USGS Science⌕ Search

SEARCH · USGS Science

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 19 recordsLinked to original sources
USGS2025

A comprehensive assessment of membrane bioreactor contaminant removal efficacy through analytical chemistry, fish exposures, and microbiome characterization

Treated municipal wastewater effluent is an important pathway for Contaminants of Emerging Concern (CEC) to enter aquatic ecosystems. As the aging wastewater infrastructure in many industrialized countries requires upgrades or replacement, assessing new treatment technologies in the context of CEC effects may provide additional support for science-based resource management. Here, we used three lines of evidence, analytical chemistry, fish exposure experiments, and fish and water microbiome analysis, to assess the effectiveness of membrane bioreactor treatment (MBR) to replace traditional activated sludge treatment. To do this, we sampled a municipal wastewater treatment plant with a split wastewater stream, a portion of which was treated with an MBR and another via an oxidation ditch (OXI). The OXI and MBR treatments substantially reduced most measured CECs compared to the primary effluent (PRI). Only pesticides and some pharmaceuticals were recalcitrant to both secondary treatment methods. While ammonia toxicity of PRI prevented its inclusion in fish exposure experiments, exposure of fish with waters from the OXI or MBR treated wastewater produced only subtle biological differences with no adverse apical outcomes. These findings were consistent with low chemically derived exposure: activity ratios for OXI and MBR. Microbiome analysis of fish and wastewater highlighted the significant reduction of microbial abundance and diversity in the MBR treatment compared to all other treatments. The comparable removal efficacy of CECs in MBR makes it an attractive alternative to traditional OXI, especially when MBR may eliminate the need for tertiary treatment for wastewater disinfection.

Environmental Toxicology and Chemistry↗
USGS2014

Integrated assessment of runoff from livestock farming operations: analytical chemistry, in vitro bioassays, and in vivo fish exposures

Animal waste from livestock farming operations can contain varying levels of natural and synthetic androgens and/or estrogens, which can contaminate surrounding waterways. In the present study, surface stream water was collected from 6 basins containing livestock farming operations. Aqueous concentrations of 12 hormones were determined via chemical analyses. Relative androgenic and estrogenic activity was measured using in vitro cell assays (MDA-kb2 and T47D-Kbluc assays, respectively). In parallel, 48-h static-renewal in vivo exposures were conducted to examine potential endocrine-disrupting effects in fathead minnows. Mature fish were exposed to surface water dilutions (0%, 25%, 50%, and 100%) and 10-ng/L of 17α-ethynylestradiol or 50-ng/L of 17β-trenbolone as positive controls. Hepatic expression of vitellogenin and estrogen receptor α mRNA, gonadal ex vivo testosterone and 17β-estradiol production, and plasma vitellogenin concentrations were examined. Potentially estrogenic and androgenic steroids were detected at low nanogram per liter concentrations. In vitro estrogenic activity was detected in all samples, whereas androgenic activity was detected in only 1 sample. In vivo exposures to the surface water had no significant dose-dependent effect on any of the biological endpoints, with the exception of increased male testosterone production in 1 exposure. The present study, which combines analytical chemistry measurements, in vitro bioassays, and in vivo fish exposures, highlights the integrated value and future use of a combination of techniques to obtain a comprehensive characterization of an environmental chemical mixture.

Arkansas, Iowa, Kentucky, New York, Wisconsin↗
USGS2010

A role for analytical chemistry in advancing our understanding of the occurrence, fate, and effects of Corexit Oil Dispersants

On April 24, 2010, the sinking of the Deepwater Horizon oil rig resulted in the release of oil into the Gulf of Mexico. As of July 19, 2010, the federal government's Deepwater Horizon Incident Joint Information Center estimates the cumulative range of oil released is 3,067,000 to 5,258,000 barrels, with a relief well to be completed in early August. By comparison, the Exxon Valdez oil spill released a total of 260,000 barrels of crude oil into the environment. As of June 9, BP has used over 1 million gallons of Corexit oil dispersants to solubilize oil and help prevent the development of a surface oil slick. Oil dispersants are mixtures containing solvents and surfactants that can exhibit toxicity toward aquatic life and may enhance the toxicity of components of weathered crude oil. Detailed knowledge of the composition of both Corexit formulations and other dispersants applied in the Gulf will facilitate comprehensive monitoring programs for determining the occurrence, fate, and biological effects of the dispersant chemicals. The lack of information on the potential impacts of oil dispersants has caught industry, federal, and state officials off guard. Until compositions of Corexit 9500 and 9527 were released by the U.S. Environmental Protection Agency online, the only information available consisted of Material Safety Data Sheets (MSDS), patent documentation, and a National Research Council report on oil dispersants. Several trade and common names are used for the components of the Corexits. For example, Tween 80 and Tween 85 are oligomeric mixtures.

Environmental Science & Technology↗
USGS2006

Chlorfenapyr and mallard ducks: Overview, study design, macroscopic effects, and analytical chemistry

The first commercial pesticide derived from a class of compounds known as halogenated pyrroles was registered for use in the United States in 2001. Chlorfenapyr degrades slowly in soil, sediment, and water and is highly toxic to birds. Information on biochemical or histological endpoints in birds is lacking; therefore, a two‐year study was conducted to provide information needed to develop diagnostic criteria for chlorfenapyr toxicosis. In the first year, male mallard ducks were fed concentrations of 0, 2, 5, or 10 ppm technical chlorfenapyr or 5 ppm of a formulated product in their diet during a 10‐week chronic exposure study. Survival, body weight, feed consumption (removal), behavior, and molt progression were monitored. Feed and liver were analyzed for chlorfenapyr and two metabolites. Five of 10 ducks in the 10‐ppm group died, and neurotoxic effects were observed in the 5‐and 10‐ppm groups. Feed removal increased for ducks receiving chlorfenapyr and body weights of 5‐ and 10‐ppm ducks were reduced. Loss of body fat, muscle atrophy, and bile retention were suggestive of metabolic disruption or a decreased ability to digest and absorb nutrients. Liver and kidney weights and liver and kidney weight/body weight ratios exhibited a positive response to concentrations of chlorfenapyr in the diet. Emaciation and elevated organ weight/body weight ratios are candidates for a suite of indicators of chronic chlorfenapyr exposure. Liver is the preferred tissue for chemical confirmation of exposure.

Environmental Toxicology and Chemistry↗
USGS2024

Determination of antimycin–a in a liquid formulation by high performance liquid chromatography–mass spectrometry

Pesticide formulations containing the active ingredient antimycin–a (ANT–A) have been used by fisheries and aquaculture managers for several decades to remove nuisance fish species. Analytical methods for measuring ANT–A during pesticide treatments have been done using high performance liquid chromatography (HPLC) paired with multiple detection methods (for example, electrochemical, ultraviolet, fluorescence, mass spectrometry). However, instruments and analytical chemistry methods can advance over time because of the need to develop timely, reliable, cost effective, and reproducible methods. Subsequently, ANT–A analytical chemistry methods and sample processing techniques also have improved over the past several decades. In the present study, we describe a liquid chromatography–mass spectrometry method and its verification across three analysts. Each analyst group created a single calibration curve and verified ANT–A in a liquid formulation using the averaged total response of all major ANT–A homologs (A1, A3, A3, A4). The advantage of this technique is that it creates a more resilient ANT–A quantification method amendable to batch-batch differences in major homologs. The method demonstrated how ANT–A can be effectively measured with high accuracy (98–99 percent), precision (2.7–16.2 percent), and specificity within a pesticide liquid formulation using a method applicable for Federal registration requirements.

Open-File Report↗
USGS2013

Comparison of select hematology and serum chemistry analtyes between wild-caught and aquarium-housed lake sturgeon ( Acipenser fulvescens )

Hematology and serum chemistry analytes were compared between wild-caught and aquarium-housed lake sturgeon ( Acipenser fulvescens ) to potentially improve understanding of medical issues in lake sturgeon. Blood samples were taken from 30 lake sturgeon exhibited in 11 institutions in the United States and from 23 experimentally stocked lake sturgeon caught in gill nets in the lower Genesee River in Rochester, New York, USA. For hematology, only segmented neutrophil count was significantly different, with wild-caught fish having a higher number of circulating neutrophils. For clinical chemistry analytes, chloride, uric acid, calcium, phosphate, glucose, aspartate aminotransferase, triglycerides, and creatine kinase were significantly different between the two cohorts. These differences are likely not clinically significant and are attributable to handling stress, variability in environmental parameters, or differences in nutritional status. This is the first report of hematology and serum chemistry values in aquarium-housed lake sturgeon and provides useful reference intervals for clinicians.

New York↗
USGS2025

Flow cytometric detection of waterborne bacteria metabolic response to anthropogenic chemical inputs to aquatic ecosystems

Typical investigations into the biological consequences of suspected xenobiotics or nutrients introduced in watersheds include analytical chemistry screens of environmental samples—such as periphyton responses or studies of fish condition—which are all costly in terms of equipment, reagents, time, and human resources. An alternative is to assess pollutant effects on waterborne bacteria. A flow cytometric method was developed to yield rapid, same-day results that could be used to proactively screen for suspected chemical inputs into watersheds using water sampling methods that are identical to those in standard use. The analytical methods are microbe cultivation-independent, for use with waterborne bacteria that are typically viable but not culturable. The procedure is quick and inexpensive, generating measures of bacterial esterase that reflect metabolic activity and are sensitive and statistically robust. After phosphate-EDTA incubation to increase cell wall permeability, staining was performed with 5(6) carboxyfluorescein diacetate (enzyme activity) and propidium iodide (cell viability) with three bacterial species in exponential phase growth having been incubated with organic wastewater compounds (atrazine, pharmaceuticals [17α-ethynylestradiol and trenbolone], and antimicrobials [tylosin and butylparaben]). This method successfully detected metabolic changes in all bacterial species, with atrazine inducing the greatest change. Additional fluorescent stains can target specific microbial structures or functions of interest in a particular watershed. This biotechnology can inform analytical chemistry and study of biota at sites of interest and has the potential to be automated.

Cells↗
USGS2010

Evaluation of a portable automated serum chemistry analyzer for field assessment of harlequin ducks, Histrionicus histrionicus

A portable analytical chemistry analyzer was used to make field assessments of wild harlequin ducks ( Histrionicus histrionicus ) in association with telemetry studies of winter survival in Prince William Sound, Alaska. We compared serum chemistry results obtained on-site with results from a traditional laboratory. Particular attention was paid to serum glucose and potassium concentrations as potential indicators of high-risk surgical candidates based on evaluation of the field data. The median differential for glucose values ( 𝑁 = 8 2 ) between methods was 0.6 mmol/L (quartiles 0.3 and 0.9 mmol/L) with the median value higher when assayed on site. Analysis of potassium on site returned a median of 2.7 mmol/L ( 𝑁 = 8 8 ; quartiles 2.4 and 3.0 mmol/L). Serum potassium values were too low for quantitation by the traditional laboratory. Changes in several serum chemistry values following a three-day storm during the study support the value of on site evaluation of serum potassium to identify presurgical patients with increased anesthetic risk.

Alaska↗
USGS1987

Methods for geochemical analysis

The laboratories for analytical chemistry within the Geologic Division of the U.S. Geological Survey are administered by the Office of Mineral Resources. The laboratory analysts provide analytical support to those programs of the Geologic Division that require chemical information and conduct basic research in analytical and geochemical areas vital to the furtherance of Division program goals. Laboratories for research and geochemical analysis are maintained at the three major centers in Reston, Virginia, Denver, Colorado, and Menlo Park, California. The Division has an expertise in a broad spectrum of analytical techniques, and the analytical research is designed to advance the state of the art of existing techniques and to develop new methods of analysis in response to special problems in geochemical analysis. The geochemical research and analytical results are applied to the solution of fundamental geochemical problems relating to the origin of mineral deposits and fossil fuels, as well as to studies relating to the distribution of elements in varied geologic systems, the mechanisms by which they are transported, and their impact on the environment.

Bulletin↗
USGS2010

The H4IIE cell bioassay as an indicator of dioxin-like chemicals in wildlife and the environment

The H4IIE cell bioassay has proven utility as a screening tool for planar halogenated hydrocarbons (PHHs) and structurally similar chemicals accumulated in organisms from the wild. This bioassay has additional applications in hazard assessment of PHH exposed populations. In this review, the toxicological principles, current protocols, performance criteria, and field applications for the assay are described. The H4IIE cell bioassay has several advantages over the analytical measurement of PHHs in environmental samples, but conclusions from studies can be strengthened when both bioassay and analytical chemistry data are presented together. Often, the bioassay results concur with biological effects in organisms and support direct measures of PHHs. For biomonitoring purposes and prioritization of PHH-contaminated environments, the H4IIE bioassay may be faster and less expensive than analytical measurements. The H4IIE cell bioassay can be used in combination with other biomarkers such as in vivo measurements of CYP1A1 induction to help pinpoint the sources and identities of dioxin-like chemicals. The number of studies that measure H4IIE-derived TCDD-EQs continues to increase, resulting in subtle improvements over time. Further experiments are required to determine if TCDD-EQs derived from mammalian cells are adequate predictors of toxicity to non-mammalian species. The H4IIE cell bioassay has been used in over 300 published studies, and its combination of speed, simplicity, and ability to integrate the effects of complex containment mixtures makes it a valuable addition to hazard assessment and biomonitoring studies.

Critical Reviews in Toxicology↗
USGS2021

Potential use of the benthic foraminifers Bulimina denudata and Eggerelloides advenus in marine sediment toxicity testing

The benthic foraminifers Bulimina denudata and Eggerelloides advenus are commonly abundant in offshore regions in the Pacific Ocean, especially in waste-discharge sites. The relationship between their abundance and standard macrofaunal sediment toxicity tests (amphipod survival and sea urchin fertilization) as well as sediment chemistry analyte measurements were determined for sediments collected in 1997 in Santa Monica Bay, California, USA, an area impacted by historical sewage input from the Hyperion Outfall primarily since the late 1950s. Very few surface samples proved to be contaminated based on either toxicity or chemistry tests and the abundance of B. denudata did not correlate with any of these. The abundance of E. advenus also did not correlate with toxicity, but positively correlated with total solids and negatively correlated with arsenic, beryllium, chromium, lead, mercury, nickel, zinc, iron, and TOC. In contrast, several downcore samples proved to be contaminated as indicated by both toxicity and chemistry data. The abundance of B. denudata positively correlated with amphipod survival and negatively correlated with arsenic, cadmium, unionized ammonia, and TOC; E. advenus negatively correlated with sea urchin fertilization success as well as beryllium, cadmium, and total PCBs. As B. denudata and E. advenus are tolerant of polluted sediments and their relative abundances appear to track those of macrofaunal toxicity tests, their use as cost- and time-effective marine sediment toxicity tests may have validity and should be further investigated.

California↗
USGS2014

Transcriptomic effects-based monitoring for endocrine active chemicals: Assessing relative contribution of treated wastewater to downstream pollution

The present study investigated whether a combination of targeted analytical chemistry information with unsupervised, data-rich biological methodology (i.e., transcriptomics) could be utilized to evaluate relative contributions of wastewater treatment plant (WWTP) effluents to biological effects. The effects of WWTP effluents on fish exposed to ambient, receiving waters were studied at three locations with distinct WWTP and watershed characteristics. At each location, 4 d exposures of male fathead minnows to the WWTP effluent and upstream and downstream ambient waters were conducted. Transcriptomic analyses were performed on livers using 15 000 feature microarrays, followed by a canonical pathway and gene set enrichment analyses. Enrichment of gene sets indicative of teleost brain–pituitary–gonadal–hepatic (BPGH) axis function indicated that WWTPs serve as an important source of endocrine active chemicals (EACs) that affect the BPGH axis (e.g., cholesterol and steroid metabolism were altered). The results indicated that transcriptomics may even pinpoint pertinent adverse outcomes (i.e., liver vacuolization) and groups of chemicals that preselected chemical analytes may miss. Transcriptomic Effects-Based monitoring was capable of distinguishing sites, and it reflected chemical pollution gradients, thus holding promise for assessment of relative contributions of point sources to pollution and the efficacy of pollution remediation.

Environmental Science & Technology↗
USGS2006

Mass spectrometric in the analysis of inorganic substances

Mass spectrometry is an analytical technique used to measure the composition of a substance by isolating specific analyte components according to their individual atomic or molecular mass‐to‐charge ratios. Inorganic mass spectrometry is specifically used to determine the elemental and isotopic composition of the material being analyzed. The techniques are capable of the measurement of a range of concentrations from major components to ultratrace constituents. Several instrumental approaches are used to separate and measure the abundance of component ions formed from the sample. These techniques include electron ionization mass spectrometry (EIMS), inductively coupled plasma mass spectrometry (ICPMS), thermal ionization mass spectrometry (TIMS) and spark source mass spectrometry (SSMS). These techniques utilize a variety of mass spectrometers including ion trap, quadrupole, magnetic sector and time‐of‐flight mass analyzers, depending on the type of sample being analyzed and the desired quality of the results. Often sample introduction techniques can be utilized to enhance the capabilities for solving specific analytical chemistry problems.

Book chapter↗
USGS2015

Pathway-based approaches for assessment of real-time exposure to an estrogenic wastewater treatment plant effluent on fathead minnow reproduction

Wastewater treatment plant (WWTP) effluents are known contributors of chemical mixtures into the environment. Of particular concern are endocrine-disrupting compounds, such as estrogens, which can affect the hypothalamic-pituitary-gonadal axis function in exposed organisms. The present study examined reproductive effects in fathead minnows exposed for 21 d to a historically estrogenic WWTP effluent. Fathead minnow breeding pairs were held in control water or 1 of 3 effluent concentrations (5%, 20%, and 100%) in a novel onsite, flow-through system providing real-time exposure. The authors examined molecular and biochemical endpoints representing key events along adverse outcome pathways linking estrogen receptor activation and other molecular initiating events to reproductive impairment. In addition, the authors used chemical analysis of the effluent to construct a chemical-gene interaction network to aid in targeted gene expression analyses and identifying potentially impacted biological pathways. Cumulative fecundity was significantly reduced in fish exposed to 100% effluent but increased in those exposed to 20% effluent, the approximate dilution factor in the receiving waters. Plasma vitellogenin concentrations in males increased in a dose-dependent manner with effluent concentration; however, male fertility was not impacted. Although in vitro analyses, analytical chemistry, and biomarker responses confirmed the effluent was estrogenic, estrogen receptor agonists were unlikely the primary driver of impaired reproduction. The results provide insights into the significance of pathway-based effects with regard to predicting adverse reproductive outcomes.

Environmental Toxicology and Chemistry↗