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U.S. Geological Survey Standard Reference Sample Project: Performance Evaluation of Analytical Laboratories

Since 1962, the U.S. Geological Survey (USGS) has operated the Standard Reference Sample Project to evaluate the performance of USGS, cooperator, and contractor analytical laboratories that analyze chemical constituents of environmental samples. The laboratories are evaluated by using performance evaluation samples, called Standard Reference Samples (SRSs). SRSs are submitted to laboratories semi-annually for round-robin laboratory performance comparison purposes. Currently, approximately 100 laboratories are evaluated for their analytical performance on six SRSs for inorganic and nutrient constituents. As part of the SRS Project, a surplus of homogeneous, stable SRSs is maintained for purchase by USGS offices and participating laboratories for use in continuing quality-assurance and quality-control activities. Statistical evaluation of the laboratories results provides information to compare the analytical performance of the laboratories and to determine possible analytical deficiences and problems. SRS results also provide information on the bias and variability of different analytical methods used in the SRS analyses.

Fact Sheet

Water-quality monitoring of Sweetwater Reservoir

Sweetwater Authority is concerned with the quality of water it provides to its customers. Results from the water-quality monitoring study that the USGS is conducting in the Sweetwater watershed show that the contaminant concentrations in bed sediments, water, and air are reflected in increased urbanization. The bed sediments show the most dramatic evidence of this impact with a sharp increase of persistent organic chemical concentrations over the past 65 years. Water quality is also affected by urbanization in the form of chemicals in the runoff water and deposition of airborne chemicals. The concentrations of the detected organic chemicals in Sweetwater and Loveland Reservoirs are all well below the guidance limits set by State and Federal agencies to protect human health. Many of these compounds are detected only because of the sensitive analytical methods used. This monitoring program provides the Sweetwater Authority with information on what monitored chemicals are present in the reservoirs, and at what concentrations. With this information, the Authority can assess the associated risks, and consider future water treatment and remediation. These results also help focus and support future efforts by Sweetwater Authority to protect the watershed.

Fact Sheet

Reconstructing historical changes in the environmental health of watersheds by using sediment cores from lakes and reservoirs in Salt Lake Valley, Utah

The Great Salt Lake Basins study area of the National Water-Quality Assessment (NAWQA) program, which began in 1997, is increasing the scientific understanding of factors that affect surface-water quality within the study-area boundaries (fig. 1). One way to improve the understanding of these factors is to look at historical trends in existing water-quality data. Unfortunately, short record lengths, in- consistent analytical methods, numerous measurements at less than detection levels, and questionable accuracy limit the usefulness of historical monitoring data for most trace inorganic and organic contaminants found in streams, rivers, and lakes in the study area.

Idaho, Utah, Wyoming

The Stanford-U.S. Geological Survey SHRIMP ion microprobe--a tool for micro-scale chemical and isotopic analysis

Answers to many questions in Earth science require chemical analysis of minute volumes of minerals, volcanic glass, or biological materials. Secondary Ion Mass Spectrometry (SIMS) is an extremely sensitive analytical method in which a 5–30 micrometer diameter "primary" beam of charged particles (ions) is focused on a region of a solid specimen to sputter secondary ions from 1–5 nanograms of the sample under high vacuum. The elemental abundances and isotopic ratios of these secondary ions are determined with a mass spectrometer. These results can be used for geochronology to determine the age of a region within a crystal thousands to billions of years old or to precisely measure trace abundances of chemical elements at concentrations as low as parts per billion. A partnership of the U.S. Geological Survey and the Stanford University School of Earth Sciences operates a large SIMS instrument, the Sensitive High-Resolution Ion Microprobe with Reverse Geometry (SHRIMP–RG) on the Stanford campus.

Fact Sheet

Chemist postcard

Chemists design analytical methods, analyze samples, and review instrument results to ensure high-quality, defensible data are provided to our Nation’s decision makers. For more information, visit https://www.usajobs.gov .

General Information Product

Regional geochemical maps of the Tonopah 1 degree by 2 degrees Quadrangle, Nevada, based on samples of stream sediment and nonmagnetic heavy-mineral concentrate

This report is part of a series of geologic, geochemical, and geophysical maps of the Tonopah 1° x 2° quadrangle, Nevada, prepared during studies of the area for the Conterminous United States Mineral Assessment Program (CUSMAP). Included here are 21 maps showing the distributions of selected elements or combinations of elements. These regional geochemical maps are based on chemical analyses of the minus-60 mesh (0.25 mm) fraction of stream-sediment samples and the nonmagnetic heavy-mineral concentrate derived from stream sediment. Stream sediments were collected at 1,217 sites. Our geochemical studies of mineralized rock samples provide a framework for evaluating the results from stream sediments. The Tonopah 1° x 2° quadrangle comprises about 19,100 km 2 (7,450 mi 2 ) in west-central Nevada (fig. 1). Topography is typical of the Basin and Range province, consisting of angular mountain ranges separated by broad valleys that comprise about half the area. Topographic relief is generally about 1,000 m but in some places is more than 1,500 m. Most of the ranges have well-developed drainages in steep-walled canyons occupied by intermittent streams. The climate is semi-arid to arid. Pinon pine and juniper grow in most places at elevations above 2,100 m, and sagebrush is abundant at lower elevations. Major access is provided by U.S. Routes 6 and 95, and there are numerous county maintained gravel roads and unmaintained jeep trails. Bedrock geology of the Tonopah quadrangle is a complex mosaic of late Precambrian to Tertiary rocks juxtaposed by numerous thrust and high-angle faults. Useful geologic summaries can be found in reports by Ross (1961), Albers and Stewart (1972), Stewart and Carlson (1978), and Kleinhampl and Ziony (1985). Mineral prospects and mines occur in igneous, metamorphic, and sedimentary rocks of all ages, and mines are particularly abundant in the central and western parts of the quadrangle. The complex geology produces clasts of mixed lithology in alluvium in all drainage basins sampled in this study, and the numerous mines and prospects probably contaminate many drainages. The geochemical maps in this report are based on analytical results reported by Fairfield and others (1985), Hill and others (1986), and Siems and others (1986). These reports also describe the sample preparation and analytical methods and provide information on the location of the sample sites.

Nevada

Water-quality and water-level data for a freshwater tidal wetland, West Branch Canal Creek, Aberdeen Proving Ground, Maryland, October 1998-September 1999

This report presents water-quality data for ground-water and surface-water samples and water-level data collected by the U.S. Geological Survey from October 1998 through September 1999 at West Branch Canal Creek, Aberdeen Proving Ground, Maryland. The report also provides a description of the sampling and analytical methods that were used to collect and analyze the samples, and includes an evaluation of the quality-assurance data. The ground-water sampling network includes 88 wells or piezometers, including four 2-inch wells, two 4-inch wells, thirty 0.75-inch piezo-meters, and fifty-two 0.25-inch piezometers. Water levels were measured in 105 wells or piezometers. Surface-water samples were collected at five sites. Samples were collected from wells and 0.75-inch piezometers for measurement of field parameters, and analysis of inorganic and organic constituents during three sampling rounds: March, May through June, and July through August of 1999. Inorganic constituents and organic constituents were analyzed in samples collected from 0.25-inch piezometers during three sampling rounds in February through March, May, and September of 1999. Water levels were measured in October and November of 1998, and in February and May of 1999. Surface-water samples were collected between February and August of 1999 for analysis of organic constituents.

Open-File Report

Water quality monitoring of Sweetwater and Loveland reservoirs--Phase one results 1998-1999

In 1998, the U.S. Geological Survey began a study to assess the overall health of the watershed feeding the Sweetwater Reservoir in southern San Diego County, California. The study focussed on monitoring for organic chemical contamination and the effects of construction and operation of State Route 125 on water quality. Three environmental compartments (air, water, and bed sediments) are being sampled regularly for chemical contaminants, including volatile organic compounds, polynuclear aromatic hydrocarbons, polychlorinated biphenyls, pesticides, and major and trace elements. The study is divided into two phases. Phase I sampling is designed to establish baseline conditions for target compounds in terms of detection frequency and concentration in air, water, and bed sediments. Phase II sampling will continue at the established monitoring sites during and after construction of State Route 125 to assess chemical impact on water quality in the reservoir resulting from land-use changes and development in the watershed. This report describes the study design, the sampling and analytical methods, and presents the data results for the first year of the study, September 1998 to September 1999.

Open-File Report

Processing and interpretation of aeromagnetic data for the Santa Cruz Basin–Patagonia Mountains area, south-central Arizona

In 1997, the U.S. Geological Survey (USGS) contracted with Sial Geosciences Inc. for a detailed aeromagnetic survey of the Santa Cruz basin and Patagonia Mountains area of south-central Arizona. The contractor's Operational Report is included as an Appendix in this report. This section describes the data processing performed by the USGS on the digital aeromagnetic data received from the contractor. This processing was required in order to remove flight line noise, estimate the depths to the magnetic sources, and estimate the locations of the magnetic contacts. Three methods were used for estimating source depths and contact locations: the horizontal gradient method, the analytic signal method, and the local wavenumber method. The depth estimates resulting from each method are compared, and the contact locations are combined into an interpretative map showing the dip direction for some contacts.

Arizona

Results of analyses of the fungicide Chlorothalonil, its degradation products, and other selected pesticides at 22 surface-water sites in five Southern states, 2003-04

In accordance with the mission of the U.S. Geological Survey (USGS) Toxic Substances Hydrology Program, a pesticide study was conducted during 2003–04 to determine the occurrence of the fungicide chlorothalonil and its degradation products at 22 surface-water sites in five Southern States. Water-quality samples were collected during the peanut-growing season (June–September) in 2003. During the peanut-growing season in 2004, samples were collected after large storms. An analytical method was developed at the USGS Organic Geochemistry Research Laboratory in Lawrence, Kansas, to measure chlorothalonil and its degradation products by liquid chromatography/mass spectrometry (LC/MS). Chlorothalonil was detected in 4 of the 113 surface-water samples. The primary degradation product of chlorothalonil, 4-hydroxy-chlorothalonil, was detected in 26 of the 113 samples with concentrations ranging from 0.002 to 0.930 microgram per liter. The chlorothalonil degradation products, 1-amide-4-hydroxy-chorothalonil and 1,3-diamide-chlorothalonil, were detected in one water sample each at 0.020 and 0.161 microgram per liter, respectively. The USGS Methods and Research Development Group, Lakewood, Colorado, developed a custom method for chlorothalonil using gas chromatography/mass spectrometry (GC/MS) in an effort to achieve a lower laboratory reporting level (LRL) than the USGS National Water-Quality Laboratory (NWQL) schedule 2060, which analyzes the compound chlorothalonil at a LRL of 0.035 µg/L. The group succeeded in achieving a lower GC/MS reporting level of 0.01 µg/L. Chlorothalonil was detected in 5 of 68 water samples analyzed using the custom GC/MS method, whereas chlorothalonil was detected in 2 of 21 water samples analyzed using NWQL schedule 2060. In addition to analysis of chlorothalonil and its degradation products, samples were analyzed using the USGS NWQL schedules 2001 and 2060 for about 114 pesticides and their degradation products. Samples also were analyzed for dissolved organic carbon, suspended sediment, and percentage of silt- and clay-sized particles. Overall, it was found that chlorothalonil was detected only infrequently and at relatively low concentrations. Chlorothalonil’s major degradation product, 4-hydroxy-chlorothalonil, was detected most frequently, occurred generally at higher concentrations in water samples than did the parent fungicide, and the data from this study reaffirmed that it is the dominant degradation product of chlorothalonil in the peanut-growing environment.

Open-File Report

Aqueous geochemical data from the analysis of stream-water samples collected in June and July 2005 — Taylor Mountains 1:250,000 scale quadrangle, Alaska

We report on the chemical analysis of water samples collected from the Taylor Mountains 1:250,000-scale quadrangle. Parameters for which data are reported include pH, conductivity, water temperature, major cation and anion concentrations, trace-element concentrations, and dissolved organic-carbon concentrations. Samples were collected as part of a multiyear U.S. Geological Survey project "Geologic and Mineral Deposit Data for Alaskan Economic Development." Data presented here are from samples collected in June and July of 2005. The data are being released at this time with minimal interpretation. This is the second release of aqueous geochemical data from this project; 2004 aqueous geochemical data were published previously ( Wang and others, 2006 ). The data in this report augment but do not duplicate or supersede the previous data release. Site selection was based on a regional sampling strategy that focused on first- and second-order drainages. Water sample site selection was based on landscape parameters that included physiography, wetland extent, lithological changes, and a cursory field review of mineralogy from pan concentrates. Stream water in the Taylor Mountians quadrangle is dominated by bicarbonate (HCO 3- ), though in a few samples more than 50 percent of the anionic charge can be attributed to sulfate (SO 4 2- ). The major-cation chemistry ranges from Ca 2+ /Mg 2+ dominated to a mix of Ca 2+ /Mg 2+ /Na + +K + . In general, good agreement was found between the major cations and anions in the duplicate samples. Many trace elements in these samples were at or near the analytical method detection limit, but good agreement was found between duplicate samples for elements with detectable concentrations. With the exception of a total mercury concentration of 0.33 ng/L detected in a field blank, field blank major-ion and trace-elements concentrations were below detection.

Alaska

Phosphorus Concentrations in Stream-Water and Reference Samples - An Assessment of Laboratory Comparability

In 2003, a study was conducted to evaluate the accuracy and precision of 10 laboratories that analyze water-quality samples for phosphorus concentrations in the Catskill Mountain region of New York State. Many environmental studies in this region rely on data from these different laboratories for water-quality analyses, and the data may be used in watershed modeling and management decisions. Therefore, it is important to determine whether the data reported by these laboratories are of comparable accuracy and precision. Each laboratory was sent 12 samples for triplicate analysis for total phosphorus, total dissolved phosphorus, and soluble reactive phosphorus. Eight of these laboratories reported results that met comparability criteria for all samples; the remaining two laboratories met comparability criteria for only about half of the analyses. Neither the analytical method used nor the sample concentration ranges appeared to affect the comparability of results. The laboratories whose results were comparable gave consistently comparable results throughout the concentration range analyzed, and the differences among methods did not diminish comparability. All laboratories had high data precision as indicated by sample triplicate results. In addition, the laboratories consistently reported total phosphorus values greater than total dissolved phosphorus values, and total dissolved phosphorus values greater than soluble reactive phosphorus values, as would be expected. The results of this study emphasize the importance of regular laboratory participation in sample-exchange programs.

Open-File Report

Preliminary analytical results for ash and burned soils from the October 2007 southern California wildfires

The U.S. Geological Survey (USGS) collected ash and burned soils from about 28 sites in southern California wildfire areas (Harris, Witch, Ammo, Santiago, Canyon and Grass Valley) from Nov. 2 through 9, 2007 (table 1). USGS researchers are applying a wide variety of analytical methods to these samples, with the goal of helping identify characteristics of the ash and soils from wildland and suburban burned areas that may be of concern for their potential to adversely affect water quality, human health, endangered species, and debris-flow or flooding hazards. These studies are part of the Southern California Multi-Hazards Demonstration Project, and preliminary findings are presented here.

Open-File Report

Simulation of Flow Regimes to Reduce Habitat for T. tubifex

Whirling disease has had a significant impact on trout fisheries of the American west by reducing the numbers and quality of rainbow trout in infected streams. A critical factor in the life cycle of the whirling disease parasite is the fine sediment that provides the optimum habitat for Tubifex tubifex, an oligochaete worm that acts as an intermediate host for the disease. This report presents a model for the simulation of flushing flows required to remove undesirable fines and sand from a pool. Undesirable fines may also need to be flushed from runs, the surface layer, and backwater areas. Well-defined links of specific particle sizes to oligochaete worm abundance is needed to justify the use of flushing flows to move sediment. An analytical method for estimating the streamflows needed to remove the fine sediment is demonstrated herein. The overall steps to follow in removing fines from a stream are: Step 1. Determine size of the sediment that is the habitat for oligochaete worms. Step 2. Determine location of the sediment that is the habitat for oligochaete worms. Step 3. Determine streamflows needed to flush (remove) the sediment that is the habitat for oligochaete worms. The case study approach is used to present the method and to demonstrate its application. The case is derived from the sediment and oligochaete worm habitat of Willow Creek, a tributary of the Upper Colorado River located in Grand County, Colo. Willow Creek Reservoir (an element of the Colorado-Big Thompson Project) controls the streamflows of the creek and is just above the study site.

Open-File Report

Klamath River Water Quality and Acoustic Doppler Current Profiler Data from Link River Dam to Keno Dam, 2007

In 2007, the U.S. Geological Survey, Watercourse Engineering, and the Bureau of Reclamation began a project to construct and calibrate a water quality and hydrodynamic model of the 21-mile reach of the Klamath River from Link River Dam to Keno Dam. To provide a basis for this work, data collection and experimental work were planned for 2007 and 2008. This report documents sampling and analytical methods and presents data from the first year of work. To determine water velocities and discharge, a series of cross-sectional acoustic Doppler current profiler (ADCP) measurements were made on the mainstem and four canals on May 30 and September 19, 2007. Water quality was sampled weekly at five mainstem sites and five tributaries from early April through early November, 2007. Constituents reported here include field parameters (water temperature, pH, dissolved oxygen concentration, specific conductance); total nitrogen and phosphorus; particulate carbon and nitrogen; filtered orthophosphate, nitrite, nitrite plus nitrate, ammonia, organic carbon, iron, silica, and alkalinity; specific UV absorbance at 254 nm; phytoplankton and zooplankton enumeration and species identification; and bacterial abundance and morphological subgroups. The ADCP measurements conducted in good weather conditions in May showed that four major canals accounted for most changes in discharge along the mainstem on that day. Direction of velocity at measured locations was fairly homogeneous across the channel, while velocities were generally lowest near the bottom, and highest near surface, ranging from 0.0 to 0.8 ft/s. Measurements in September, made in windy conditions, raised questions about the effect of wind on flow. Most nutrient and carbon concentrations were lowest in spring, increased and remained elevated in summer, and decreased in fall. Dissolved nitrite plus nitrate and nitrite had a different seasonal cycle and were below detection or at low concentration in summer. Many nutrient and carbon concentrations were similar at the top and bottom of the water column, though ammonia and particulate carbon showed more variability in summer. Averaged over the season, particulate carbon and particulate nitrogen decreased in the downstream direction, while ammonia and orthophosphate concentrations increased in the downstream direction. At most sites, bacteria, phytoplankton, and zooplankton populations reached their maximums in summer. Large bacterial cells made up most of the bacteria biovolume, though cocci were the most numerous bacteria type. The cocci were smaller than the filter pore sizes used to separate dissolved from particulate matter in this study. Phytoplankton biovolumes were dominated by the blue-green alga Aphanizomenon flos-aquae most of the sampling season, though a spring diatom bloom occurred. Phytoplankton biovolumes were generally highest at the upstream Link River and Railroad Bridge sites and decreased in the downstream direction. Zooplankton populations were dominated by copepods in early spring, and by cladocerans and rotifers in summer, with rotifers more common farther downstream.

Open-File Report

Simultaneous Speciation of Arsenic, Selenium, and Chromium by HPLC-ICP-MS

An adaptation of an analytical method developed for chromium speciation has been utilized for the simultaneous determination of As(III), As(V), Se(IV), Se(VI), Cr(III), and Cr(VI) species using high performance liquid chromatography (HPLC) separation with ICP-MS detection. Reduction of interferences for the determination of As, Se, and Cr by ICP-MS is a major consideration for this method. Toward this end, a Dynamic Reaction Cell (DRC) ICP-MS system was used to detect the species eluted from the chromatographic column. A variety of reaction cell gases and conditions may be utilized, and the advantages and limitations of the gases tested to date will be presented and discussed. The separation and detection of the As, Se, and Cr species of interest can be achieved using the same chromatographic conditions in less than 2 minutes by complexing the Cr(III) with EDTA prior to injection on the HPLC column. Practical aspects of simultaneous speciation analysis will be presented and discussed, including issues with HPLC sample vial contamination, standard and sample contamination, species stability, and considerations regarding sample collection and preservation methods. The results of testing to determine the method's robustness to common concomitant element and anion effects will also be discussed. Finally, results will be presented using the method for the analysis of a variety of environmental and geological samples including waters, soil leachates and simulated bio-fluid leachates.

Open-File Report

Geochemical data from analyses of rock, sediment, water, and solid-phase leaching at the Tuba City Open Dump, Tuba City, Arizona

This report releases data collected by the U.S. Geological Survey from the Tuba City Open Dump area from January 2008 to September 2008 with cooperation from the U.S. Bureau of Indian Affairs and the Navajo and Hopi Tribes. These data were collected in support of investigations into the possible sources and resulting transport of radionuclides and other dissolved constituents in the surrounding ground water from the Tuba City Open Dump. This report provides a discussion of data collection and analytical methods with the data in a tabular format.

Arizona

Occurrence of Selected Pharmaceutical and Organic Wastewater Compounds in Effluent and Water Samples from Municipal Wastewater and Drinking-Water Treatment Facilities in the Tar and Cape Fear River Basins, North Carolina, 2003-2005

Samples of treated effluent and treated and untreated water were collected at 20 municipal wastewater and drinkingwater treatment facilities in the Tar and Cape Fear River basins of North Carolina during 2003 and 2005. The samples were analyzed for a variety of prescription and nonprescription pharmaceutical compounds and a suite of organic compounds considered indicative of wastewater. Concentrations of these compounds generally were less than or near the detection limits of the analytical methods used during this investigation. None of these compounds were detected at concentrations that exceeded drinking-water standards established by the U.S. Environmental Protection Agency. Bromoform, a disinfection byproduct, was the only compound detected at a concentration that exceeded regulatory guidelines. The concentration of bromoform in one finished drinking-water sample, 26 micrograms per liter, exceeded North Carolina water-quality criteria. Drinking-water treatment practices were effective at removing many of the compounds detected in untreated water. Disinfection processes used in wastewater treatment - chlorination or irradiation with ultraviolet light - did not seem to substantially degrade the organic compounds evaluated during this study.

North Carolina