Search USGS⌕ Search

SEARCH · Search USGS

Results for “Analytical Chemistry”

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

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

At least 217 records · Page 12Linked to original sources
USGS2006

Use of field-applied quality control samples to monitor performance of a Goulden large-sample extractor/GC-MS method for pesticides in water

Since 1985, the Goulden large-sample extractor (GLSE) has been used to isolate a broad array of trace-organic contaminants from large volumes of water. In this study, field-applied quality control measures, including matrix and surrogate spikes and blanks, were used to monitor method performance from GLSE extraction through GC-MS analysis. The method was applied to the determination of multiple classes of pesticides isolated from 4- to 112-L filtered surface-water samples. Average recoveries of six surrogate compounds ranged from 84 ?? 18% for [2H10]diazinon to 15 ?? 13% for 4,4'-[2H8]DDT, the low recoveries for which were largely a result of unmonitored breakdown of this surrogate by the GC injection system. Field-matrix-spike samples were prepared by fortifying 10-L, 35-L, and 110-L filtered surface-water samples with 68 pesticides to amended concentrations of 11- to 50-ng/L each. Recoveries ranged from not detected to greater than 100%. Variability in pesticide recoveries from triplicate 10-L water samples collected at one site averaged 5.7% relative standard deviation and did not exceed 19%.Since 1985, the Goulden large-sample extractor (GLSE) has been used to isolate a broad array of trace-organic contaminants from large volumes of water. In this study, field-applied quality control measures, including matrix and surrogate spikes and blanks, were used to monitor method performance from GLSE extraction through GC-MS analysis. The method was applied to the determination of multiple classes of pesticides isolated from 4- to 112-L filtered surface-water samples. Average recoveries of six surrogate compounds ranged from 84 ?? 18% for [2H10]diazinon to 15 ?? 13% for 4,4???-[2H8]DDT, the low recoveries for which were largely a result of unmonitored breakdown of this surrogate by the GC injection system. Field-matrix-spike samples were prepared by fortifying 10-L, 35-L, and 110-L filtered surface-water samples with 68 pesticides to amended concentrations of 11- to 50-ng/L each. Recoveries ranged from not detected to greater than 100%. Variability in pesticide recoveries from triplicate 10-L water samples collected at one site averaged 5.7% relative standard deviation and did not exceed 19%.

International Journal of Environmental Analytical ↗
USGS2001

Regional water-quality analysis of 2,4-D and dicamba in river water using gas chromatography-isotope dilution mass spectrometry

Gas chromatography with isotope dilution mass spectrometry (GC-MS) and enzyme-linked immunosorbent assay (ELISA) were used in regional National Water Quality Assessment studies of the herbicides, 2,4-D and dicamba, in river water across the United States. The GC-MS method involved solid-phase extraction, derivatized with deuterated 2,4-D, and analysis by selected ion monitoring. The ELISA method was applied after preconcentration with solid-phase extraction. The ELISA method was unreliable because of interference from humic substances that were also isolated by solid-phase extraction. Therefore, GC-MS was used to analyzed 80 samples from river water from 14 basins. The frequency of detection of dicamba (28%) was higher than that for 2,4-D (16%). Concentrations were higher for dicamba than for 2,4-D, ranging from less than the detection limit (7lt; 0.05 μg/L) to 3.77μg/L, in spite of 5 times more annual use of 2,4-D as compared to dicamba. These results suggest that 2,4-D degrades more rapidly in the environment than dicamba.

International Journal of Environmental Analytical ↗
USGS2005

Occurrence of antibiotics in water from 13 fish hatcheries, 2001-2003

A 2-year study of extensive and intensive fish hatcheries was conducted to assess the general temporal occurrence of antibiotics in aquaculture. Antibiotics were detected in 15% of the water samples collected during the 2001-2002 collection period and in 31% of the samples during the 2003 collection period. Antibiotics were detected more frequently in samples from the intensive hatcheries (17 and 39%) than in samples from the extensive hatcheries (14 and 4%) during the 2001-2002 and 2003 collection periods, respectively. The maximum ormetoprim, oxytetracycline, and sulphadimethoxine concentrations were higher in samples from the intensive hatcheries (12, 10, and 36 &micro;g L-1), respectively, than in samples from the extensive hatcheries (<0.05, 0.31, and 1.2 &micro;g L-1), respectively. Sulphadimethoxine persisted for a longer period of time (up to 48 days) than ormetoprim (up to 28 days) and oxytetracycline (less than 20 days).

International Journal of Environmental Analytical ↗
USGS2007

Input, flux, and persistence of six select pesticides in San Francisco Bay

Temporal patterns of pesticide inputs to San Francisco Bay were identified and correlated with timing of application and transport mechanism. Fluxes were calculated from measured concentrations and estimated flow. Persistence of the pesticides under typical riverine or estuarine conditions were estimated from laboratory experiments. Simazine was detected most frequently and had the highest flux into the Bay, which could be explained by its continuous use and long half-life. In comparison, diazinon was detected at lower concentrations and had a lower flux which corresponded to its lower use and shorter half-life. The order-of-magnitude lower fluxes of carbofuran and methidathion corresponded to their lower use and expected hydrolysis. Molinate was detected at the highest concentration but its flux was lower than expected, considering its very high use and persistence in the laboratory experiments. Additional loss of molinate is likely to occur from volatilization and photodegradation on the rice fields. Although thiobencarb had the second highest use, it had the lowest flux of the six pesticides, which can be attributed to its loss via hydrolysis, photodegradation, volatilization, and sorption to sediments. Fluxes into San Francisco Bay were equal to or greater than those reported for other estuaries, except for the Gulf of Mexico.

California↗
USGS2007

Use of a watershed model to characterize the fate and transport of fluometuron, a soil-applied cotton herbicide, in surface water

The Soil and Water Assessment Tool (SWAT) was used to characterize the fate and transport of fluometuron (a herbicide used on cotton) in the Bogue Phalia Basin in northwestern Mississippi, USA. SWAT is a basin-scale watershed model, able to simulate hydrological, chemical, and sediment transport processes. After adjustments to a few parameters (specifically the SURLAG variable, the runoff curve number, Manning's N for overland flow, soil available water capacity, and the base-flow alpha factor) the SWAT model fit the observed streamflow well (the Coefficient of Efficiency and R2 were greater than 60). The results from comparing observed fluometuron concentrations with simulated concentrations were reasonable. The simulated concentrations (which were daily averages) followed the pattern of observed concentrations (instantaneous values) closely, but could be off in magnitude at times. Further calibration might have improved the fit, but given the uncertainties in the input data, it was not clear that any improvement would be due to a better understanding of the input variables. ?? 2007 Taylor & Francis.

International Journal of Environmental Analytical ↗
USGS2007

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

A multi-residue method is described for the determination o triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 μg/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

International Journal of Environmental Analytical ↗
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 &mu;g/L. At a concentration of 1 &mu;g/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 ↗
USGS1996

The deethylatrazine/atrazine ratio as an indicator of the onset of the spring flush of herbicides into surface water of the Midwestern United States

The ratio of deethylatrazine to atrazine (DAR) may be used to record the first major runoff of herbicides from non-point-source corn fields to surface water in the Midwestern United States. The DAR dramatically decreases from ∼0.5 to < 0.1 upon application of herbicide and the first major runoff event of a basin. The DAR then gradually increases to values of approximately 0.4–0.6 during the harvest season. Furthermore, the DAR may be used in studies of surface water movement to give a temporal indicator of water moving into reservoirs for possible storage of herbicides. It is hypothesized that deethylatrazine, which accounts for only 6% of the degradation of atrazine, becomes a significant metabolite in surface water (∼ 50% of parent compound) because of its selective removal from soil. This removal process may be an important concept for consideration in studies of herbicide contamination of rivers and reservoirs.

International Journal of Environmental Analytical ↗
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↗
USGS1992

A critical review of inductively coupled plasma-mass spectrometry for geoanalysis, geochemistry and hydrology, Part 1. Analytical performance

Present-day inductively coupled plasma-mass spectrometry (ICP-MS) instrumentation is described briefly. Emphasis is placed on performance characteristics for geoanalysis, geochemistry, and hydrology. Applications where ICP-MS would be indispensable are indicated. Determination of geochemically diagnostic trace elements (such as the rare earth elements [REE], U and Th), of isotope ratios for fingerprinting, tracer and other geo-isotope applications, and benchmark isotope dilution determinations are considered to be typical priority applications for ICP-MS. It is concluded that ICP-MS furnishes unique geoanalytical and environmental data that are not readily provided by conventional spectroscopic (emission and absorption) techniques.

Critical Reviews in Analytical Chemistry↗
USGS2013

Normalized rare earth elements in water, sediments, and wine: identifying sources and environmental redox conditions

The concentrations of the rare earth elements (REE) in surface waters and sediments, when normalized on an element-by-element basis to one of several rock standards and plotted versus atomic number, yield curves that reveal their partitioning between different sediment fractions and the sources of those fractions, for example, between terrestrial-derived lithogenous debris and seawater-derived biogenous detritus and hydrogenous metal oxides. The REE of ancient sediments support their partitioning into these same fractions and further contribute to the identification of the redox geochemistry of the sea water in which the sediments accumulated. The normalized curves of the REE that have been examined in several South American wine varietals can be interpreted to reflect the lithology of the bedrock on which the vines may have been grown, suggesting limited fractionation during soil development.

American Journal of Analytical Chemistry↗
USGS1954

Polarographic determination of tungsten in rocks

This work was undertaken to develop a simpler and faster method than the classical gravimetric procedure for the determination of tungsten in rocks and ores. A new polarographic wave of tungsten is obtained in a supporting electrolyte of dilute hydrochloric acid containing tartrate ion. This permits the determination of tungsten both rapidly and accurately. No precipitation of the tungsten is necessary, and only the iron need be separated from the tungsten. The accuracy is within the limits of a polarographic procedure; comparison of polarographic and gravimetric results is given. The method reduces appreciably the amount of time ordinarily consumed in determination of tungsten.

Analytical Chemistry↗
USGS1954

Tables for evaluating Bateman equation coefficients for radioactivity calculations

Tables of decay constants and functions thereof are presented to simplify the problem of calculating the constants involved in the Bateman equation. These tables make it possible to calculate any constant involved in any of the four radioactive series by a maximum of three mathematical operations, either by three divisions or by two multiplications and a division. They are useful and time-saving where a large number of such calculations are involved.

Analytical Chemistry↗
USGS1955

Rapid determination of carbon dioxide in silicate rocks

In the development of rapid methods for silicate rock analysis, a simpler and faster means was needed for the determination of carbon dioxide than the conventional "train" procedures. With the method presented here, which involves measurement of the volume of carbon dioxide evolved, the time required for a determination is about 5 minutes per sample. It provides a saving of 30 to 40 minutes for each determination without significant loss of accuracy.

Analytical Chemistry↗
USGS1955

Determination of small and large amounts of fluorine in rocks

Gelatinous silica and aluminum ions retard the distillation of fluorine in the Willard and Winter distillation method. A generally applicable, simple method for the determination of fluorine in rocks containing aluminum or silicon or both as major constituents was desired. In the procedure developed, the sample is fused with a mixture of sodium carbonate and zinc oxide, leached with water, and filtered. The residue is granular and retains nearly all of the silica. The fluorine in the filtrate is distilled directly from a perchloric acid-phosphoric acid mixture. Phosphoric acid permits the quantitative distillation of fluorine in the presence of much aluminum at the usual distillation temperature and without the collection of large volumes of distillate. The fluorine is determined either by microtitration with thorium nitrate or colorimetrically with thoron. The procedure is rapid and has yielded excellent results on silicate rocks and on samples from the aluminum phosphate (leached) zone of the Florida phosphate deposits.

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↗