amorphous remains of algae and their zooplankton predators. These uncarbonized indigenous tissues indicate that temperatures were lower than those determined by geochemical and fluid inclusion methods. The presence of different kinds of carbon-bearing compounds could account for the discrepancy between the palynological and geochemical data. The uncarbonized organic tissues comprise such a small percentage of these rocks that they could be easily missed by bulk analytical methods. The presence of uncarbonized tissues helps to constrain the duration of the high heat flow that is shown by the fluid inclusion data. The presence of mixed signals suggests that the protographite may be the product of chemical rather than thermal reactions.

Nevada↗

Determination of 15N/14N and 13C/12C in solid and aqueous cyanides

The stable isotopic compositions of nitrogen and carbon in cyanide compounds can be determined by combusting aliquots in sealed tubes to form N 2 gas and CO 2 gas and analyzing the gases by mass spectrometry. Free cyanide (CN - aq + HCN aq ) in simple solutions can also be analyzed by first precipitating the cyanide as copper(II) ferrocyanide and then combusting the precipitate. Reproducibility is ±0.5‰ or better for both δ 15 N and δ 13 C. If empirical corrections are made on the basis of carbon yields, the reproducibility of δ 13 C can be improved to ±0.2‰. The analytical methods described herein are sufficiently accurate and precise to apply stable isotope techniques to problems of cyanide degradation in natural waters and industrial process solutions.

Analytical Chemistry↗

Estimating hydraulic properties of volcanic aquifers using constant-rate and variable-rate aquifer tests

In recent years the ground-water demand of the population of the island of Maui, Hawaii, has significantly increased. To ensure prudent management of the ground-water resources, an improved understanding of ground-water flow systems is needed. At present, large-scale estimations of aquifer properties are lacking for Maui. Seven analytical methods using constant-rate and variable-rate withdrawals for single wells provide an estimate of hydraulic conductivity and transmissivity for 103 wells in central Maui. Methods based on constant-rate tests, although not widely used on Maui, offer reasonable estimates. Step-drawdown tests, which are more abundantly used than other tests, provide similar estimates as constant-rate tests. A numerical model validates the suitability of analytical solutions for step-drawdown tests and additionally provides an estimate of storage parameters. The results show that hydraulic conductivity is log-normally distributed and that for dike-free volcanic rocks it ranges over several orders of magnitude from 1 to 2,500 m/d. The arithmetic mean, geometric mean, and median values of hydraulic conductivity are respectively 520, 280, and 370 m/d for basalt and 80, 50, and 30 m/d for sediment. A geostatistical approach using ordinary kriging yields a prediction of hydraulic conductivity on a larger scale. Overall, the results are in agreement with values published for other Hawaiian islands. ?? 2007 American Water Resources Association.

Journal of the American Water Resources Associatio↗

Methods for estimating annual exceedance probability discharges for streams in Arkansas, based on data through water year 2013

In 2013, the U.S. Geological Survey initiated a study to update regional skew, annual exceedance probability discharges, and regional regression equations used to estimate annual exceedance probability discharges for ungaged locations on streams in the study area with the use of recent geospatial data, new analytical methods, and available annual peak-discharge data through the 2013 water year. An analysis of regional skew using Bayesian weighted least-squares/Bayesian generalized-least squares regression was performed for Arkansas, Louisiana, and parts of Missouri and Oklahoma. The newly developed constant regional skew of -0.17 was used in the computation of annual exceedance probability discharges for 281 streamgages used in the regional regression analysis. Based on analysis of covariance, four flood regions were identified for use in the generation of regional regression models. Thirty-nine basin characteristics were considered as potential explanatory variables, and ordinary least-squares regression techniques were used to determine the optimum combinations of basin characteristics for each of the four regions. Basin characteristics in candidate models were evaluated based on multicollinearity with other basin characteristics (variance inflation factor < 2.5) and statistical significance at the 95-percent confidence level ( p ≤ 0.05). Generalized least-squares regression was used to develop the final regression models for each flood region. Average standard errors of prediction of the generalized least-squares models ranged from 32.76 to 59.53 percent, with the largest range in flood region D. Pseudo coefficients of determination of the generalized least-squares models ranged from 90.29 to 97.28 percent, with the largest range also in flood region D. The regional regression equations apply only to locations on streams in Arkansas where annual peak discharges are not substantially affected by regulation, diversion, channelization, backwater, or urbanization. The applicability and accuracy of the regional regression equations depend on the basin characteristics measured for an ungaged location on a stream being within range of those used to develop the equations.

Arkansas↗

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↗

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↗

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↗

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↗

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↗

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↗

Amino acid racemization dating of fossil bones, I. inter-laboratory comparison of racemization measurements

Enantiomeric measurements for aspartic acid, glutamic acid, and alanine in twenty-one different fossil bone samples have been carried out by three different laboratories using different analytical methods. These inter-laboratory comparisons demonstrate that D/L aspartic acid measurements are highly reproducible, whereas the enantiomeric measurements for the other amino acids show a wide variation between the three laboratories. At present, aspartic acid measurements are the most suitable for racemization dating of bone because of their superior analytical precision.

Earth and Planetary Science Letters↗

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↗

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↗