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Results for “Journal of Chromatography A”

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At least 73 records · Page 4Linked to original sources
USGS1990

Production of sulfur gases and carbon dioxide by synthetic weathering of crushed drill cores from the Santa Cruz porphyry copper deposit near Casa Grande, Pinal County, Arizona

Samples of ground drill cores from the southern part of the Santa Cruz porphyry copper deposit, Casa Grande, Arizona, were oxidized in simulated weathering experiments. The samples were also separated into various mineral fractions and analyzed for contents of metals and sulfide minerals. The principal sulfide mineral present was pyrite. Gases produced in the weathering experiments were measured by gas chromatography. Carbon dioxide, oxygen, carbonyl sulfide, sulfur dioxide and carbon disulfide were found in the gases; no hydrogen sulfide, organic sulfides, or mercaptans were detected. Oxygen concentration was very important for production of the volatiles measured; in general, oxygen concentration was more important to gas production than were metallic element content, sulfide mineral content, or mineral fraction (oxide or sulfide) of the sample. The various volatile species also appeared to be interactive; some of the volatiles measured may have been formed through gas reactions.

Journal of Geochemical Exploration↗
USGS2007

Semipermeable membrane devices used to estimate bioconcentration of polychlorinated biphenyls

ABSTRACT: Aquatic organisms passively accumulate hydrophobic organic compounds, such as polychlorinated biphenyls, even when ambient water concentrations of the contaminant are below analytical detection limits. However, contaminant concentrations in tissue samples are subject to an inherently high level of variability due to differences in species, life stage, and gender bioconcentration potentials. Semipermeable membrane devices (SPMDs) were used to sample Aroclor 1254, a mixture of readily bioconcentrated polychlorinated biphenyls (PCBs), in a contaminated wetland near Flat Top, WV. The devices consisted of triolein, a lipid found in fish, enclosed in a polyethylene membrane. SPMDs were deployed in the water column and in direct contact with wetland sediments along a previously identified concentration gradient of PCBs. The devices were retrieved after a 25-day exposure period. Analytes were recovered by dialyzing the devices in nanograde hexane. Hexane dialysates were condensed and analyzed by gas chromatography. All deployed devices sequestered quantifiable amounts of Aroclor 1254. Water-column SPMDs accumulated PCBs far in excess of ambient water concentrations. The devices contacting sediments accumulated PCBs at all sites, though accumulated concentrations did not exceed concentrations in sediment. Patterns of PCB concentration in the devices corresponded to the identified gradient at the site. Results from the water-column SPMDs were used to estimate the concentration of the dissolved, bioavailable fraction of PCBs present in the water column. These concentrations ranged from 0.01 to 0.09 μg/L of bioavailable Aroclor 1254.

Journal of the American Water Resources Associatio↗
USGS2020

Identification of polychlorinated biphenyls in two bald eagles by combined gas-liquid chromatography-mass spectrometry

Polychlorinated biphenyls are widely used industrial compounds marketed in the United States under the trade name Aroclor. They have appeared in fish and wildlife tissues in this country and Europe. They are known to be toxic, but more importantly, their presence in samples along with the commonly occurring organochlorine pesticides complicates the analysis to a serious degree, making identification of pesticide residues by GLC without preliminary separation extremely unreliable. Residues of both polychlorinated biphenyls and organochloride pesticides were present in eagle carcasses. Many of the polychlorinated biphenyl components had retention times identical with those of certain organochlorine pesticide residues. Identification was accomplished by preliminary separations on thin layer plates followed by combined GLC- mass spectromtry.

Journal of the Association of Official Analytical ↗
USGS2000

Comparison of enzyme-linked immunosorbent assay and gas chromatography procedures for the detection of cyanazine and metolachlor in surface water samples

Enzyme-linked immunosorbent assay (ELISA) data from surface water reconnaissance were compared to data from samples analyzed by gas chromatography for the pesticide residues cyanazine (2-[[4-chloro-6-(ethylamino)-l,3,5-triazin-2-yl]amino]-2-methylpropanenitrile ) and metolachlor (2-chloro-N-(2-ethyl-6-methylphenyl)-N-(2-methoxy-1-methylethyl)acetamide). When ELISA analyses were duplicated, cyanazine and metolachlor detection was found to have highly reproducible results; adjusted R2s were 0.97 and 0.94, respectively. When ELISA results for cyanazine were regressed against gas chromatography results, the models effectively predicted cyanazine concentrations from ELISA analyses (adjusted R2s ranging from 0.76 to 0.81). The intercepts and slopes for these models were not different from 0 and 1, respectively. This indicates that cyanazine analysis by ELISA is expected to give the same results as analysis by gas chromatography. However, regressing ELISA analyses for metolachlor against gas chromatography data provided more variable results (adjusted R2s ranged from 0.67 to 0.94). Regression models for metolachlor analyses had two of three intercepts that were not different from 0. Slopes for all metolachlor regression models were significantly different from 1. This indicates that as metolachlor concentrations increase, ELISA will over- or under-estimate metolachlor concentration, depending on the method of comparison. ELISA can be effectively used to detect cyanazine and metolachlor in surface water samples. However, when detections of metolachlor have significant consequences or implications it may be necessary to use other analytical methods.

Journal of Agricultural and Food Chemistry↗
USGS2010

Use of volatile organic components in scat to identify canid species

Identification of wildlife species from indirect evidence can be an important part of wildlife management, and conventional +methods can be expensive or have high error rates. We used chemical characterization of the volatile organic constituents (VOCs) in scat as a method to identify 5 species of North American canids from multiple individuals. We sampled vapors of scats in the headspace over a sample using solid-phase microextraction and determined VOC content using gas chromatography with a flame ionization detector. We used linear discriminant analysis to develop models for differentiating species with bootstrapping to estimate accuracy. Our method correcdy classified 82.4% (bootstrapped 95% CI = 68.8-93.8%) of scat samples. Red fox (Vulpes vulpes) scat was most frequendy misclassified (25.0% of scats misclassified); red fox was also the most common destination for misclassified samples. Our findings are the first reported identification of animal species using VOCs in vapor emissions from scat and suggest that identification of wildlife species may be plausible through chemical characterization of vapor emissions of scat.

Journal of Wildlife Management↗
USGS1981

Geochemical prospecting for hydrocarbons in the outer continental shelf, Southern Bering Sea, Alaska

This geochemical survey is based on 20 stations located on the outer continental shelf of the southern Bering Sea in an area of 30,000 km 2 that includes St. George basin. Hydrocarbon gases from sediment samples recovered by gravity coring at each of the stations were analyzed by gas chromatography. Data are summarized for a subbottom depth of 0.5 m, because core penetration, although variable, reached at least this depth at all of these stations. Two parameters were used to distinguish the possible presence of thermogenic hydrocarbons: (1) ratios less than 50 of methane to ethane plus propane; and (2) ratios greater than 1 of ethane to ethene. No major hydrocarbon anomalies were discovered; however, at two stations at the northern end of St. George basin, our data indicate that thermogenic hydrocarbons may be present at depth. Major faulting in the vicinity of these stations could provide the pathways for the gas.

Journal of Geochemical Exploration↗
USGS1995

Concentrations of dissolved and particulate Polychlorinated Biphenyls in water from the Saginaw River, Michigan

The Saginaw River receives water from a major drainage basin in the east-central portion of the lower peninsula of Michigan. Historically the river has been contaminated with polychlorinated biphenyls (PCBs) from several sources. The present study was conducted to determine the concentrations of PCBs in both the dissolved and particulate phases of water in the lower Saginaw River, as well as the relative contribution of PCBs from the lower portion of the river relative to more upstream locations. Water samples were collected in 1990–1991, during a range of discharge conditions. Suspended particulates were collected from water onto glass-fiber filters by use of a “Penta-plate” filtration apparatus. Filtered water was subsequently passed through XAD-2 macroreticular resin to collect the “dissolved” PCBs. Concentrations of PCBs in both phases were determined by congener specific gas chromatography with electron capture detection. Total concentrations of PCBs ranged from 11 to 31 ng/L. The concentrations of PCBs in the dissolved phase ranged from 1.9 to 16 ng/L. The ratio of total PCBs bound to suspended particulates, relative to dissolved PCBs, was 2:1 and remained fairly constant for discharges less than approximately 400 M 3 /sec. The loading of total PCBs to Saginaw Bay was estimated to be 225 kg/yr, of which approximately 60% was found to be contributed by the lower 8 km of the Saginaw River.

Michigan↗
USGS2020

Determination of low concentrations of acetochlor in water by automated solid-phase extraction and gas chromatography with mass-selective detection

A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C 18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 μg/L Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 μg\L. Average single-operator precision, over the course of 1 week, was better than 5%.

Journal of AOAC International↗
USGS2020

American eels produce and release bile acids that vary across life stage

The American eel ( Anguilla rostrata ) is an imperilled fish hypothesized to use conspecific cues, in part, to coordinate long‐distance migration during their multistage life history. Here, holding water and tissue from multiple American eel life stages was collected and analysed for the presence, profile and concentration of bile acids. Distinct bile acid profiles were identified in glass, elver, yellow eel and silver eel holding waters using ultraperformance liquid chromatography high‐resolution mass spectrometry and principal component analysis. Taurochenodeoxycholic acid, taurodeoxycholic acid, cholic acid, deoxycholic acid, taurolithocholic acid and taurocholic acid were detected in whole tissue of American glass eels and elvers, and in liver, intestine and gallbladder samples of late‐stage yellow eels. Bile acids were not a major component of silver eel washings or tissue. This study is novel because little was previously known about bile acids produced and emitted into the environment by American eels. Future behavioural studies could evaluate whether any bile acids produced by American eels influence conspecific migratory behaviour.

Journal of Fish Biology↗
USGS1996

Optimization of the Ames/salmonella mutagenicity assay for use with extracts of aquatic sediments

Non-mutagenic components interfered with the ability of the standard Ames/salmonella assay to detect mutagenicity in extracts of contaminated Great Lakes sediments. The use of gel permeation chromatography (GPC) to remove these macromolecules from methylene chloride extracts prior to Ames testing enhanced the likelihood of transfer of mutagenic components into dimethyl sulf oxide (the assay solvent). Therefore, to optimize the assay's sensitivity we pre-treated sediment extracts using GPC and increased metabolic activity through the use of a 30% S9 mix. Increasing the level of Aroclor 1254-induced rat liver S9, typically used to metabolically activate promutagens, had the additional beneficial effect of reducing the cytotoxicity of the extracts. As applied in this study, the Ames assay can serve as a sensitive test for screening the mutagenic potential of large numbers of uncharacterized sediment extracts.

Journal of Great Lakes Research↗
USGS1985

Chemical investigations of wolf (Canis lupus) anal-sac secretion in relation to breeding season

The volatile constituents of wolf anal-sac secretions were examined via capillary gas chromatography and compared among intact males, females, castrate males, ovariectomized females, and anosmic and pinealectomized males and females. Some chemical compounds were deemed significantly different ( t test, 95% confidence level) among the groups both during and outside of the mating season, implying that the volatile components of anal-sac secretion can be used to communicate information regarding gender or endocrine state. As a result of treating the anal sac with antibiotics, some of these compounds, including 1-octen-3-ol and indole, were implicated as being products of microbial action. In addition, short-chain carboxylic acids were investigated and essentially no significant variations were seen among the groups.

Journal of Chemical Ecology↗
USGS1970

Organochlorine insecticide residues in soils and soil invertebrates from agricultural lands

Soils and earthworms and other soil invertebrates were collected from 67 agricultural fields in eight States. Samples were analyzed by gas chromatography for DDE, DDD, DDT, aldrin, dieldrin, endrin, heptachlor, heptachlor epoxide, and gamma-chlordane insecticides. Organochlorine insecticides in soils averaged 1.5 ppm, dry weight, and in earthworms, 13.8 ppm. Residues in earthworms averaged nine times that in soils. Residues ranged from a trace to 19.1 ppm in soils and from a trace to 159.4 ppm in earthworms. Residues in beetle larvae from two fields averaged 0.6 ppm; in snails from two fields, 3.5 ppm; and in slugs from four fields, 89.0 ppm. Amounts of insecticides in earthworms varied directly with amounts in soils. Coefficients of correlation between residues in soils and residues in earthworms usually were significant for DDE, DDD, and DDT regardless of crop or soil type.

Pesticides Monitoring Journal↗
USGS1990

Selenium speciation methods and application to soil saturation extracts from San Joaquin Valley, California

Methods to determine soluble concentrations of selenite, selenate, and organic Se were evaluated on saturation extracts of soil samples collected from three sites on the Panoche Creek alluvial fan in the western San Joaquin Valley, California. The methods were used in combination with hydride-generation atomic-absorption spectrometry for detection of Se, and included a selective chemical-digestion method and three chromatographic methods using XAD-8 resin, Sep-Pak C 18 cartridge, and a combination of XAD-8 resin and activated charcoal. The chromatography methods isolate dissolved organic matter that can inhibit Se detection by hydride-generation atomic-absorption spectrometry. Isolation of hydrophobic organic matter with XAD-8 did not affect concentrations of selenite and selenate, and the isolated organic matter represents a minimal estimation of organic Se. Ninety-eight percent of the Se in the extracts was selenate and about 100% of the isolated organic Se was associated with the humic acid fraction of dissolved organic matter. The depth distribution of Se species in the soil saturation extracts support a hypothesis that the distribution of soluble Se and salinity in these soils is the result of evaporation from a shallow water table and leaching by irrigation water low in Se and salinity.

California↗
USGS2019

Assessing the chemistry and bioavailability of dissolved organic matter from glaciers and rock glaciers

As glaciers thaw in response to warming, they release dissolved organic matter (DOM) to alpine lakes and streams. The United States contains an abundance of both alpine glaciers and rock glaciers. Differences in DOM composition and bioavailability between glacier types, like rock and ice glaciers, remain undefined. To assess differences in glacier and rock glacier DOM we evaluated bioavailability and molecular composition of DOM from four alpine catchments each with a glacier and a rock glacier at their headwaters. We assessed bioavailability of DOM by incubating each DOM source with a common microbial community and evaluated chemical characteristics of DOM before and after incubation using untargeted gas chromatography–mass spectrometry‐based metabolomics. Prior to incubations, ice glacier and rock glacier DOM had similar C:N ratios and chemical diversity, but differences in DOM composition. Incubations with a common microbial community showed that DOM from ice glacier meltwaters contained a higher proportion of bioavailable DOM and resulted in greater bacterial growth efficiency. After incubation, DOM composition from each source was statistically indistinguishable. This study provides an example of how MS‐based metabolomics can be used to assess effects of DOM composition on differences in bioavailability of DOM. Furthermore, it illustrates the importance of microbial metabolism in structuring composition of DOM. Even though rock glaciers had significantly less bioavailable DOM than ice glaciers, both glacial types still have potential to be important sources of bioavailable DOM to alpine headwaters over the coming decades.

Colorado↗
USGS2002

Analysis and detection of the herbicides dimethenamid and flufenacet and their sulfonic and oxanilic acid degradates in natural water

Dimethenamid [2-chloro-N-(2,4-dimethyl-3-thienyl)-N-(2-methoxy-1-methylethyl)acetamide] and flufenacet [N-(4-fluorophenyl)-N-(1-methylethyl)-2-(5-(trifluoromethyl)-1,3,4- thiadiazol-2-yl)oxy] were isolated by C-18 solid-phase extraction and separated from their ethanesulfonic acid (ESA) and oxanilic acid (OXA) degradates during their elution using ethyl acetate for the parent compound, followed by methanol for the polar degradates. The parent compounds were detected using gas chromatography-mass spectrometry in selected-ion mode. The ESA and OXA degradates were detected using high-performance liquid chromatography-electrospray mass spectrometry (HPLC-ESPMS) in negative-ion mode. The method detection limits for a 123-mL sample ranged from 0.01 to 0.07 μg/L. These methods are compatible with existing methods and thus allow for analysis of 17 commonly used herbicides and 18 of their degradation compounds with one extraction. In a study of herbicide transport near the mouth of the Mississippi River during 1999 and 2000, dimethenamid and its ESA and OXA degradates were detected in surface water samples during the annual spring flushes. For flufenacet, the only detections at the study site were for the ESA degradates in samples collected at the peak of the herbicide spring flush in 2000. The low frequency of detections in surface water likely is due to dimethenamid and flufenacet being relatively new herbicides. In addition, detectable amounts of the stable degradates have not been detected in ground water.

Journal of Agricultural and Food Chemistry↗
USGS1982

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection < 0.005 mg/L for both chemicals). A combined buffer (pH 4) and internal standard (3-chlorodiphenylamine) reagent is added to the water sample, which is injected through a Sep Pak C 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

Canadian Journal of Fisheries and Aquatic Sciences↗
USGS1973

Determination of the association and dissociation of humic acid fractions by small angle X-ray scattering

A procedure has been devised for the fractionation of humic acid samples from different environments. This procedure involves fractionation of the sample by adsorption chromatography on a Sephadex G-50 column followed by chromatography on either a G-25 or a G-100 column. The fractions of the solutions are then examined by small angle X-ray scattering. Three different types of behavior have been detected among the humic acid fractions: (1) Some fractions show very little change in aggregation at pH values above 3.5. (2) One fraction forms aggregates at pH values above and below pH 7, but at pH 7 it is completely dissociated. (3) In some fractions the degree of aggregation decreases with increasing pH. However, even at pH values as high as 11.5 some large particles are still present. These differences in association behavior are due to the interaction of different attractive and repulsive forces. In many aggregating systems only one type of attractive force is dominant; however in humic acid systems hydrogen bonding, &pi; bonding between planar aromatic moieties, and other coulombic interactions apparently all play a role in the formation of molecular aggregates.

Journal of Research of the U.S. Geological Survey↗
USGS1991

Rotenone persistence in freshwater ponds: Effects of temperature and sediment adsorption

The persistence of rotenone was compared between a cement-lined pond (0.04 hectare) and an earthen-bottom pond (0.02 hectare) treated with 5 μL Noxfish/L (250 μg rotenone/L) during spring, summer, and fall. Water temperatures on the days of treatment in each season were 8, 22, and 15°C, respectively. Both ponds were filled with pond water from a common source 1 week before each of the three treatments. Water samples (filtered and unfiltered) and sediment samples were analyzed by high-performance liquid chromatography to monitor the decrease of rotenone until residues were at or below the detection limit (<2.0 μg/L for water and < 25 ng/g for sediments). The loss of rotenone from water generally followed a first-order rate ofdecay. Rotenone disappeared two to three times faster in the earthen pond than in the concrete pond. The rotenone half-life times in the spring, summer, and fall treatments were 3.7, 1.3, and 5.2 d, respectively, in the concrete pond, and 1.8, 0.7, and 1.8 d in the earthen pond. Rates of decay in both ponds were directly correlated with water temperature. Filtered water samples from both ponds contained less rotenone than unfiltered water, indicating that some rotenone was bound to suspended material. The highest concentration of rotenone in sediment samples was 102 ng/g; residues decreased to below the detection limit within 14 d in the spring treatment and within 3 d in the summer and fall treatments.

North American Journal of Fisheries Management↗