Search USGS⌕ Search

Geology topics

S.L. Werner

Publications and source records attributed to S.L. Werner.

8 recordsLinked to original sources

Determination of submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples by solid-phase extraction and liquid chromatography

A method for determining submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples has been developed. Caffeine is extracted from a 1 L water sample with a 0.5 g graphitized carbon-based solid-phase cartridge, eluted with methylene chloride-methanol (80 + 20, v/v), and analyzed by liquid chromatography with photodiode-array detection. The single-operator method detection limit for organic-free water samples was 0.02 μg/L. Mean recoveries and relative standard deviations were 93 ± 13% for organic- free water samples fortified at 0.04 μg/L and 84 ± 4% for laboratory reagent spikes fortified at 0.5 μg/L. Environmental concentrations of caffeine ranged from 0.003 to 1.44 μg/L in surface water samples and from 0.01 to 0.08 μg/L in groundwater samples.

Journal of AOAC International↗

Bioaccumulation of pharmaceuticals and other anthropogenic waste indicators in earthworms from agricultural soil amended with biosolid or swine manure

Analysis of earthworms offers potential for assessing the transfer of organic anthropogenic waste indicators (AWIs) derived from land-applied biosolid or manure to biota. Earthworms and soil samples were collected from three Midwest agricultural fields to measure the presence and potential for transfer of 77 AWIs from land-applied biosolids and livestock manure to earthworms. The sites consisted of a soybean field with no amendments of human or livestock waste (Site 1), a soybean field amended with biosolids from a municipal wastewater treatment plant (Site 2), and a cornfield amended with swine manure (Site 3). The biosolid applied to Site 2 contained a diverse composition of 28 AWIs, reflecting the presence of human-use compounds. The swine manure contained 12 AWIs, and was dominated by biogenic sterols. Soil and earthworm samples were collected in the spring (about 30 days after soil amendment) and fall (140−155 days after soil amendment) at all field sites. Soils from Site 1 contained 21 AWIs and soil from Sites 2 and 3 contained 19 AWIs. The AWI profiles at Sites 2 and 3 generally reflected the relative composition of AWIs present in waste material applied. There were 20 AWIs detected in earthworms from Site 1 (three compounds exceeding concentrations of 1000 µg/kg), 25 AWIs in earthworms from Site 2 (seven compounds exceeding concentrations of 1000 µg/kg), and 21 AWIs in earthworms from Site 3 (five compounds exceeding concentrations of 1000 µg/kg). A number of compounds that were present in the earthworm tissue were at concentrations less than reporting levels in the corresponding soil samples. The AWIs detected in earthworm tissue from the three field sites included pharmaceuticals, synthetic fragrances, detergent metabolites, polycyclic aromatic hydrocarbons (PAHs), biogenic sterols, disinfectants, and pesticides, reflecting a wide range of physicochemical properties. For those contaminants detected in earthworm tissue and soil, bioaccumulation factors (BAF) ranged from 0.05 (galaxolide) to 27 (triclosan). This study documents that when AWIs are present in source materials that are land applied, such as biosolids and swine manure, AWIs can be transferred to earthworms.

Environmental Science & Technology↗

Survey of organic wastewater contaminants in biosolids destined for land application

In this study, the presence, composition, and concentrations of organic wastewater contaminants (OWCs) were determined in solid materials produced during wastewater treatment. This study was undertaken to evaluate the potential of these solids, collectively referred to as biosolids, as a source of OWCs to soil and water in contact with soil. Nine different biosolid products, produced by municipal wastewater treatment plants in seven different states, were analyzed for 87 different OWCs. Fifty-five of the OWCs were detected in at least one biosolid product. The 87 different OWCs represent a diverse cross section of emerging organic contaminants that enter wastewater treatment plants and may be discharged without being completely metabolized or degraded. A minimum of 30 and a maximum of 45 OWCs were detected in any one biosolid. The biosolids used in this study are produced by several production methods, and the plants they originate from have differing population demographics, yet the percent composition of total OWC content, and of the most common OWCs, typically did not vary greatly between the biosolids tested. The summed OWC content ranged from 64 to 1811 mg/kg dry weight. Six biosolids were collected twice, 3−18 months apart, and the total OWC content of each biosolid varied by less than a factor of 2. These results indicate that the biosolids investigated in this study have OWC compositions and concentrations that are more similar than different and that biosolids are highly enriched in OWCs (as mass-normalized concentrations) when compared to effluents or effluent-impacted water. These results demonstrate the need to better describe the composition and fate of OWCs in biosolids since about 50% of biosolids are land applied and thus become a potentially ubiquitous nonpoint source of OWCs into the environment.

Environmental Science & Technology↗

Presence and distribution of wastewater-derived pharmaceuticals in soil irrigated with reclaimed water

Three sites in the Front Range of Colorado, USA, were monitored from May through September 2003 to assess the presence and distribution of pharmaceuticals in soil irrigated with reclaimed water derived from urban wastewater. Soil cores were collected monthly, and 19 pharmaceuticals, all of which were detected during the present study, were measured in 5‐cm increments of the 30‐cm cores. Samples of reclaimed water were analyzed three times during the study to assess the input of pharmaceuticals. Samples collected before the onset of irrigation in 2003 contained numerous pharmaceuticals, likely resulting from the previous year's irrigation. Several of the selected pharmaceuticals increased in total soil concentration at one or more of the sites. The four most commonly detected pharmaceuticals were erythromycin, carbamazepine, fluoxetine, and diphenhydramine. Typical concentrations of the individual pharmaceuticals observed were low (0.02–15 μg/kg dry soil). The existence of subsurface maximum concentrations and detectable concentrations at the lowest sampled soil depth might indicate interactions of soil components with pharmaceuticals during leaching through the vadose zone. Nevertheless, the present study demonstrates that reclaimed‐water irrigation results in soil pharmaceutical concentrations that vary through the irrigation season and that some compounds persist for months after irrigation.

Environmental Toxicology and Chemistry↗

Transport of chemical and microbial compounds from known wastewater discharges: Potential for use as indicators of human fecal contamination

The quality of drinking and recreational water is currently (2005) determined using indicator bacteria. However, the culture tests used to analyze for these bacteria require a long time to complete and do not discriminate between human and animal fecal material sources. One complementary approach is to use chemicals found in human wastewater, which would have the advantages of (1) potentially shorter analysis times than the bacterial culture tests and (2) being selected for human-source specificity. At 10 locations, water samples were collected upstream and at two successive points downstream from a wastewaster treatment plant (WWTP); a treated effluent sample was also collected at each WWTP. This sampling plan was used to determine the persistence of a chemically diverse suite of emerging contaminants in streams. Samples were also collected at two reference locations assumed to have minimal human impacts. Of the 110 chemical analytes investigated in this project, 78 were detected at least once. The number of compounds in a given sample ranged from 3 at a reference location to 50 in a WWTP effluent sample. The total analyte load at each location varied from 0.018 μg/L at the reference location to 97.7 μg/L in a separate WWTP effluent sample. Although most of the compound concentrations were in the range of 0.01−1.0 μg/L, in some samples, individual concentrations were in the range of 5−38 μg/L. The concentrations of the majority of the chemicals present in the samples generally followed the expected trend:  they were either nonexistent or at trace levels in the upstream samples, had their maximum concentrations in the WWTP effluent samples, and then declined in the two downstream samples. This research suggests that selected chemicals are useful as tracers of human wastewater discharge.

Environmental Science & Technology↗

Routine low-level monitoring of polar pesticides and pesticide degradates by HPLC/ESI-MS: Evaluating long-term performance

The sensitivity and selective determination of polar pesticides were analyzed using high-performance liquid chromatography/electrospray ionization-mass spectrometry (HPLC/ESI-MS). The effects of multiple operators and instruments on method performance were evaluated using 440 pairs of fortified reagent-water and blank reagent-water samples. The influence of varying environmental matrices on recovery and precision were also analyzed using 200 fortified ambient water samples and duplicate ambient water samples. The results show that compound stability in filtered water was matrix-, chemical class- and compound-dependent which ranged from 1 day to 2 weeks.

Conference Paper↗

Routine determination of sulfonylurea, imidazolinone, and sulfonamide herbicides at nanogram-per-liter concentrations by solid-phase extraction and liquid chromatography/mass spectrometry

Sulfonylurea (SU), imidazolinone (IMI), and sulfonamide (SA) herbicides are new classes of low-application-rate herbicides increasingly used by farmers. Some of these herbicides affect both weed and crop species at low dosages and must be carefully used. Less is known about the effect of these compounds on non-crop plant species, but a concentration of 100 ng/l in water has been proposed as the threshold for possible plant toxicity for most of these herbicides. Hence, analytical methods must be capable of detecting SUs, IMIs, and SAs at concentrations less than 100 ng/l in ambient water samples. The authors developed a two-cartridge, solid-phase extraction method for isolating 12 SU, 3 IMI, and 1 SA herbicides by using high-performance liquid chromatography/electrospray ionization-mass spectrometry (HPLC/ESI-MS) to identify and quantify these herbicides to 10 ng/l. This method was used to analyze 196 surface- and ground-water samples collected from May to August 1998 throughout the Midwestern United States, and more than 100 quality-assurance and quality-control samples. During the 16 weeks of the study, the HPLC/ESI-MS maintained excellent calibration linearity across the calibration range from 5 to 500 ng/l, with correlation coefficients of 0.9975 or greater. Continuing calibration verification standards at 100-ng/l concentration were analyzed throughout the study, and the average measured concentrations for individual herbicides ranged from 93 to 100 ng/l. Recovery of herbicides from 27 reagent-water samples spiked at 50 and 100 ng/l ranged from 39 to 92%, and averaged 73%. The standard deviation of recoveries ranged from 14 to 26%, and averaged 20%. This variability reflects multiple instruments, operators, and the use of automated and manual sample preparation. Spiked environmental water samples had similar recoveries, although for some herbicides, the sample matrix enhanced recoveries by as much as 200% greater than the spiked concentration. This matrix enhancement was sample- and compound-dependent. Concentrations of herbicides in unspiked duplicate environmental samples were typically within 25% of each other. The results demonstrate the usefulness of HPLC/ESI-MS for determining low-application-rate herbicides at ambient concentrations.

Science of Total Environment↗

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of selected carbamate pesticides in water by high-performance liquid chromatography

As part of its primary responsibility concerning water as a national resource, the U.S. Geological Survey collects and analyzes samples of ground water and surface water to determine water quality. This report describes the method used since June 1987 to determine selected total-recoverable carbamate pesticides present in water samples. High- performance liquid chromatography is used to separate N-methyl carbamates, N-methyl carbamoyloximes, and an N-phenyl carbamate which have been extracted from water and concentrated in dichloromethane. Analytes, surrogate compounds, and reference compounds are eluted from the analytical column within 25 minutes. Two modes of analyte detection are used: (1) a photodiode-array detector measures and records ultraviolet-absorbance profiles, and (2) a fluorescence detector measures and records fluorescence from an analyte derivative produced when analyte hydrolysis is combined with chemical derivatization. Analytes are identified and confirmed in a three-stage process by use of chromatographic retention time, ultraviolet (UV) spectral comparison, and derivatization/fluorescence detection. Quantitative results are based on the integration of single-wavelength UV-absorbance chromatograms and on comparison with calibration curves derived from external analyte standards that are run with samples as part of an instrumental analytical sequence. Estimated method detection limits vary for each analyte, depending on the sample matrix conditions, and range from 0.5 microgram per liter to as low as 0.01 microgram per liter. Reporting levels for all analytes have been set at 0.5 microgram per liter for this method. Corrections on the basis of percentage recoveries of analytes spiked into distilled water are not applied to values calculated for analyte concentration in samples. These values for analyte concentrations instead indicate the quantities recovered by the method from a particular sample matrix.

Open-File Report↗