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USGS2014

Precise determination of δ 88 Sr in rocks, minerals, and waters by double-spike TIMS: A powerful tool in the study of chemical, geologic, hydrologic and biologic processes

We present strontium isotopic ( 88 Sr/ 86 Sr and 87 Sr/ 86 Sr) results obtained by 87 Sr– 84 Sr double spike thermal ionization mass-spectrometry (DS-TIMS) for several standards as well as natural water samples and mineral samples of abiogenic and biogenic origin. The detailed data reduction algorithm and a user-friendly Sr-specific stand-alone computer program used for the spike calibration and the data reduction are also presented. Accuracy and precision of our δ 88 Sr measurements, calculated as permil (‰) deviations from the NIST SRM-987 standard, were evaluated by analyzing the NASS-6 seawater standard, which yielded δ 88 Sr = 0.378 ± 0.009‰. The first DS-TIMS data for the NIST SRM-607 potassium feldspar standard and for several US Geological Survey carbonate, phosphate, and silicate standards (EN-1, MAPS-4, MAPS-5, G-3, BCR-2, and BHVO-2) are also reported. Data obtained during this work for Sr-bearing solids and natural waters show a range of δ 88 Sr values of about 2.4‰, the widest observed so far in terrestrial materials. This range is easily resolvable analytically because the demonstrated external error (±SD, standard deviation) for measured δ 88 Sr values is typically ≤0.02‰. It is shown that the “true” 87 Sr/ 86 Sr value obtained by the DS-TIMS or any other external normalization method combines radiogenic and mass-dependent mass-fractionation effects, which cannot be separated. Therefore, the “true” 87 Sr/ 86 Sr and the δ 87 Sr parameter derived from it are not useful isotope tracers. Data presented in this paper for a wide range of naturally occurring sample types demonstrate the potential of the δ 88 Sr isotope tracer in combination with the traditional radiogenic 87 Sr/ 86 Sr tracer for studying a variety of biological, hydrological, and geological processes.

Journal of Analytical Atomic Spectrometry↗

USGS2002

Quantitative radiochemical method for determination of major sources of natural radioactivity in ores and minerals

When an ore sample contains radioactivity other than that attributable to the uranium series in equilibrium, a quantitative analysis of the other emitters must be made in order to determine the source of this activity. Thorium-232, radon-222, and lead-210 have been determined by isolation and subsequent activity analysis of some of their short-lived daughter products. The sulfides of bismuth and polonium are precipitated out of solutions of thorium or uranium ores, and the α -particle activity of polonium-214, polonium-212, and polonium-210 is determined by scintillation-counting techniques. Polonium-214 activity is used to determine radon-222, polonium-212 activity for thorium-232, and polonium-210 for lead-210. The development of these methods of radiochemical analysis will facilitate the rapid determination of some of the major sources of natural radioactivity.

Analytical Chemistry↗

USGS1958

Apparatus and technique for multiple tests by the confined-spot method of colorimetric analysis: Application to field estimation of nickel and copper

The confined-spot method of colorimetric analysis is generally applicable to the semiquantitative estimation of traces of ions in solution that form colored precipitates or otherwise alter material on a confined area of reagent paper. For precise results, the rate of flow of test solutions through the reagent paper must be reproduced on successive runs, so that the same proportion of reaction products is collected each time on the confined spot. A simple apparatus gives a controlled rate of flow and makes possible the analysis of many samples at one time with good reproducibility. This apparatus utilizes the increasing pull, resulting from the gradual lowering of the water level in a tank, to draw a sample solution through a confined area of reagent paper at a reproducible rate. Application to the rapid determination of nickel with dimethylglyoxime and of copper with rubeanic acid provides a method for determination of as little as 0.06 γ of nickel and 0.03 γ of copper. The coefficients of variation are 14 and 22%, respectively. This method has wide applicability in more rapid and convenient determination of trace amounts of many metals.

Analytical Chemistry↗

USGS1950

Spectrographic analysis of coal and coal ash

Coal can be analyzed on the spectrograph for per cent ash and composition of ash in a matter of a few minutes, using the total energy method. The composition of the ash so determined can be used to calculate ash softening temperatures. This analysis can be made in sufficiently short a time to control tipple and washing operations for preparation of coal to meet specifications. This spectrographic method can be readily adapted to the analysis of rocks, minerals, and inorganic chemicals of all kinds.

Analytical Chemistry↗

USGS2010

A new capture fraction method to map how pumpage affects surface water flow

All groundwater pumped is balanced by removal of water somewhere, initially from storage in the aquifer and later from capture in the form of increase in recharge and decrease in discharge. Capture that results in a loss of water in streams, rivers, and wetlands now is a concern in many parts of the United States. Hydrologists commonly use analytical and numerical approaches to study temporal variations in sources of water to wells for select points of interest. Much can be learned about coupled surface/groundwater systems, however, by looking at the spatial distribution of theoretical capture for select times of interest. Development of maps of capture requires (1) a reasonably well-constructed transient or steady state model of an aquifer with head-dependent flow boundaries representing surface water features or evapotranspiration and (2) an automated procedure to run the model repeatedly and extract results, each time with a well in a different location. This paper presents new methods for simulating and mapping capture using three-dimensional groundwater flow models and presents examples from Arizona, Oregon, and Michigan. Journal compilation ?? 2010 National Ground Water Association. No claim to original US government works.

Ground Water↗

USGS2001

Evaluation of persistent hydrophobic organic compounds in the Columbia River Basin using semipermeable-membrane devices

Persistent hydrophobic organic compounds are of concern in the Columbia River because they have been correlated with adverse effects on wildlife. We analysed samples from nine main-stem and six tributary sites throughout the Columbia River Basin (Washington and Oregon) for polychlorinated dibenzo-p-dioxins, dibenzofurans, polychlorinated biphenyls, organochlorine pesticides, and priority-pollutant polycyclic aromatic hydrocarbons. Because these compounds may have important biological consequences at aqueous concentrations well below the detection limits associated with conventional sampling methods, we used semipermeable-membrane devices to sample water and achieved parts-per-quintillion detection limits. All of these compound classes were prevalent within the basin, but concentrations of many analytes were highest in the vicinity of Portland-Vancouver, indicating that the Willamette subbasin-and perhaps the urban area in particular-is an important source of these compounds. Data collected during basin low-flow conditions in 1997 and again during basin high-flow conditions in 1998 indicate that in-stream processes such as dilution by relatively clean inflow, and flow through island hyporheic zones may be important mechanisms for attenuating dissolved concentrations of hydrophobic compounds.

Hydrological Processes↗

USGS2019

Rapid pre-concentration of mercury in solids and water for isotopic analysis

The precise quantification of mercury (Hg) stable isotope compositions in low concentration or dilute samples poses analytical challenges due to Hg mass limitations. Common Hg pre-concentration procedures require extended processing times, making rapid Hg stable isotope measurements challenging. Here we present a modified pre-concentration method that combines commonly used Hg reduction and gold trap amalgamation followed by semi-rapid thermal desorption (less than 1 h) and chemical trapping. This custom designed system was demonstrated to perform adequately on multiple trapping matrices including a new bromine monochloride (BrCl) wet oxidant trap (40% 3HNO 3 :BrCl), capable of trapping consistently in 2 mL volume over a wide range of Hg masses (5–200 ng). The procedure was also shown to work effectively on natural matrices, waters and sediments, producing comparable isotope results to the direct digestion analyses. Here, we present a method that can effectively triple sample throughput in comparison to traditional procedures, and also access lower concentration matrices without compromising the accuracy or precision of Hg isotope measurements.

Analytica Chimica Acta↗

USGS2005

Comparison of a novel passive sampler to standard water-column sampling for organic contaminants associated with wastewater effluents entering a New Jersey stream

Four water samples collected using standard depth and width water-column sampling methodology were compared to an innovative passive, in situ, sampler (the polar organic chemical integrative sampler or POCIS) for the detection of 96 organic wastewater-related contaminants (OWCs) in a stream that receives agricultural, municipal, and industrial wastewaters. Thirty-two OWCs were identified in POCIS extracts whereas 9-24 were identified in individual water-column samples demonstrating the utility of POCIS for identifying contaminants whose occurrence are transient or whose concentrations are below routine analytical detection limits. Overall, 10 OWCs were identified exclusively in the POCIS extracts and only six solely identified in the water-column samples, however, repetitive water samples taken using the standard method during the POCIS deployment period required multiple trips to the sampling site and an increased number of samples to store, process, and analyze. Due to the greater number of OWCs detected in the POCIS extracts as compared to individual water-column samples, the ease of performing a single deployment as compared to collecting and processing multiple water samples, the greater mass of chemical residues sequestered, and the ability to detect chemicals which dissipate quickly, the passive sampling technique offers an efficient and effective alternative for detecting OWCs in our waterways for wastewater contaminants.

New Jersey↗

USGS2019

A supervolcano and its sidekicks: A 100 ka eruptive chronology of the Fish Canyon Tuff and associated units of the La Garita magmatic system

Establishing temporal constrains on major volcanic eruptions is limited by the precision of existing geochronometers. Prior work on the La Garita caldera, created by the eruption of the Fish Canyon Tuff, failed to resolve temporal differences between pre-, syn-, and post-collapse eruptive units. Here, we report 40Ar/39Ar geochronologic data supporting a ca. 100 ka eruptive history of the La Garita caldera, and resolving the timing of the precaldera Pagosa Peak Dacite , syncaldera Fish Canyon Tuff, and postcaldera Dacite of Nutras Creek. Minimizing uncertainty in neutron fluence by rotating samples during irradiation and employing Bayesian statistical interpretation of analytical data enables resolution of the ca. 60 ka precaldera eruptive history and a hiatus of 0 - 20 ka prior to the eruption of postcaldera lavas. The improved precision demonstrated using these methods provides previously unresolvable temporal constraints on physical processes in the La Garita magmatic system and underscores the potential of unraveling other closely-spaced events in geologic time.

Geology↗

USGS1975

An integrated-intensity method for emission spectrographic computer analysis

An integrated-intensity method has been devised to improve the computer analysis of data by emission spectrography. The area of the intensity profile of a spectral line is approximated by a rectangle whose height is related to the intensity difference between the peak and background of the line and whose width is measured at a fixed transmittance below the apex of the line. The method is illustrated by the determination of strontium in the presence of greater than 10 percent calcium. The Sr 3380.711-A line, which is unaffected by calcium and which has a linear analytical curve extending from 100-3,000 ppm, has been used to determine strontium in 18 standard reference rocks covering a wide range of geologic materials. Both the accuracy and the precision of the determinations were well within the accepted range for a semiquantitative procedure.

Journal of Research of the U.S. Geological Survey↗

USGS2007

Determination of the δ 15 N of nitrate in solids; RSIL lab code 2894

The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 2894 is to determine the δ 15 N of nitrate (NO 3 - ) in solids. The nitrate fraction of the nitrogen species is dissolved by water (called leaching) and can be analyzed by the bacterial method covered in RSIL lab code 2899. After leaching, the δ 15 N of the dissolved NO 3 - is analyzed by conversion of the NO 3 - to nitrous oxide (N 2 O), which serves as the analyte for mass spectrometry. A culture of denitrifying bacteria is used in the enzymatic conversion of NO 3 - to N 2 O, which follows the pathway shown in equation 1: NO 3 - → NO 2 - → NO → 1/2 N 2 O (1) Because the bacteria Pseudomonas aureofaciens lack N 2 O reductive activity, the reaction stops at N 2 O, unlike the typical denitrification reaction that goes to N 2 . After several hours, the conversion is complete, and the N 2 O is extracted from the vial, separated from volatile organic vapor and water vapor by an automated -65 °C isopropanol-slush trap, a Nafion drier, a CO 2 and water removal unit (Costech #021020 carbon dioxide absorbent with Mg(ClO 4 ) 2 ), and trapped in a small-volume trap immersed in liquid nitrogen with a modified Finnigan MAT (now Thermo Scientific) GasBench 2 introduction system. After the N 2 O is released, it is further purified by gas chromatography before introduction to the isotope-ratio mass spectrometer (IRMS). The IRMS is a Thermo Scientific Delta V Plus continuous flow IRMS (CF-IRMS). It has a universal triple collector, consisting of two wide cups with a narrow cup in the middle; it is capable of simultaneously measuring mass/charge ( m/z ) of the N 2 O molecule 44, 45, and 46. The ion beams from these m/z values are as follows: m/z = 44 = N 2 O = 14 N 14 N 16 O; m/z = 45 = N 2 O = 14 N 15 N 16 O or 14 N 14 N 17 O; m/z = 46 = N 2 O = 14 N 14 N 18 O. The 17 O contributions to the m/z 44 and m/z 45 ion beams are accounted for before δ 15 N values are reported.

Techniques and Methods↗

USGS2021

Experimental evaluation of spatial capture–recapture study design

A principal challenge impeding strong inference in analyses of wild populations is the lack of robust and long-term data sets. Recent advancements in analytical tools used in wildlife science may increase our ability to integrate smaller data sets and enhance the statistical power of population estimates. One such advancement, the development of spatial capture–recapture (SCR) methods, explicitly accounts for differences in spatial study designs, making it possible to equate multiple study designs in one analysis. SCR has been shown to be robust to variation in design as long as minimal sampling guidance is adhered to. However, these expectations are based on simulation and have yet to be evaluated in wild populations. Here we conduct a rigorously designed field experiment by manipulating the arrangement of artificial cover objects (ACOs) used to collect data on red-backed salamanders ( Plethodon cinereus ) to empirically evaluate the effects of design configuration on inference made using SCR. Our results suggest that, using SCR, estimates of space use and detectability are sensitive to study design configuration, namely the spacing and extent of the array, and that caution is warranted when assigning biological interpretation to these parameters. However, estimates of population density remain robust to design except when the configuration of detectors grossly violates existing recommendations.

Massachusetts↗

USGS2018

Seeking excellence: An evaluation of 235 international laboratories conducting water isotope analyses by isotope-ratio and laser-absorption spectrometry

Rationale Water stable isotope ratios ( δ 2 H and δ 18 O values) are widely used tracers in environmental studies; hence, accurate and precise assays are required for providing sound scientific information. We tested the analytical performance of 235 international laboratories conducting water isotope analyses using dual-inlet and continuous-flow isotope ratio mass spectrometers and laser spectrometers through a water isotope inter-comparison test. Methods Eight test water samples were distributed by the IAEA to international stable isotope laboratories. These consisted of a core set of five samples spanning the common δ -range of natural waters, and three optional samples (highly depleted, enriched, and saline). The fifth core sample contained unrevealed trace methanol to assess analyst vigilance to the impact of organic contamination on water isotopic measurements made by all instrument technologies. Results For the core and optional samples ~73 % of laboratories gave acceptable results within 0.2 ‰ and 1.5 ‰ of the reference values for δ 18 O and δ 2 H, respectively; ~27 % produced unacceptable results. Top performance for δ 18 O values was dominated by dual-inlet IRMS laboratories; top performance for δ 2 H values was led by laser spectrometer laboratories. Continuous-flow instruments yielded comparatively intermediate results. Trace methanol contamination of water resulted in extreme outlier δ -values for laser instruments, but also affected reactor-based continuous-flow IRMS systems; however, dual-inlet IRMS δ -values were unaffected. Conclusions Analysis of the laboratory results and their metadata suggested inaccurate or imprecise performance stemmed mainly from skill- and knowledge-based errors including: calculation mistakes, inappropriate or compromised laboratory calibration standards, poorly performing instrumentation, lack of vigilance to contamination, or inattention to unreasonable isotopic outcomes. To counteract common errors, we recommend that laboratories include 1–2 'known' control standards in all autoruns; laser laboratories should screen each autorun for spectral contamination; and all laboratories should evaluate whether derived d- excess values are realistic when both isotope ratios are measured. Combined, these data evaluation strategies should immediately inform the laboratory about fundamental mistakes or compromised samples.

Rapid Communications in Mass Spectrometry↗

USGS2014

11.12 - Volatile hydrocarbons and fuel oxygenates

Petroleum hydrocarbons and fuel oxygenates are among the most commonly occurring and widely distributed contaminants in the environment. This chapter presents a summary of the sources, transport, fate, and remediation of volatile fuel hydrocarbons and fuel additives in the environment. Much research has focused on the transport and transformation processes of petroleum hydrocarbons and fuel oxygenates, such as benzene, toluene, ethylbenzene, and xylenes and methyl tert‐butyl ether, in groundwater following release from underground storage tanks. Natural attenuation from biodegradation limits the movement of these contaminants and has received considerable attention as an environmental restoration option. This chapter summarizes approaches to environmental restoration, including those that rely on natural attenuation, and also engineered or enhanced remediation. Researchers are increasingly combining several microbial and molecular-based methods to give a complete picture of biodegradation potential and occurrence at contaminated field sites. New insights into the fate of petroleum hydrocarbons and fuel additives have been gained by recent advances in analytical tools and approaches, including stable isotope fractionation, analysis of metabolic intermediates, and direct microbial evidence. However, development of long-term detailed monitoring programs is required to further develop conceptual models of natural attenuation and increase our understanding of the behavior of contaminant mixtures in the subsurface.

Book chapter↗

USGS2006

A laboratory and field evaluation of a portable immunoassay test for triazine herbicides in environmental water samples

The usefulness and sensitivity, of a portable immunoassay test for the semiquantitative field screening of water samples was evaluated by means of laboratory and field studies. Laboratory results indicated that the tests were useful for the determination of atrazine concentrations of 0.1 to 1.5 μg/L. At a concentration of 1 μg/L, the relative standard deviation in the difference between the regression line and the actual result was about 40 percent. The immunoassay was less sensitive and produced similar errors for other triazine herbicides. After standardization, the test results were relatively insensitive to ionic content and variations in pH (range, 4 to 10), mildly sensitive to temperature changes, and quite sensitive to the timing of the final incubation step, variances in timing can be a significant source of error. Almost all of the immunoassays predicted a higher atrazine concentration in water samples when compared to results of gas chromatography. If these tests are used as a semiquantitative screening tool, this tendency for overprediction does not diminish the tests' usefulness. Generally, the tests seem to be a valuable method for screening water samples for triazine herbicides.

International Journal of Environmental Analytical ↗

USGS2017

Detection of Nanophyetus salmincola in water, snails, and fish tissues by quantitative polymerase chain reaction

We report the development and validation of two quantitative PCR (qPCR) assays to detect Nanophyetus salmincola DNA in water samples and in fish and snail tissues. Analytical and diagnostic validation demonstrated good sensitivity, specificity, and repeatability of both qPCR assays. The N. salmincola DNA copy number in kidney tissue was significantly correlated with metacercaria counts based on microscopy. Extraction methods were optimized for the sensitive qPCR detection of N. salmincola DNA in settled water samples. Artificially spiked samples suggested that the 1-cercaria/L threshold corresponded to an estimated log 10 copies per liter ≥ 6.0. Significant correlation of DNA copy number per liter and microscopic counts indicated that the estimated qPCR copy number was a good predictor of the number of waterborne cercariae. However, the detection of real-world samples below the estimated 1-cercaria/L threshold suggests that the assays may also detect other N. salmincola life stages, nonintact cercariae, or free DNA that settles with the debris. In summary, the qPCR assays reported here are suitable for identifying and quantifying all life stages of N. salmincola that occur in fish tissues, snail tissues, and water.

Journal of Aquatic Animal Health↗

USGS2026

A review of extraction techniques for per- and polyfluoroalkyl substances in graminaceous plants

Per- and polyfluoroalkyl substances (PFAS) are a wide-ranging class of manufactured chemicals that are environmentally persistent. Due to their ubiquity and resistance to degradation, PFAS readily bioaccumulate in a variety of environmental matrices and elicit a range of toxicological impacts. Despite an increase in research into these compounds, there is a clear gap in consensus on extraction techniques to quantify many PFAS in certain environmental media, particularly at critical points in agricultural food systems such as pasture grasses and feedstocks. Developing methods for more comprehensive and accurate extraction of PFAS in plant tissues is crucial for the biomonitoring of PFAS contamination in these ecosystems. This review seeks to identify relevant information pertaining to the partitioning of PFAS in plant matrices and evaluate the performance of previously established methods for the extraction of PFAS in graminaceous plants. Evaluated methods varied widely in extraction techniques, limits of detection and accuracy. This review provides a framework for enhancing PFAS analysis by tailoring extraction and cleanup strategies to both complex plant matrices and diverse analyte properties. Standardizing these methodologies will provide the high-quality data essential for ecotoxicologists and policymakers to accurately map the metabolic fate and ecological risks of these pollutants across food webs.

Critical Reviews in Analytical Chemistry↗

USGS2023

Groundwater quality in the Mohawk and western New York River Basins, New York, 2016

Water samples were collected from July through December 2016 from 9 production wells and 13 domestic wells in the Mohawk River Basin, and from 17 production wells and 17 domestic wells in the western New York River Basins. The samples were collected and processed by using standard U.S. Geological Survey methods and were analyzed for 320 physicochemical properties and constituents, including dissolved gases, major ions, nutrients, trace elements, pesticides, volatile organic compounds, radionuclides, and indicator bacteria, to characterize groundwater quality in the basins. Analytical results are provided in the companion U.S. Geological Survey data release titled “Groundwater Quality Data From the Mohawk and Western New York River Basins, New York, 2016.” The Mohawk River Basin study area covers 3,500 square miles in New York. Of the 22 wells sampled in the Mohawk River Basin, 8 are completed in sand and gravel, and 14 are completed in bedrock aquifers. Most constituents in the samples from the Mohawk River Basin were present in concentrations below the maximum contaminant levels used in public supply drinking-water regulations by the New York State Department of Health and the U.S. Environmental Protection Agency. Values for some of the properties and concentrations of some constituents—pH, color, iron, manganese, aluminum, sodium, chloride, dissolved solids, radon-222, and heterotrophic plate count—sometimes equaled or exceeded primary, secondary, or proposed drinking-water standards. The western New York River Basins study area covers 5,340 square miles in western New York and includes parts of the Lake Erie and Niagara River Basins, the western Lake Ontario Basin (between the Niagara River and Genesee River Basins), and the Allegheny River Basin. Of the 34 wells sampled in the western New York River Basins, 16 are completed in sand and gravel, and 18 are completed in bedrock aquifers. Most constituents in the samples from the western New York River Basins were present in concentrations below the maximum contaminant levels used in public supply drinking-water regulations by the New York State Department of Health and the U.S. Environmental Protection Agency. Values for some of the properties and concentrations of some constituents—color, chloride, sodium, dissolved solids, iron, manganese, aluminum, arsenic, barium, radon-222, methane, total coliform bacteria, fecal coliform bacteria, and Escherichia coli bacteria—sometimes equaled or exceeded primary, secondary, or proposed drinking-water standards.

New York↗