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USGS2011

Elk Monitoring Protocol for Lewis and Clark National Historical Park, Version 1.0

Maintaining elk (Cervus elaphus roosevelti) herds that frequent Lewis and Clark National Historical Park (NHP) is central to the park’s purpose of preserving the historic, cultural, scenic, and natural resources. Elk were critical to sustaining the members of the Lewis and Clark expedition by providing food and clothing over the winter of 1805-1806. Today, elk viewing opportunities in the park and surrounding region generate broad appeal with the visiting public, which number over 250,000 per year at the Fort Clatsop visitor center. This protocol describes procedures for monitoring trends in the use of the Fort Clatsop area by Roosevelt elk. Specific objectives of elk monitoring in Lewis and Clark NHP are to measure the relative use and proportion of area used by elk during winter in the Fort Clatsop Unit of the park, and the rate at which elk are sighted from roads in and around the park. Relative use and the proportion of area used by elk are determined from elk fecal pellet surveys conducted every other year in the Fort Clatsop park unit. Pairs of observers visit a systematic array of permanent plots in the fall to clear them of elk fecal pellets, and return to the plots in late winter to count elk fecal pellets that have accumulated during winter. Half of the subplots are counted by two independent observers, which allows for the estimation of relative use and proportion of area occupied by elk with analyses of detection biases that account for unseen elk pellet groups. Standardized road surveys are conducted in and near the Fort Clatsop park unit three or four times monthly during alternate months. Data from road surveys are used to quantify the rate that park visitors would be expected to see elk, when driving the selected set of routes. The monitoring protocol is based on three field seasons of development and testing. The protocol narrative describes the background, rationale, sampling design, field methods, analytical methods, data management, reporting, personnel requirements, and operational requirements for elk monitoring in Lewis and Clark NHP. The sampling design reflects tradeoffs between statistical and ecological considerations, safety, and current budget considerations. The protocol provides adequate power to detect a doubling or halving of elk use in the Fort Clatsop unit and surrounding areas within 15 years. Step-by-step guidance for planning and completing the monitoring tasks are in the attached standard operating procedures (SOPs). Information on the status and trends of elk use in Lewis and Clark NHP will allow park managers to assess the effects on elk of restoration programs within the park, build community partnerships, and identify potential linkages between regional land use changes and elk use of the Park. Lewis and Clark NHP has an active ecological restoration program that aims to recreate, where possible, ecological conditions that Lewis and Clark encountered. The restoration program includes an extensive exotic plant removal program, wetland restoration, and silvicultural treatments that will hasten development of late-seral conditions in recently acquired forest lands of the Fort Clatsop park unit. In the future, monitoring results can be used to test for spatial associations between ecological restoration treatments and relative use by elk. The park also plans to feature results from elk monitoring prominently in its educational outreach activities to help interpret the historical and current ecological context of the Lewis and Clark story, and engender public support for the park mission and management activities. Although NPS does not manage non-park lands, information about trends in the distribution of elk use will be valuable in public outreach and discussions with other partnering agencies and regional private landowners.

Natural Resource Report↗

USGS2008

Occurrence of organic wastewater compounds in the Tinkers Creek watershed and two other tributaries to the Cuyahoga River, northeast Ohio

The U.S. Geological Survey - in cooperation with the Ohio Water Development Authority; National Park Service; Cities of Aurora, Bedford, Bedford Heights, Solon, and Twinsburg; and Portage and Summit Counties - and in collaboration with the Ohio Environmental Protection Agency, did a study to determine the occurrence and distribution of organic wastewater compounds (OWCs) in the Tinkers Creek watershed in northeastern Ohio. In the context of this report, OWCs refer to a wide range of compounds such as antibiotics, prescription and nonprescription pharmaceuticals, personal-care products, household and industrial compounds (for example, antimicrobials, fragrances, surfactants, fire retardants, and so forth) and a variety of other chemicals. Canisters containing polar organic integrative sampler (POCIS) and semipermeable membrane device (SPMD) media were deployed instream for a 28-day period in Mayand June 2006 at locations upstream and downstream from seven wastewater-treatment-plant (WWTP) outfalls in the Tinkers Creek watershed, at a site on Tinkers Creek downstream from all WWTP discharges, and at one reference site each in two nearby watersheds (Yellow Creek and Furnace Run) that drain to the Cuyahoga River. Streambed-sediment samples also were collected at each site when the canisters were retrieved. POCIS and SPMDs are referred to as 'passive samplers' because they sample compounds that they are exposed to without use of mechanical or moving parts. OWCs detected in POCIS and SPMD extracts are referred to in this report as 'detections in water' because both POCIS and SPMDs provided time-weighted measures of concentration in the stream over the exposure period. Streambed sediments also reflect exposure to OWCs in the stream over a long period of time and provide another OWC exposure pathway for aquatic organisms. Four separate laboratory methods were used to analyze for 32 antibiotic, 20 pharmaceutical, 57 to 66 wastewater, and 33 hydrophobic compounds. POCIS and streambed-sediment extracts were analyzed by both the pharmaceutical and wastewater methods. POCIS extracts also were analyzed by the antibiotic method, and SPMD extracts were analyzed by the hydrophobic-compound method. Analytes associated with a given laboratory method are referred to in aggregate by the method name (for example, antibiotic-method analytes are referred to as 'antibiotic compounds') even though some analytes associated with the method may not be strictly classified as such. In addition, some compounds were included in the analyte list for more than one laboratory method. For a given sample matrix, individual compounds detected by more than one analytical method are included independently in counts for each method. A total of 12 antibiotic, 20 pharmaceutical, 41 wastewater, and 22 hydrophobic compounds were detected in water at one or more sites. Eight pharmaceutical and 37 wastewater compounds were detected in streambed sediments. The numbers of detections at reference sites tended to be in the low range of detection counts observed in the Tinkers Creek watershed for a given analytical method. Also, the total numbers of compounds detected in water and sediment at the reference sites were less than the total numbers of compounds detected at sites in the Tinkers Creek watershed. With the exception of hydrophobic compounds, it was common at most sites to have more compounds detected in samples collected downstream from WWTP outfalls than in corresponding samples collected upstream from the outfalls. This was particularly true for antibiotic, pharmaceutical, and wastewater compounds in water. In contrast, it was common to have more hydrophobic compounds detected in samples collected upstream from WWTP outfalls than downstream. Caffeine, fluoranthene, N,N-diethyl-meta-toluamide (DEET), phenanthrene, and pyrene were detected in water at all sites in the Tinkers Creek watershed, irrespective of whether the site was upstream or downs

Ohio↗

USGS2017

Nutrient and pesticide contamination bias estimated from field blanks collected at surface-water sites in U.S. Geological Survey Water-Quality Networks, 2002–12

Potential contamination bias was estimated for 8 nutrient analytes and 40 pesticides in stream water collected by the U.S. Geological Survey at 147 stream sites from across the United States, and representing a variety of hydrologic conditions and site types, for water years 2002–12. This study updates previous U.S. Geological Survey evaluations of potential contamination bias for nutrients and pesticides. Contamination is potentially introduced to water samples by exposure to airborne gases and particulates, from inadequate cleaning of sampling or analytic equipment, and from inadvertent sources during sample collection, field processing, shipment, and laboratory analysis. Potential contamination bias, based on frequency and magnitude of detections in field blanks, is used to determine whether or under what conditions environmental data might need to be qualified for the interpretation of results in the context of comparisons with background levels, drinking-water standards, aquatic-life criteria or benchmarks, or human-health benchmarks. Environmental samples for which contamination bias as determined in this report applies are those from historical U.S. Geological Survey water-quality networks or programs that were collected during the same time frame and according to the same protocols and that were analyzed in the same laboratory as field blanks described in this report. Results from field blanks for ammonia, nitrite, nitrite plus nitrate, orthophosphate, and total phosphorus were partitioned by analytical method; results from the most commonly used analytical method for total phosphorus were further partitioned by date. Depending on the analytical method, 3.8, 9.2, or 26.9 percent of environmental samples, the last of these percentages pertaining to all results from 2007 through 2012, were potentially affected by ammonia contamination. Nitrite contamination potentially affected up to 2.6 percent of environmental samples collected between 2002 and 2006 and affected about 3.3 percent of samples collected between 2007 and 2012. The percentages of environmental samples collected between 2002 and 2011 that were potentially affected by nitrite plus nitrate contamination were 7.3 for samples analyzed with the low-level method and 0.4 for samples analyzed with the standard-level method. These percentages increased to 14.8 and 2.2 for samples collected in 2012 and analyzed using replacement low- and standard-level methods, respectively. The maximum potentially affected concentrations for nitrite and for nitrite plus nitrate were much less than their respective maximum contamination levels for drinking-water standards. Although contamination from particulate nitrogen can potentially affect up to 21.2 percent and that from total Kjeldahl nitrogen can affect up to 16.5 percent of environmental samples, there are no critical or background levels for these substances. For total nitrogen, orthophosphate, and total phosphorus, contamination in a small percentage of environmental samples might be consequential for comparisons relative to impairment risks or background levels. At the low ends of the respective ranges of impairment risk for these nutrients, contamination in up to 5 percent of stream samples could account for at least 23 percent of measured concentrations of total nitrogen, for at least 40 or 90 percent of concentrations of orthophosphate, depending on the analytical method, and for 31 to 76 percent of concentrations of total phosphorus, depending on the time period. Twenty-six pesticides had no detections in field blanks. Atrazine with 12 and metolachlor with 11 had the highest number of detections, mostly occurring in spring or early summer. At a 99-percent level of confidence, contamination was estimated to be no greater than the detection limit in at least 98 percent of all samples for 38 of 40 pesticides. For metolachlor and atrazine, potential contamination was no greater than 0.0053 and 0.0093 micrograms per liter in 98 percent of samples. For 11 of 14 pesticides with at least one detection, the maximum potentially affected concentration of the environmental sample was less than their respective human-health or aquatic-life benchmarks. Small percentages of environmental samples had concentrations high enough that atrazine contamination potentially could account for the entire aquatic-life benchmark for acute effects on nonvascular plants, that dieldrin contamination could account for up to 100 percent of the cancer health-based screening level, or that chlorpyrifos contamination could account for 13 or 12 percent of the concentrations in the aquatic-life benchmarks for chronic effects on invertebrates or the criterion continuous concentration for chronic effects on aquatic life.

Scientific Investigations Report↗

USGS2009

Determination of glyphosate, its degradation product aminomethylphosphonic acid, and glufosinate, in water by isotope dilution and online solid-phase extraction and liquid chromatography/tandem mass spectrometry

The U.S. Geological Survey method (0-2141-09) presented is approved for the determination of glyphosate, its degradation product aminomethylphosphonic acid (AMPA), and glufosinate in water. It was was validated to demonstrate the method detection levels (MDL), compare isotope dilution to standard addition, and evaluate method and compound stability. The original method USGS analytical method 0-2136-01 was developed using liquid chromatography/mass spectrometry and quantitation by standard addition. Lower method detection levels and increased specificity were achieved in the modified method, 0-2141-09, by using liquid chromatography/tandem mass spectrometry (LC/MS/MS). The use of isotope dilution for glyphosate and AMPA and pseudo isotope dilution of glufosinate in place of standard addition was evaluated. Stable-isotope labeled AMPA and glyphosate were used as the isotope dilution standards. In addition, the stability of glyphosate and AMPA was studied in raw filtered and derivatized water samples. The stable-isotope labeled glyphosate and AMPA standards were added to each water sample and the samples then derivatized with 9-fluorenylmethylchloroformate. After derivatization, samples were concentrated using automated online solid-phase extraction (SPE) followed by elution in-line with the LC mobile phase; the compounds separated and then were analyzed by LC/MS/MS using electrospray ionization in negative-ion mode with multiple-reaction monitoring. The deprotonated derivatized parent molecule and two daughter-ion transition pairs were identified and optimized for glyphosate, AMPA, glufosinate, and the glyphosate and AMPA stable-isotope labeled internal standards. Quantitative comparison between standard addition and isotope dilution was conducted using 473 samples analyzed between April 2004 and June 2006. The mean percent difference and relative standard deviation between the two quantitation methods was 7.6 plus or minus 6.30 (n = 179), AMPA 9.6 plus or minus 8.35 (n = 206), and glufosinate 9.3 plus or minus 9.16 (n = 16). The analytical variation of the method, comparison of quantitation by isotope dilution and multipoint linear regressed standard curves, and method detection levels were evaluated by analyzing six sets of distilled-water, groundwater, and surface-water samples spiked in duplicate at 0.0, 0.05, 0.10 and 0.50 microgram per liter and analyzed on 6 different days during 1 month. The grand means of the normalized concentration percentage recovery for glyphosate, AMPA, and glufosinate among all three matrices and spiked concentrations ranged from 99 to 114 plus or minus 2 to 7 percent of the expected spiked concentration. The grand mean of the percentage difference between concentrations calculated by standard addition and linear regressed multipoint standard curves ranged from 8 to 15 plus or minus 2 to 9 percent for the three compounds. The method reporting levels calculated from all the 0.05- microgram per liter spiked samples were 0.02 microgram per liter for all three compounds. Compound stability experiments were conducted on 10 samples derivatized four times for periods between 136 to 269 days. The glyphosate and AMPA concentrations remained relatively constant in samples held up to 136 days before derivatization. The half life of glyphosate varied from 169 to 223 days in the underivatized samples. Derivatized samples were analyzed the day after derivitization, and again 54 and 64 days after derivatization. The derivatized samples analyzed at days 52 and 64 were within 20 percent of the concentrations of the derivatized samples analyzed the day after derivatization.

Techniques and Methods↗

USGS2012

Determination of steroid hormones and related compounds in filtered and unfiltered water by solid-phase extraction, derivatization, and gas chromatography with tandem mass spectrometry

A new analytical method has been developed and implemented at the U.S. Geological Survey National Water Quality Laboratory that determines a suite of 20 steroid hormones and related compounds in filtered water (using laboratory schedule 2434) and in unfiltered water (using laboratory schedule 4434). This report documents the procedures and initial performance data for the method and provides guidance on application of the method and considerations of data quality in relation to data interpretation. The analytical method determines 6 natural and 3 synthetic estrogen compounds, 6 natural androgens, 1 natural and 1 synthetic progestin compound, and 2 sterols: cholesterol and 3--coprostanol. These two sterols have limited biological activity but typically are abundant in wastewater effluents and serve as useful tracers. Bisphenol A, an industrial chemical used primarily to produce polycarbonate plastic and epoxy resins and that has been shown to have estrogenic activity, also is determined by the method. A technique referred to as isotope-dilution quantification is used to improve quantitative accuracy by accounting for sample-specific procedural losses in the determined analyte concentration. Briefly, deuterium- or carbon-13-labeled isotope-dilution standards (IDSs), all of which are direct or chemically similar isotopic analogs of the method analytes, are added to all environmental and quality-control and quality-assurance samples before extraction. Method analytes and IDS compounds are isolated from filtered or unfiltered water by solid-phase extraction onto an octadecylsilyl disk, overlain with a graded glass-fiber filter to facilitate extraction of unfiltered sample matrices. The disks are eluted with methanol, and the extract is evaporated to dryness, reconstituted in solvent, passed through a Florisil solid-phase extraction column to remove polar organic interferences, and again evaporated to dryness in a reaction vial. The method compounds are reacted with activated -methyl--trimethylsilyl trifluoroacetamide at 65 degrees Celsius for 1 hour to form trimethylsilyl or trimethylsilyl-enol ether derivatives that are more amenable to gas chromatographic separation than the underivatized compounds. Analysis is carried out by gas chromatography with tandem mass spectrometry using calibration standards that are derivatized concurrently with the sample extracts. Analyte concentrations are quantified relative to specific IDS compounds in the sample, which directly compensate for procedural losses (incomplete recovery) in the determined and reported analyte concentrations. Thus, reported analyte concentrations (or analyte recoveries for spiked samples) are corrected based on recovery of the corresponding IDS compound during the quantification process. Recovery for each IDS compound is reported for each sample and represents an absolute recovery in a manner comparable to surrogate recoveries for other organic methods used by the National Water Quality Laboratory. Thus, IDS recoveries provide a useful tool for evaluating sample-specific analytical performance from an absolute mass recovery standpoint. IDS absolute recovery will differ and typically be lower than the corresponding analyte’s method recovery in spiked samples. However, additional correction of reported analyte concentrations is unnecessary and inappropriate because the analyte concentration (or recovery) already is compensated for by the isotope-dilution quantification procedure. Method analytes were spiked at 10 and 100 nanograms per liter (ng/L) for most analytes (10 times greater spike levels were used for bisphenol A and 100 times greater spike levels were used for 3--coprostanol and cholesterol) into the following validation-sample matrices: reagent water, wastewater-affected surface water, a secondary-treated wastewater effluent, and a primary (no biological treatment) wastewater effluent. Overall method recovery for all analytes in these matrices averaged 100 percent, with overall relative standard deviation of 28 percent. Mean recoveries of the 20 individual analytes for spiked reagent-water samples prepared along with field samples and analyzed in 2009–2010 ranged from 84–104 percent, with relative standard deviations of 6–36 percent. Concentrations for two analytes, equilin and progesterone, are reported as estimated because these analytes had excessive bias or variability, or both. Additional database coding is applied to other reported analyte data as needed, based on sample-specific IDS recovery performance. Detection levels were derived statistically by fortifying reagent water at six different levels (0.1 to 4 ng/L) and range from about 0.4 to 4 ng/L for 16 analytes. Interim reporting levels applied to analytes in this report range from 0.8 to 8 ng/L. Bisphenol A and the sterols (cholesterol and 3-beta-coprostanol) were consistently detected in laboratory and field blanks. The minimum reporting levels were set at 100 ng/L for bisphenol A and at 200 ng/L for the two sterols to prevent any bias associated with the presence of these compounds in the blanks. A minimum reporting level of 2 ng/L was set for 11-ketotestosterone to minimize false positive risk from an interfering siloxane compound emanating as chromatographic-column bleed, from vial septum material, or from other sources at no more than 1 ng/L.

Techniques and Methods↗

USGS1994

Maps showing interpretation, using R-mode factor analysis, of trace-element abundances in heavy-mineral concentrate samples, Delta 1° x 2° quadrangle, Utah

A set of heavy-mineral concentrate data for the Delta 1° x 2° quadrangle, Utah Conterminous U.S. Mineral Assessment Program (CUSMAP) project was compiled from results of analyses of samples collected during the National Uranium Resource Evaluation Program (SURE), as well as results obtained from samples collected more recently by the USGS. Data results, sampling methods, and analytical methods are provided in Abrogast and others, 1993; 1990; 1988a; 1988b). A similar report, discussing results obtained from stream-sediment samples, is presented in Zimbelman (1993a). The Delta 1° x 2° quadrangle, Utah (figure 1) contains a variety of hydrothermal mineral deposit types, including porphyry-, vein-, replacement-, and Carlin-type deposits. These deposit types have been worked for commodities including gold, silver, beryllium, uranium, lead, zinc, copper, manganese, and cadmium (Lindsey, 1977; Morris and Mogensen, 1978; Zimbelman and others, 1990; Zimbelman and others, 1988). Heavy-mineral concentrate and stream-sediment samples derived from these hydrothermally altered rocks typically contain many geochemical anomalies (for example, see Zimbelman 1993b, c, d). Element associations characterizing lithology and hydrothermal mineral deposits can be distinguished using R-mode factor analysis. This tool often is useful in reconnaissance-scale surveys where sample anomalies are often weak. and single-element distributions may not help to delineate targets. R-mode factors analysis can help identify geologic trends and areas most likely to contain the mineral deposits. R-mode factor analysis was performed on a data set of results of analyses for 19 elements in 643 samples and produced a six-factor model. These six factors represent the geochemical contributions to the data set provided by lithologic and mineralization processes, The distribution of samples that contain high scores for mineralization-related factors is widespread in the Delta quadrangle. These sample sites are though to relate to both known prospect and mineralization areas, as well as define new areas that are geochemically favorable to contain altered or mineralized rocks.

Utah↗

USGS2009

Adjustment of pesticide concentrations for temporal changes in analytical recovery, 1992-2006

Recovery is the proportion of a target analyte that is quantified by an analytical method and is a primary indicator of the analytical bias of a measurement. Recovery is measured by analysis of quality-control (QC) water samples that have known amounts of target analytes added ('spiked' QC samples). For pesticides, recovery is the measured amount of pesticide in the spiked QC sample expressed as percentage of the amount spiked, ideally 100 percent. Temporal changes in recovery have the potential to adversely affect time-trend analysis of pesticide concentrations by introducing trends in environmental concentrations that are caused by trends in performance of the analytical method rather than by trends in pesticide use or other environmental conditions. This report examines temporal changes in the recovery of 44 pesticides and 8 pesticide degradates (hereafter referred to as 'pesticides') that were selected for a national analysis of time trends in pesticide concentrations in streams. Water samples were analyzed for these pesticides from 1992 to 2006 by gas chromatography/mass spectrometry. Recovery was measured by analysis of pesticide-spiked QC water samples. Temporal changes in pesticide recovery were investigated by calculating robust, locally weighted scatterplot smooths (lowess smooths) for the time series of pesticide recoveries in 5,132 laboratory reagent spikes; 1,234 stream-water matrix spikes; and 863 groundwater matrix spikes. A 10-percent smoothing window was selected to show broad, 6- to 12-month time scale changes in recovery for most of the 52 pesticides. Temporal patterns in recovery were similar (in phase) for laboratory reagent spikes and for matrix spikes for most pesticides. In-phase temporal changes among spike types support the hypothesis that temporal change in method performance is the primary cause of temporal change in recovery. Although temporal patterns of recovery were in phase for most pesticides, recovery in matrix spikes was greater than recovery in reagent spikes for nearly every pesticide. Models of recovery based on matrix spikes are deemed more appropriate for adjusting concentrations of pesticides measured in groundwater and stream-water samples than models based on laboratory reagent spikes because (1) matrix spikes are expected to more closely match the matrix of environmental water samples than are reagent spikes and (2) method performance is often matrix dependent, as was shown by higher recovery in matrix spikes for most of the pesticides. Models of recovery, based on lowess smooths of matrix spikes, were developed separately for groundwater and stream-water samples. The models of recovery can be used to adjust concentrations of pesticides measured in groundwater or stream-water samples to 100 percent recovery to compensate for temporal changes in the performance (bias) of the analytical method.

Scientific Investigations Report↗

USGS2011

Adjustment of pesticide concentrations for temporal changes in analytical recovery, 1992–2010

Data Series↗

USGS1977

Methods for determination of radioactive substances in water and fluvial sediments

Analytical methods for the determination of some of the more important components of fission or neutron activation product radioactivity and of natural radioactivity found in water are reported. The report for each analytical method includes conditions for application of the method, a summary of the method, interferences, required apparatus and reagents, analytical procedures, calculations, reporting of results, and estimation of precision. The fission product isotopes considered are cesium-137, strontium-90, and ruthenium-106. The natural radioelements and isotopes considered are uranium, lead-210, radium-226, radium-228, tritium, and carbon-14. A gross radioactivity survey method and a uranium isotope ratio method are given. When two analytical methods are in routine use for an individual isotope, both methods are reported with identification of the specific areas of application of each. Techniques for the collection and preservation of water samples to be analyzed for radioactivity are discussed.

Techniques of Water-Resources Investigations↗

USGS2009

Bacteria holding times for fecal coliform by mFC agar method and total coliform and Escherichia coli by Colilert®-18 Quanti-Tray® method

Bacteria holding-time experiments of up to 62 h were performed on five surface-water samples from four urban stream sites in the vicinity of Atlanta, GA, USA that had relatively high densities of coliform bacteria ( Escherichia coli densities were all well above the US Environmental Protection Agency criterion of 126 colonies (100 ml)  − 1 for recreational waters). Holding-time experiments were done for fecal coliform using the membrane filtration modified fecal coliform (mFC) agar method and for total coliform and E. coli using the Colilert ® -18 Quanti-Tray ® method. The precisions of these analytical methods were quantified. Precisions determined for fecal coliform indicated that the upper bound of the ideal range of counts could reasonably be extended upward and would improve precision. For the Colilert ® -18 method, analytical precisions were similar to the theoretical precisions for this method. Fecal and total coliform densities did not change significantly with holding times up to about 27 h. Limited information indicated that fecal coliform densities might be stable for holding times of up to 62 h, whereas total coliform densities might not be stable for holding times greater than about 27 h. E. coli densities were stable for holding times of up to 18 h—a shorter period than indicated from a previous studies. These results should be applicable to non-regulatory monitoring sampling designs for similar urban surface-water sample types.

Environmental Monitoring and Assessment↗

USGS1954

U.S. Geological Survey Trace Elements and related reports through 1953

This report combines and brings up-to-date the information previously given in Trace Elements Investigations Report 325, "Numerical list of U.S. Geological Survey Trace Elements Reports to April 30, 1953," and Trace Elements Investigations Report 301, "Topical index and bibliography of U.S. Geological Survey Trace Elements and related reports." Part I is a numerical list of U.S. Geological Survey Trace Elements Investigations and Memorandum reports. It supersedes TEI-325. This part lists not only reports (followed by a date) that have been transmitted to the U.S. Atomic Energy Commission, but also reports in preparation (followed by an asterisk) for which tentative titles were available on December 31, 1953. Reports that have been published are indicated by the abbreviation of the medium of publication. (See also part II.) Part II is a reference guide to Trace Elements and related reports that are available to the public; this part supersedes Part 2 of the TEI-301 (published as Geological survey Circular 281). These reports are grouped according to the type of publication or release. Abstracts published in Nuclear Science Abstracts are not included in Part II, although certain TEI and TEM reports, the abstracts of which have been published in NSA, are so indicated in Part I. Publications in process on December 31, 1953, are designated by an asterisk. Part III is a finding list of states, areas, and subjects. It is based on information derived mostly from the titles of reports and, where titles are of a general nature, from a cursory review of the reports. This list is not a complete index of the information given in Trace Elements and related reports, but is designed to find subjects of major interest. Because of the numerous entries for Colorado and Utah, information has been listed by counties and, where possible, by subject under these states. Other states have county listings only if a county is included in the title of a report; otherwise, areas may be listed separately under the state. Major subjects are listed separately in the index and also where appropriate under states. Analytical methods and subjects related to analytical research are listed under Analytical Methods and Research, but not separately throughout the index. Most mineralogic studies are included under the heading Mineralogy, but are not necessarily listed according to location. Part IV is a finding list of authors. The words “with” and “and” are used to indicate seniority of authorship. For example, a listing of Jones and Brown indicates that Jones is the senior author. A listing of Jones with Brown indicates that Brown is the senior author. In both parts III and IV all Trace Elements reports are listed, as well as other related reports that have not been issued as Trace Elements reports. The following standard abbreviations have been used: TEI, Trace Elements Investigations report; TEM, Trace Elements Memorandum report; P, Professional Paper; B, Bulletin; C, Circular; J, Journal; OF, open file; TIS, Technical Information Service release; NSA, Nuclear Science Abstracts; QM, Quadrangle Map Series; and OM, Oil and Gas map or Mineral Investigations map or report.

Trace Elements Investigations↗

USGS1955

U.S. Geological Survey Trace Elements and related reports through 1954

This report supersedes TEI-400, "U.S. Geological Survey Trace Elements and related reports through 1953." Part I is a numerical list of U.S. Geological Survey Trace Elements Investigations and Memorandum reports. This part lists not only reports (followed by a date) that have been transmitted to the U.S> Atomic Energy Commission, but also reports in preparation (followed by an asterisk) for which tentative titles were available on December 31, 1954. If a report, or portion of a report, has been published, the fact is indicated by the abbreviation of the medium of publication. (See also Part II.) Part II is a reference guide to Trace Elements and related reports that are available to the public (this part supersedes Part I of Bulletin 1019-B). These reports are grouped according to the type of publication or release. If a report, or portion of the report, has been published in more than one form, appropriate cross-references are given to indicate the other forms of publication. Abstracts published in Nuclear Science Abstracts are not included in Part II; however, if the abstract of a Trace Elements report has been published in NSA, the fact is indicated in Part I. Publications in process on December 31, 1954, are designated by an asterisk. Part III is a finding list of states, areas, and subjects and supersedes Part II of Bulletin 1019-B. It is based on information derived mostly from the titles of reports and, where titles are of general nature, from a cursory review of the reports. This list is not a complete index of the information given in Trace Elements and related reports, but is designed to find subjects of major interest, Because of the numerous entries for Colorado and Utah, information has been listed by counties and, where possible, by subject under these states. Other states have county listings only if a county is included in the title of a report; otherwise, area may be listed separately under the state. Major subjects are listed separately in the index and also, where appropriate under states. Analytical methods and subjects related to analytical research are listed under Analytical Methods and Research, but not separately throughout the index. Most mineralogic studies are included under the heading Mineralogy, but are not necessarily listed according to location. Part IV is an author index. The words “with” and “and” are used to indicate seniority of authorship. For example, a listing of Smith and Brown indicated that Smith is the senior author. A listing of Smith with Brown indicates that Brown is the senior author. In both parts III and IV all Trace Elements reports are listed, as well as other related reports that have not been issued as Trace Elements reports. The following abbreviations have been used: TEI, Trace Elements Investigations report; TEM, Trace Elements Memorandum report; OF, open file; TIS, Technical Information Service release; C, Circular; B, Bulletin; P, Professional Paper; MC, Maps and Charts; J, Journal; and NSA, Nuclear Science Abstracts.

Trace Elements Investigations↗

USGS2022

San Francisco Estuary chlorophyll sensor and sample analysis intercomparison

This report presents an assessment of chlorophyll collection methods and anonymous results of field and laboratory comparisons in 2018 - 2019 by agencies in the San Francisco Estuary (SFE). The methods assessment and comparison exercises, with funding provided by the Delta Regional Monitoring Program and Bay Nutrient Management Strategy and in-kind contributions from participating agencies, are a first step to facilitate future comparisons and syntheses of data and inform best science practices in the region. In situ sonde comparison exercises found general agreement between two models of Yellow Springs Instrument (YSI) sensors, but the newer sensor (EXO v2 - total algae) measured higher chlorophyll fluorescence (fCHL) relative to the older YSI sensor (6-series 6025). Results may be attributed to the use of a two-point calibration and the fluorescence response of algal cultures in sensor development by the manufacturer. The laboratory comparison included participation by 12 distinct field - laboratory pairs (or groups), with one group analyzing filters using two analytical methods. Filters were collected in triplicate across three sampling events in 2018, and all sample results were pooled together. Results of statistical analyses indicated that nominal filter pore size, the grinding method associated with pigment extraction, and analytical methods do not introduce variability to the chlorophyll-a measurement (Chl-a). When Chl-a results were assessed by sample event, however, significant differences between nominal pore size and analytical methods existed; these differences could be attributed to the small sample size per event. Consistent reporting units and high-concentration calibration standards for field sensors among data collection agencies would improve the consistency and comparability of data collected in the SFE. More routine split sampling events, longer term sensor comparison exercises, and further processing and analytical comparisons that control for individual filterers may also enhance comparability in the region.

California↗

USGS2011

Sources and preparation of data for assessing trends in concentrations of pesticides in streams of the United States, 1992–2010

This report updates a previously published water-quality dataset of 44 commonly used pesticides and 8 pesticide degradates suitable for a national assessment of trends in pesticide concentrations in streams of the United States. Water-quality samples collected from January 1992 through September 2010 at stream-water sites of the U.S. Geological Survey (USGS) National Water-Quality Assessment (NAWQA) Program and the National Stream Quality Accounting Network (NASQAN) were compiled, reviewed, selected, and prepared for trend analysis. The principal steps in data review for trend analysis were to (1) identify analytical schedule, (2) verify sample-level coding, (3) exclude inappropriate samples or results, (4) review pesticide detections per sample, (5) review high pesticide concentrations, and (6) review the spatial and temporal extent of NAWQA pesticide data and selection of analytical methods for trend analysis. The principal steps in data preparation for trend analysis were to (1) select stream-water sites for trend analysis, (2) round concentrations to a consistent level of precision for the concentration range, (3) identify routine reporting levels used to report nondetections unaffected by matrix interference, (4) reassign the concentration value for routine nondetections to the maximum value of the long-term method detection level (maxLT-MDL), (5) adjust concentrations to compensate for temporal changes in bias of recovery of the gas chromatography/mass spectrometry (GCMS) analytical method, and (6) identify samples considered inappropriate for trend analysis. Samples analyzed at the USGS National Water Quality Laboratory (NWQL) by the GCMS analytical method were the most extensive in time and space and, consequently, were selected for trend analysis. Stream-water sites with 3 or more water years of data with six or more samples per year were selected for pesticide trend analysis. The selection criteria described in the report produced a dataset of 21,988 pesticide samples at 212 stream-water sites. Only 21,144 pesticide samples, however, are considered appropriate for trend analysis.

Data Series↗

USGS1989

Evaluation of methods used from 1965 through 1982 to determine inorganic constituents in water samples

Since 1962, the U.S. Geological Survey has prepared and distributed Standard Reference Water Samples (SRWS) to participating laboratories in order to alert them to possible analytical deficiencies. This report marks the first time that a concentrated effort has been made to examine and compare the SRWS data for each constituent by the analytical method that was used to obtain the data. Unlike laboratories that participate in interlaboratory studies that are designed to determine the precision and accuracy of a particular analytical method, laboratories that participate in the SRWS program are allowed to select the method used to analyze a reference sample and are requested to report the method used. Data for a particular method could not be compared with a 'true' value because the data were obtained from analyses of reference samples that were prepared using natural waters; however, where possible a comparison was made between the mean concentrations obtained by the various analytical methods that were used to determine each constituent. Where enough information is available, models for predicting the precisions of the methods have been developed, and the precisions have been compared. In addition to the data presented in the reports, this evaluation provides a good indication of methods that were used routinely to analyze water samples during the 18 years of study.

Water Supply Paper↗

USGS2010

Antibiotic, pharmaceutical, and wastewater-compound data for Michigan, 1998-2005

Beginning in the late 1990's, the U.S. Geological Survey began to develop analytical methods to detect, at concentrations less than 1 microgram per liter (ug/L), emerging water contaminants such as pharmaceuticals, personal-care chemicals, and a variety of other chemicals associated with various human and animal sources. During 1998-2005, the U.S. Geological Survey analyzed the following Michigan water samples: 41 samples for antibiotic compounds, 28 samples for pharmaceutical compounds, 46 unfiltered samples for wastewater compounds (dissolved and suspended compounds), and 113 filtered samples for wastewater compounds (dissolved constituents only). The purpose of this report is to summarize the status of emerging contaminants in Michigan waters based on data from several different project-specific sample-collection efforts in Michigan during an 8-year period. During the course of the 8-year sampling effort, antibiotics were determined at 20 surface-water sites and 2 groundwater sites, pharmaceuticals were determined at 11 surface-water sites, wastewater compounds in unfiltered water were determined at 31 surface-water sites, and wastewater compounds in filtered water were determined at 40 surface-water and 4 groundwater sites. Some sites were visited only once, but others were visited multiple times. A variety of quality-assurance samples also were collected. This report describes the analytical methods used, describes the variations in analytical methods and reporting levels during the 8-year period, and summarizes all data using current (2009) reporting criteria. Very few chemicals were detected at concentrations greater than current laboratory reporting levels, which currently vary from a low of 0.005 ug/L for some antibiotics to 5 ug/L for some wastewater compounds. Nevertheless, 10 of 51 chemicals in the antibiotics analysis, 9 of 14 chemicals in the pharmaceuticals analysis, 34 of 67 chemicals in the unfiltered-wastewater analysis, and 56 of 62 chemicals in the filtered-wastewater analysis were detected. Antibiotics were detected at 7 of 20 tested surface-water sites, but none were detected in 2 groundwater samples. Pharmaceuticals were detected at 7 of 11 surface-water sites. Wastewater compounds were detected at 25 of 31 sites for which unfiltered water samples were analyzed and at least once at all 40 surface-water sites and all 4 groundwater sites for which filtered water samples were analyzed. Overall, the chemicals detected most frequently in Michigan waters were similar to those reported frequently in other studies nationwide. Patterns of chemical detections were site specific and appear to be related to local sources, overall land use, and hydrologic conditions at the time of sampling. Field-blank results provide important information for the design of future sampling programs in Michigan and demonstrate the need for careful field-study design. Field-replicate results indicated substantial confidence regarding the presence or absence of the many chemicals tested. Overall, data reported herein indicate that a wide array of antibiotic, pharmaceutical, and organic wastewater compounds occur in Michigan waters. Patterns of occurrence, with respect to hydrologic, land use, and source variables, generally appear to be similar for Michigan as for other sampled waters across the United States. The data reported herein can serve as a basis for future studies in Michigan.

Michigan↗

USGS2006

Occurrence of organic wastewater compounds in drinking water, wastewater effluent, and the Big Sioux River in or near Sioux Falls, South Dakota, 2001-2004

The U.S. Geological Survey (USGS) in cooperation with the city of Sioux Falls conducted several rounds of sampling to determine the occurrence of organic wastewater compounds (OWCs) in the city of Sioux Falls drinking water and waste-water effluent, and the Big Sioux River in or near Sioux Falls during August 2001 through May 2004. Water samples were collected during both base-flow and storm-runoff conditions. Water samples were collected at 8 sites, which included 4 sites upstream from the wastewater treatment plant (WWTP) discharge, 2 sites downstream from the WWTP discharge, 1 finished drinking-water site, and 1 WWTP effluent (WWE) site. A total of 125 different OWCs were analyzed for in this study using five different analytical methods. Analyses for OWCs were performed at USGS laboratories that are developing and/or refining small-concentration (less than 1 microgram per liter (ug/L)) analytical methods. The OWCs were classified into six compound classes: human pharmaceutical compounds (HPCs); human and veterinary antibiotic compounds (HVACs); major agricultural herbicides (MAHs); household, industrial,and minor agricultural compounds (HIACs); polyaromatic hydrocarbons (PAHs); and sterol compounds (SCs). Some of the compounds in the HPC, MAH, HIAC, and PAH classes are suspected of being endocrine-disrupting compounds (EDCs). Of the 125 different OWCs analyzed for in this study, 81 OWCs had one or more detections in environmental samples reported by the laboratories, and of those 81 OWCs, 63 had acceptable analytical method performance, were detected at concentrations greater than the study reporting levels, and were included in analyses and discussion related to occurrence of OWCs in drinking water, wastewater effluent, and the Big Sioux River. OWCs in all compound classes were detected in water samples from sampling sites in the Sioux Falls area. For the five sampling periods when samples were collected from the Sioux Falls finished drinking water, only one OWC was detected at a concentration greater than the study reporting level (metolachlor; 0.0040 ug/L). During base-flow conditions, Big Sioux River sites upstream from the WWTP discharge had OWC contributions that primarily were from nonpoint animal or crop agriculture sources or had OWC concentrations that were minimal. The influence of the WWTP discharge on OWCs at downstream river sites during base-flow conditions ranged from minimal influence to substantial influence depending on the sampling period. During runoff conditions, OWCs at sites upstream from the WWTP discharge probably were primarily contributed by nonpoint animal and/or crop agriculture sources and possibly by stormwater runoff from nearby roads. OWCs at sites downstream from the WWTP discharge probably were contributed by sources other than the WWTP effluent discharge, such as stormwater runoff from urban and/or agriculture areas and/or resuspension of OWCs adsorbed to sediment deposited in the Big Sioux River. OWC loads generally were substantially smaller for upstream sites than downstream sites during both base-flow and runoff conditions.discharge had OWC contributions that primarily were from nonpoint animal or crop agriculture sources or had OWC concentrations that were minimal. The influence of the WWTP discharge on OWCs at downstream river sites during base-flow conditions ranged from minimal influence to substantial influence depending on the sampling period. During runoff conditions, OWCs at sites upstream from the WWTP discharge probably were primarily contributed by nonpoint animal and/or crop agriculture sources and possibly by stormwater runoff from nearby roads. OWCs at sites downstream from the WWTP discharge probably were contributed by sources other than the WWTP effluent discharge, such as stormwater runoff from urban and/or agriculture areas and/or resuspension of OWCs adsorbed to sediment deposited in the Big Sioux River. OWC loads generally were substantially smaller for

South Dakota↗

USGS2000

Comparability of suspended-sediment concentration and total suspended solids data

Two laboratory analytical methods — suspended-sediment concentration (SSC) and total suspended solids (TSS) — are predominantly used to quantify concentrations of suspended solid-phase material in surface waters of the United States. The analytical methods differ. SSC data are produced by measuring the dry weight of all the sediment from a known volume of a water-sediment mixture. TSS data are produced by several methods, most of which entail measuring the dry weight of sediment from a known volume of a subsample of the original. An evaluation of 3,235 paired SSC and TSS data, of which 860 SSC values include percentages of sand-size material, shows bias in the relation between SSC and TSS —SSC values tend to increase at a greater rate than their corresponding paired TSS values. As sand-size material in samples exceeds about a quarter of the sediment dry weight, SSC values tend to exceed their corresponding paired TSS values. TSS analyses of three sets of quality-control samples (35 samples) showed unexpectedly small sediment recoveries and relatively large variances in the TSS data. Two quality-control data sets (18 samples) that were analyzed for SSC showed both slightly deficient sediment recoveries, and variances that are characteristic of most other quality-control data compiled as part of the U.S. Geological Survey’s National Sediment Laboratory Quality Assurance Program. The method for determining TSS, which was originally designed for analyses of wastewater samples, is shown to be fundamentally unreliable for the analysis of natural-water samples. In contrast, the method for determining SSC produces relatively reliable results for samples of natural water, regardless of the amount or percentage of sand-size material in the samples. SSC and TSS data collected from natural water are not comparable and should not be used interchangeably. The accuracy and comparability of suspended solid-phase concentrations of the Nation’s natural waters would be greatly enhanced if all these data were produced by the SSC analytical method.

Water-Resources Investigations Report↗