SEARCH · Search USGS

Results for “Analytical Methods”

Search indexed USGS publications on groundwater, aquifers, geologic maps, mineral resources and earthquakes. Explore source records by subject and place.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,009 records · Page 56Linked to original sources

USGS1978

Historical profile, Quality of Water Laboratories, U. S. Geological Survey

During the period 1918 to 1973 the U.S. Geological Survey, Water Resources Division, established 22 District-type water quality laboratories. These facilities provided the analytical capability and water-quality information for hydrologic investigations and the national baseline inventory of chemical, physical, fluvial sediment, and biological characteristics of surface and ground waters in the United States. Prior to 1950, most methods used in the laboratory were gravimetric, colorimetric, or titrimetric. Flame photometric equipment was common to most laboratories in the 1950's, and the atomic absorption spectrophotometer was added to larger laboratories in the 1960's. In the late 1960's, the first of the automatic analyzers was installed. Total annual production averaged about 480 adjusted complete analyses during the early years 1919-28, about 7,800 in 1946, and about 50,000 in 1970. Budget estimates for the majority of laboratories ranged from $25,000 to $50,000 (1940-50) and $75,000 to $300,000 (1965-73). Beginning in 1972, major functions of the 22 laboratories have been combined into two comprehensive highly-automated facilities located at Denver (Arvada), Colo., and Atlanta (Doraville), Ga. These laboratories comprise the Central Laboratory System for the U.S. Geological Survey. (Woodard-USGS)

Open-File Report↗

USGS2016

Montana StreamStats

About this volume Montana StreamStats is a Web-based geographic information system ( http://water.usgs.gov/osw/streamstats/ ) application that provides users with access to basin and streamflow characteristics for gaged and ungaged streams in Montana. Montana StreamStats was developed by the U.S. Geological Survey (USGS) in cooperation with the Montana Departments of Transportation, Environmental Quality, and Natural Resources and Conservation. The USGS Scientific Investigations Report consists of seven independent but complementary chapters dealing with various aspects of this effort. Chapter A describes the Montana StreamStats application, the basin and streamflow datasets, and provides a brief overview of the streamflow characteristics and regression equations used in the study. Chapters B through E document the datasets, methods, and results of analyses to determine streamflow characteristics, such as peak-flow frequencies, low-flow frequencies, and monthly and annual characteristics, for USGS streamflow-gaging stations in and near Montana. The StreamStats analytical toolsets that allow users to delineate drainage basins and solve regression equations to estimate streamflow characteristics at ungaged sites in Montana are described in Chapters F and G.

Montana↗

USGS1993

Concentration history during pumping from a leaky aquifer with stratified initial concentration

Analytical and numerical solutions are employed to examine the concentration history of a dissolved substance in water pumped from a leaky aquifer. Many aquifer systems are characterized by stratification, for example, a sandy layer overlain by a clay layer. To obtain information about separate hydrogeologic units, aquifer pumping tests are often conducted with a well penetrating only one of the layers. When the initial concentration distribution is also stratified (the concentration varies with elevation only), the concentration breakthrough in the pumped well may be interpreted to provide information on aquifer hydraulic and transport properties. To facilitate this interpretation, we present some simple analytical and numerical solutions for limiting cases and illustrate their application to a fractured bedrock/glacial drift aquifer system where the solute of interest is dissolved radon gas. In addition to qualitative information on water source, this method may yield estimates of effective porosity and saturated thickness (or fracture transport aperture) from a single-hole test. Little information about dispersivity is obtained because the measured concentration is not significantly affected by dispersion in the aquifer.

Conference Paper↗

USGS2020

A comparison of groundwater sampling technologies, including passive diffusion sampling, for radionuclide contamination

Using traditional high-flow purge methods for long-term water quality monitoring of deep groundwater wells can be expensive, affect contaminant migration, and produce excessive volumes of discharge water that can be difficult to manage. The use of low-flow pumping methods and depth discrete bailers (DDBs) can reduce the cost of sampling deep groundwater wells. In general, using different pumping methods to obtain reproducible and representative groundwater can be challenging. Passive diffusion samplers (PDSs) have successfully been used in long-term monitoring for volatile organic compounds, major ions, and trace-elements, but application has been limited for stable and radioactive isotopes. Beginning in 2018, the United States Geological Survey (USGS) conducted three sampling events to test the ability of PDSs and DDBs to obtain reproducible and representative groundwater samples. The sampled well is completed in a regional, permeable carbonate aquifer and is one in a set of wells that have historically been used for tritium tracer testing. All samples were obtained at 180 m (590 ft) below land surface (bls) in a 13.97 cm (5.5 inch) uncased well that has a total depth of 202 m (662 ft) bls. The first sampling event deployed a regenerated cellulose dialysis membrane (RCDM) PDS for 14 days with deionized water as the blank. The second sampling event deployed a RCDM for 27 days also with deionized water as the blank. The third sampling event deployed a Dual Membrane (DM) PDS for 65 days using a blank of tritium-dead carbonate water. The DM PDS was used to assess the effect of longer-term deployment on tritium concentrations and address whether or not the PDSs reached equilibrium with ambient groundwater. The day after each of the three passive samplers were retrieved a DDB was used to obtain discrete non-integrated groundwater samples. For each DDB sampling day, the bailer was lowered into the well 10 consecutive times to determine if the water chemistry changed from the first to the last bailed sample. Quality assurance samples including blanks and duplicates were obtained during all three sampling events. All blank waters had tritium concentrations less than 21±33 pCi/L. Major ion (e.g. calcium, chloride, sodium, and sulfate) results were compared between all samples obtained with RCDM and DDB. Major ion concentrations showed a coefficient of variation of less than 6% between all RCDM and DDB samples; however, the coefficient of variation between the different deployment times and the two different methods for trace-element concentrations was much larger, particularly for manganese (82%), lead (41%), and zinc (33%). Stable isotope values were compared between the RCDM and DDB samples. The DDB sample results all fell within analytical uncertainty and were considered representative of the formation groundwater. The stable isotope values from the RCDM samples indicated that a longer deployment time was necessary to gain equilibrium and to obtain representative groundwater samples. Tritium results from groundwater samples obtained from the RCDM, DM, and DDB indicate that groundwaters obtained with PDSs produced tritium concentrations 2 to 3 times higher (between 1,426 and 3,060±87 pCi/L) than groundwaters obtained with a DDB (479 to 1,219±51 pCi/L). The longer the passive diffusion samplers were deployed, the higher the tritium concentration, suggesting that equilibrium with tritium was not reached within a 27-day deployment. DDB samples showed tritium results declining from the first to the last bailed sample for all three sampling events. This research suggests that tritium results from groundwater samples obtained from PDSs are more reproducible than samples obtained from DDBs. Also, PDSs likely do not accumulate isotopes of water but rather equilibrate with the ambient groundwater. On the other hand, both PDSs and DDBs were able to provide representative groundwater samples for major ions and have the potential to produce.

Conference Paper↗

USGS2002

Measurement of the oxygen isotopic composition of nitrate in seawater and freshwater using the denitrifier method

We report a novel method for measurement of the oxygen isotopic composition ( 18 O/ 16 O) of nitrate (NO 3 - ) from both seawater and freshwater. The denitrifier method, based on the isotope ratio analysis of nitrous oxide generated from sample nitrate by cultured denitrifying bacteria, has been described elsewhere for its use in nitrogen isotope ratio ( 15 N/ 14 N) analysis of nitrate. 1 Here, we address the additional issues associated with 18 O/ 16 O analysis of nitrate by this approach, which include (1) the oxygen isotopic difference between the nitrate sample and the N 2 O analyte due to isotopic fractionation associated with the loss of oxygen atoms from nitrate and (2) the exchange of oxygen atoms with water during the conversion of nitrate to N 2 O. Experiments with 18 O-labeled water indicate that water exchange contributes less than 10%, and frequently less than 3%, of the oxygen atoms in the N 2 O product for Pseudomonas aureofaciens. In addition, both oxygen isotope fractionation and oxygen atom exchange are consistent within a given batch of analyses. The analysis of appropriate isotopic reference materials can thus be used to correct the measured 18 O/ 16 O ratios of samples for both effects. This is the first method tested for 18 O/ 16 O analysis of nitrate in seawater. Benefits of this method, relative to published freshwater methods, include higher sensitivity (tested down to 10 nmol and 1 μM NO 3 - ), lack of interference by other solutes, and ease of sample preparation.

Analytical 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↗

USGS2009

Collection of pyrethroids in water and sediment matrices: Development and validation of a standard operating procedure

Loss of pyrethroid insecticides onto surfaces during sample collection can confound the interpretation of analytical and toxicity test results. Sample collection devices, container materials, and water matrix composition have a significant influence on the association of pyrethroids to container walls, which can be as high as 50 percent. Any sample collection method involving transfer through multiple containers or pieces of equipment increases the potential for pyrethroid loss. This loose 'surface-association' with container walls can be reversed through agitation. When sampling water matrices with pumps or autosamplers, no pyrethroids were lost as long as the water was moving continuously through the system. When collecting water matrices in containers, the material with the least amount of pyrethroid sorption is as follows: glass less than (<) plastic less than (<) Teflon. Additionally, pyrethroids were easier to re-suspend from the glass container walls. Since the amount of surface-association is proportional to the ratio of volume-to-contact-area of the sample, taking larger-volume field samples (greater than 3 liters) reduced pyrethroid losses to less than 10 percent. The amount of surface-association cannot be predicted easily because of the dependence on water matrix composition; samples with higher dissolved organic carbon or suspended-sediment concentrations were observed to have lower percent loss. Sediment samples were not affected by glass-container sorption (the only containers tested). Standardized sample-collection protocols are critical to yield accurate pyrethroid concentrations for assessment of potential effects, and have been summarized in an accompanying standard operating procedure.

Scientific Investigations Report↗

USGS2005

Organic wastewater compounds, pharmaceuticals, and coliphage in ground water receiving discharge from onsite wastewater treatment systems near La Pine, Oregon: Occurrence and implications for transport

The occurrence of organic wastewater compounds (components of 'personal care products' and other common household chemicals), pharmaceuticals (human prescription and nonprescription medical drugs), and coliphage (viruses that infect coliform bacteria, and found in high concentrations in municipal wastewater) in onsite wastewater (septic tank effluent) and in a shallow, unconfined, sandy aquifer that serves as the primary source of drinking water for most residents near La Pine, Oregon, was documented. Samples from two types of observation networks provided basic occurrence data for onsite wastewater and downgradient ground water. One observation network was a group of 28 traditional and innovative (advanced treatment) onsite wastewater treatment systems and associated downgradient drainfield monitoring wells, referred to as the 'innovative systems network'. The drainfield monitoring wells were located adjacent to or under onsite wastewater treatment system drainfield lines. Another observation network, termed the 'transect network', consisted of 31 wells distributed among three transects of temporary, stainless-steel-screened, direct-push monitoring wells installed along three plumes of onsite wastewater. The transect network, by virtue of its design, also provided a basis for increased understanding of the transport of analytes in natural systems. Coliphage were frequently detected in onsite wastewater. Coliphage concentrations in onsite wastewater were highly variable, ranging from less than 1 to 3,000,000 plaque forming units per 100 milliliters. Coliphage were occasionally detected (eight occurrences) at low concentrations in samples from wells located downgradient from onsite wastewater treatment system drainfield lines. However, coliphage concentrations were below method detection limits in replicate or repeat samples collected from the eight sites. The consistent absence of coliphage detections in the replicate or repeat samples is interpreted to indicate that the detections reported for ground-water samples represented low-level field or laboratory contamination, and it would appear that coliphage were effectively attenuated to less than 1 PFU/100 mL over distances of several feet of transport in the La Pine aquifer and (or) overlying unsaturated zone. Organic wastewater compounds were frequently detected in onsite wastewater. Of the 63 organic wastewater compounds in the analytical schedule, 45 were detected in the 21 samples of onsite wastewater. Concentrations of organic wastewater compounds reached a maximum of 1,300 ug/L (p-cresol). Caffeine was detected at concentrations as high as 320 ug/L. Fourteen of the 45 compounds were detected in more than 90 percent of onsite wastewater samples. Fewer (nine) organic wastewater compounds were detected in ground water, despite the presence of nitrate and chloride likely from onsite wastewater sources. The nine organic wastewater compounds that were detected in ground-water samples were acetyl-hexamethyl-tetrahydro-naphthalene (AHTN), caffeine, cholesterol, hexahydrohexamethyl-cyclopentabenzopyran, N,N-diethyl-meta-toluamide (DEET), tetrachloroethene, tris (2-chloroethyl) phosphate, tris (dichloroisopropyl) phosphate, and tributyl phosphate. Frequent detection of household-chemical type organic wastewater compounds in onsite wastewater provides evidence that some of these organic wastewater compounds may be useful indicators of human waste effluent dispersal in some hydrologic environments. The occurrence of organic wastewater compounds in ground water downgradient from onsite wastewater treatment systems demonstrates that a subgroup of organic wastewater compounds is transported in the La Pine aquifer. The consistently low concentrations (generally less than 1 ug/L) of organic wastewater compounds in water samples collected from wells located no more than 19 feet from drainfield lines indicates that the reactivity (sorption, degradation) of this suite of organic waste.

Oregon↗

USGS2026

A simplified two-station approach for modeling metabolism in dam tailwaters subject to diel flow variation

Tailwaters are ubiquitous and highly managed ecosystems whose food webs often rely disproportionately on autochthonous energy. In situ continuous dissolved oxygen data are increasingly being used to estimate gross primary productivity and ecosystem respiration in rivers, but this approach is complicated in tailwaters, where upriver discontinuities (i.e., dams) violate commonly employed one-station approaches. In such cases, two-station metabolism models can be applied, although substantial diel variation in flow (a common outcome of hydropower production) requires more complex treatment of water parcel travel times. Here, we present a new two-station metabolism model that allows estimation of reach-scale gross primary productivity and ecosystem respiration in streams and rivers that experience within-day variation in flow. Our approach simplifies two-station variable flow model implementation compared to previous efforts. We apply our model to a 6-yr dissolved oxygen time series and use Bayesian inference to estimate daily gross primary productivity, ecosystem respiration, and gas exchange velocity ( k 600 ) for a ~12-km reach of the Colorado River downriver of Glen Canyon Dam. We compare our model's performance to a more mechanistically detailed and computationally intensive Eulerian dynamic flow model and also to a widely-used one-station model that uses assumptions of reach uniformity that are often strongly violated in tailwaters. These comparisons show that our metabolism estimates conform with output from the more detailed dynamic flow model and that the one-station approach deviates substantially from both two-station approaches. Our new stream metabolism model can help resolve a fundamental analytical impediment in tailwater ecology.

Arizona↗

USGS2002

Determination of fluorine in organic compounds: Microcombustion method

A reliable and widely applicable means of determining fluorine in organic compounds has long been needed. Increased interest in this field of research in recent years has intensified the need. Fluorine in organic combinations may be determined by combustion at 900° C. in a quartz tube with a platinum catalyst, followed by an acid-base titration of the combustion products. Certain necessary precautions and known limitations are discussed in some detail. Milligram samples suffice, and the accuracy of the method is about that usually associated with the other halogen determinations. Use of this method has facilitated the work upon organic fluorine compounds in this laboratory and it should prove to be equally valuable to others.

Analytical Chemistry↗

USGS1987

Analytically-derived sensitivities in one-dimensional models of solute transport in porous media

Analytically-derived sensitivities are presented for parameters in one-dimensional models of solute transport in porous media. Sensitivities were derived by direct differentiation of closed form solutions for each of the odel, and by a time integral method for two of the models. Models are based on the advection-dispersion equation and include adsorption and first-order chemical decay. Boundary conditions considered are: a constant step input of solute, constant flux input of solute, and exponentially decaying input of solute at the upstream boundary. A zero flux is assumed at the downstream boundary. Initial conditions include a constant and spatially varying distribution of solute. One model simulates the mixing of solute in an observation well from individual layers in a multilayer aquifer system. Computer programs produce output files compatible with graphics software in which sensitivities are plotted as a function of either time or space. (USGS)

Open-File Report↗

USGS2005

Handbook of capture-recapture analysis

Every day, biologists in parkas, raincoats, and rubber boots go into the field to capture and mark a variety of animal species. Back in the office, statisticians create analytical models for the field biologists' data. But many times, representatives of the two professions do not fully understand one another's roles. This book bridges this gap by helping biologists understand state-of-the-art statistical methods for analyzing capture-recapture data. In so doing, statisticians will also become more familiar with the design of field studies and with the real-life issues facing biologists. Reliable outcomes of capture-recapture studies are vital to answering key ecological questions. Is the population increasing or decreasing? Do more or fewer animals have a particular characteristic? In answering these questions, biologists cannot hope to capture and mark entire populations. And frequently, the populations change unpredictably during a study. Thus, increasingly sophisticated models have been employed to convert data into answers to ecological questions. This book, by experts in capture-recapture analysis, introduces the most up-to-date methods for data analysis while explaining the theory behind those methods. Thorough, concise, and portable, it will be immensely useful to biologists, biometricians, and statisticians, students in both fields, and anyone else engaged in the capture-recapture process.

Book↗

USGS2007

Seismoelectric imaging of shallow targets

We have undertaken a series of controlled field experiments to develop seismoelectric experimental methods for near-surface applications and to improve our understanding of seismoelectric phenomena. In a set of off-line geometry surveys (source separated from the receiver line), we place seismic sources and electrode array receivers on opposite sides of a man-made target (two sand-filled trenches) to record separately two previously documented seismoelectric modes: (1) the electromagnetic interface response signal created at the target and (2) the coseismic electric fields located within a compressional seismic wave. With the seismic source point in the center of a linear electrode array, we identify the previously undocumented seismoelectric direct field, and the Lorentz field of the metal hammer plate moving in the earth's magnetic field. We place the seismic source in the center of a circular array of electrodes (radial and circumferential orientations) to analyze the source-related direct and Lorentz fields and to establish that these fields can be understood in terms of simple analytical models. Using an off-line geometry, we create a multifold, 2D image of our trenches as dipping layers, and we also produce a complementary synthetic image through numerical modeling. These images demonstrate that off-line geometry (e.g., crosswell) surveys offer a particularly promising application of the seismoelectric method because they effectively separate the interface response signal from the (generally much stronger) coseismic and source-related fields. ?? 2007 Society of Exploration Geophysicists.

Geophysics↗

USGS2001

A bacterial method for the nitrogen isotopic analysis of nitrate in seawater and freshwater

We report a new method for measurement of the isotopic composition of nitrate (NO 3 - ) at the natural-abundance level in both seawater and freshwater. The method is based on the isotopic analysis of nitrous oxide (N 2 O) generated from nitrate by denitrifying bacteria that lack N 2 O-reductase activity. The isotopic composition of both nitrogen and oxygen from nitrate are accessible in this way. In this first of two companion manuscripts, we describe the basic protocol and results for the nitrogen isotopes. The precision of the method is better than 0.2‰ (1 SD) at concentrations of nitrate down to 1 μM, and the nitrogen isotopic differences among various standards and samples are accurately reproduced. For samples with 1 μM nitrate or more, the blank of the method is less than 10% of the signal size, and various approaches may reduce it further.

Analytical Chemistry↗

USGS2012

Digital Mapping Techniques '10-Workshop Proceedings, Sacramento, California, May 16-19, 2010

The Digital Mapping Techniques '10 (DMT'10) workshop was attended by 110 technical experts from 40 agencies, universities, and private companies, including representatives from 19 State geological surveys (see Appendix A). This workshop, hosted by the California Geological Survey, May 16-19, 2010, in Sacramento, California, was similar in nature to the previous 13 meetings (see Appendix B). The meeting was coordinated by the U.S. Geological Survey's (USGS) National Geologic Map Database project. As in the previous meetings, the objective was to foster informal discussion and exchange of technical information. It is with great pleasure that I note that the objective was again successfully met, as attendees continued to share and exchange knowledge and information, and renew friendships and collegial work begun at past DMT workshops. At this meeting, oral and poster presentations and special discussion sessions emphasized (1) methods for creating and publishing map products ("publishing" includes Web-based release); (2) field data capture software and techniques, including the use of LiDAR; (3) digital cartographic techniques; (4) migration of digital maps into ArcGIS Geodatabase format; (5) analytical GIS techniques; and (6) continued development of the National Geologic Map Database.

Open-File Report↗

USGS1999

Loch Vale Watershed Project quality assurance report, 1995-1998

The Loch Vale Watershed (LVWS) project was initiated in 1980 by the National Park Service with funding from the Aquatic Effects Research Program of the National Acid Precipitation Assessment Program. Initial research objectives were to understand the processes that would either mitigate or accelerate the effects of pollution on soil and surface water chemistry, and to build a record in which long-term trends could be identified and examined. It is important for all data collected in Loch Vale to meet the high standards of quality set forth in previous LVWS QA/QC reports and LVWS Methods Manuals. Given the ever-widening usage of data collected in Loch Vale, it is equally important to provide users of that data with a report assuring that all data are sound. Parameters covered in this report are the quality of meteorological measurements, hydrological measurements, surface water chemistry, and similarities in catch efficiency of two raingage types in Loch Vale for the period of 1995-1998. Routine sampling of weather conditions, precipitation chemistry, and stream/lake water chemistry began in 1982. Since then, all samples and data have been analyzed according to widely accepted and published methods. Weather data have been collected, analyzed, and stored by LVWS project personnel. Methods for the handling of meteorological data are well documented (Denning 1988, Edwards 1991, Newkirk 1995,and Allstott 1995). Precipitation chemistry has always been collected according to National Atmospheric Deposition Program protocol (Bigelow 1988), and analyzed at the Central Analytical Laboratory of the Illinois State Water Survey in Champaign, IL. QA/QC procedures of the National Atmospheric Deposition Program are well documented (Aubertin 1990). Protocols for sampling surface waters are also well documented (Newkirk 1995). Analysis of surface water chemistry has been performed using standard EPA protocol at the US Forest Service's Rocky Mt. Station Biogeochemistry Laboratory since 1993.

Open-File Report↗

USGS2002

Occurrence and transport of diazinon in the Sacramento River, California, and selected tributaries during three winter storms, January-February 2000

The organophosphate pesticide diazinon is applied as a dormant orchard spray in the Sacramento Valley, California, during the winter when the area receives a majority of its annual rainfall. Dormant spray pesticides, thus, have the potential to wash off the areas of application and migrate with storm runoff to streams in the Sacramento River Basin. Previous monitoring studies have shown that rain and associated runoff from winter storms plays an important role in the transport of diazinon from point of application to the Sacramento River and tributaries. Between January 30 and February 25, 2000, diazinon concentrations in the Sacramento River and selected tributaries were monitored on 5 consecutive days during each of three winter storms that moved through the Sacramento Valley after diazinon had been applied to orchards in the basin. Water samples were collected at 17 sites chosen to represent the effect of upstream land use at local and regional scales. Most samples were analyzed using an enzyme-linked immunosorbent assay (ELISA). Analysis by gas chromatography with electron capture detector and thermionic specific detector (GC/ECD/TSD) and gas chromatography with mass spectrometry (GC/MS) was done on split replicates from over 30 percent of the samples to confirm ELISA results and to provide lower analytical reporting limits at selected sites [30 ng/L (nanogram per liter) for ELISA, 20 ng/L for GC/ECD/TSD, and 2 ng/L for GC/MS]. Concentrations determined from ELISA analyses were consistently higher than concentrations for split samples analyzed by gas chromatography methods. Because of bias between diazinon concentrations using ELISA and gas chromatography methods, results from ELISA analyses were not compared to water-quality criteria. Load calculations using the ELISA analyses are similarly biased. Because the bias was consistent, however, the ELISA data is useful in site-to-site comparisons used to rank the relative levels and contributions of diazinon from individual subbasins in the watershed. Concentrations of diazinon in 138 samples analyzed by gas chromatography methods ranged from below detection (2 ng/L) to 2,890 ng/L with a median of 44 ng/L. Thirty percent of the samples had concentrations greater than 80 ng/L, which is considered by California as the criterion maximum concentration for the protection of aquatic habitat. Concentrations were highest in small tributaries and canals draining subbasins with predominantly agricultural land use and in a channel draining the Yuba City urban area. Load estimates using concentrations derived from GC/MS analyses indicate that about 30 percent of the diazinon in the lower Sacramento River is from the Feather River Basin. Loads estimated using ELISA analyses show a similar, but slightly higher fraction of the total load coming from that basin. The source of over half the total load measured at Sacramento River at Alamar appears to have originated in the part of the drainage basin upstream of the city of Colusa. Of the diazinon reported applied to agricultural land in Sacramento Valley (about 42,500 pounds active ingredient) just before and during the monitoring period, about 0.4 percent appeared to be transported to the lower Sacramento River during the period of monitoring. A similar percent of applied diazinon was estimated to have entered the Feather River from upstream sources. Diazinon use in the study area during the 1999-2000 dormant spray season was unusually low, about 60 percent of the average of the previous 4 years. Therefore, diazinon loadings may be higher in subsequent years, should use increase and pesticide management practices remain the same. Although diazinon was the most frequently detected pesticide and the pesticide detected at the highest concentrations, 10 other pesticides were detected in the samples collected. These included the insecticides methidathion and chlorpyrifos, and the herbicides simazine, molinate and thiobencarb.

California↗

USGS2025

Revealing organofluorine contamination in effluents and surface waters with complementary analytical approaches: Fluorine-19 nuclear magnetic resonance spectroscopy (19F-NMR) and liquid chromatography-tandem mass spectrometry (LC-MS/MS)

Fluorinated organic contaminants, including per- and polyfluoroalkyl substances (PFASs) and fluorinated pesticides and pharmaceuticals (FPPs), pose a persistent threat to environmental health. Widely used liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods fail to capture large fractions of total organofluorine in environmental samples, confounding the assessment of fluorinated contamination. Fluorine-19 nuclear magnetic resonance spectroscopy ( 19 F-NMR) is an inclusive method for total and class-based organofluorine analysis. Here, we apply 19 F-NMR to 31 effluent, surface water, and foam samples collected at 13 potential organofluorine point sources or source regions and compare the results to targeted LC-MS/MS for 34 or 64 PFASs. LC-MS/MS detected a median of 11.4% of total organofluorine detected by 19 F-NMR (range: nondetect to 8190 nM F 19 F-NMR; nondetect to 8010 nM F LC-MS/MS). The highest 19 F-NMR total organofluorine concentrations, detected in wastewater treatment plant (WWTP)-associated foam and at a soy oil production facility, arose from resonances characteristic of per- and polyfluorinated alkyl chains. 19 F-NMR resonances from aryl CF 3 moieties were abundant in the WWTP-associated samples, consistent with prior reports of substantial contributions from pharmaceuticals to WWTP effluents. 19 F-NMR enables the quantitative assessment of total organofluorine and qualitative insight into fluorinated structures, providing complementary analysis of organofluorine compounds missed by targeted mass spectrometry-based protocols.

Environmental Science & Technology↗