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At least 955 records · Page 53Linked to original sources
USGS2002

Determination of methyl mercury by aqueous phase ethylation, followed by gas chromatographic separation with cold vapor atomic fluorescence detection

A recent national sampling of streams in the United States revealed low methyl mercury concentrations in surface waters. The resulting median and mean concentrations, calculated from 104 samples, were 0.06 nanograms per liter (ng/L) and 0.15 ng/L, respectively. This level of methyl mercury in surface water in the United States has created a need for analytical techniques capable of detecting sub-nanogram per liter concentrations. In an attempt to create a U.S. Geological Survey approved method, the Wisconsin District Mercury Laboratory has adapted a distillation/ethylation/ gas-phase separation method with cold vapor atomic fluorescence spectroscopy detection for the determination of methyl mercury in filtered and unfiltered waters. This method is described in this report. Based on multiple analyses of surface water and ground-water samples, a method detection limit of 0.04 ng/L was established. Precision and accuracy were evaluated for the method using both spiked and unspiked ground-water and surface-water samples. The percent relative standard deviations ranged from 10.2 to 15.6 for all analyses at all concentrations. Average recoveries obtained for the spiked matrices ranged from 88.8 to 117 percent. The precision and accuracy ranges are within the acceptable method-performance limits. Considering the demonstrated detection limit, precision, and accuracy, the method is an effective means to quantify methyl mercury in waters at or below environmentally relevant concentrations

Open-File Report↗
USGS1994

Using analytical services at the National Water Quality Laboratory

The National Water Quality Laboratory (NWQL) offers a variety of analytical services for the determination of constituents in samples of water, sediment, and biological material. As technology has advanced, many new methods have been introduced but not always incorporated into plans and schedules developed in the districts. The strengths and weaknesses of many different techniques are discussed and evaluated to promote a broad understanding of the services available at the NWQL. Method detection limits, precision, and costs are discussed, as well as possible applications for the methods. To aid in project planning, several tables have been developed that list the approved method for certain determination, particularly those being requested to satisfy cooperator or U.S. Environ- mental Protection Agency regulatory requirements.

Open-File Report↗
USGS1999

Hydrologic data for the Columbia/Eagle Bluffs Wetland Complex, Columbia, Missouri-1993-96

The U.S. Geological Survey, in cooperation with the Missouri Department of Conservation and the city of Columbia, Missouri, collected hydrologic data from September 1993 through October 1996 as part of a hydrologic characterization of the Columbia/Eagle Bluffs Wetland Complex. The wetland complex was constructed in the Missouri River alluvial plain adjacent to the Columbia municipal supply wells. Part of the wetland complex was designed to treat sewage effluent from Columbia, with the treated effluent being used as the primary water source for wetland management practices on the Eagle Bluffs Wildlife Area. This report presents hydrologic data and the procedures used to collect the data, which include water-quality analyses of samples collected quarterly from 28 wells and 2 surface-water sites. Four additional wells were incorporated into the monitoring network in November 1994 and also were sampled quarterly. Data from these 4 wells also are included. Water samples were analyzed for specific conductance, pH, temperature, dissolved oxygen, bacteria, alkalinity, major cations and anions, nutrients, trace elements, and total and dissolved organic carbon. Dissolved nitrite plus nitrate as nitrogen concentrations were equal to or less than 5.2 milligrams per liter for all ground-water samples and were equal to or less than 2.7 milligrams per liter in surface-water samples. Dissolved phosphorous concentrations ranged from less than 0.01 to 2.2 milligrams per liter in the ground-water samples, and from less than 0.01 to 0.19 milli-grams per liter in the surface-water samples. Fecal coliform bacteria counts ranged from less than 1 to 39 colonies per 100 milliliters for ground-water samples, and from 1 to greater than 6,000 colonies per 100 milliliters for surface-water samples. Fecal streptococcus bacteria counts ranged from less than 1 to 92 colonies per 100 milliliters for ground-water samples, and from 2 to greater than 10,000 colonies per 100 milliliters for surface-water samples. Samples for well USGS-6 had dissolved arsenic concentrations that exceeded 50 micrograms per liter. Dissolved manganese concentrations exceeded 50 micrograms per liter at least once for each site except for USGS-9S. Dissolved iron concentrations exceeded 300 micro-grams per liter at least once for 28 of 34 sites. Samples from 8 of the 32 wells and both surface-water sites were analyzed for base/neutral/ acid semi-volatile organic compounds, selected pesticides, selected organochlorine compounds, and purgeable volatile organic compounds. All but one of the organic compounds detected in the samples collected from the monitoring wells or surface-water sites were pesticides. Atrazine was detected consistently at both surface-water sites. Other frequently detected pesticides include metolachlor, diazinon, chlorpyrifos, prometon, and simazine. Following the 1993 Missouri River flood samples of residual flood water and flood-deposited sediments were collected from the Columbia/ Eagle Bluffs Wetland Complex. A brief description of the flooding and damage to the study area is presented. Methods of collection of the four residual flood water and the four flood-deposited sediment samples, as well as the analytical results of these samples, are included in this report. Data from two continuous water-level recorders and from quarterly water-level measurements in wells also are included.

Missouri↗
USGS1997

Models and methods to characterize site amplification from a pair of records

The paper presents a tutorial review of the models and methods that are used to characterize site amplification from the pairs of rock- and soil-site records, and introduces some new techniques with better theoretical foundations. The models and methods discussed include spectral and cross-spectral ratios, spectral ratios for downhole records, response spectral ratios, constant amplification factors, parametric models, physical models, and time-varying filters. An extensive analytical and numerical error analysis of spectral and cross-spectral ratios shows that probabilistically cross-spectral ratios give more reliable estimates of site amplification. Spectral ratios should not be used to determine site amplification from downhole-surface recording pairs because of the feedback in the downhole sensor. Response spectral ratios are appropriate for low frequencies, but overestimate the amplification at high frequencies. The best method to be used depends on how much precision is required in the estimates.

Earthquake Spectra↗
USGS1985

Management of ground water and evolving hydrogeologic studies in New Jersey : a heavily urbanized and industrialized state in the northeastern United States

New Jersey is the most densely populated and one of the most industrialized states in the United States. An abundance of freshwater and proximity to major northeastern metropolitan centers has facilitated this development. Pumpage of freshwater from all aquifers in the State in 1980 was 730 million gallons per day (2.76 million cubic meters per day). Management and efficient development of the ground-water resources of the State are the responsibility of the New Jersey Department of Environmental Protection. Laws have been enacted and updated by the State legislature to manage water allocation and to control the disposal of hazardous wastes. Present resource management is guided by the New Jersey Water-Supply Master Plan of 1981. Funding for management activities is partially derived from the sale of state-approved bonds. Effective planning and regional management require accurate and up-to-date hydrologic information and analyses. The U.S. Geological Survey, in cooperation with the New Jersey Geological Survey, is conducting three intensive ground-water studies involving the collection and interpretation of hydrologic data to meet the urgent water-management needs of New Jersey. These studies are part of a long-term cooperative program and are funded through the Water-Supply Bond Act of 1981. They began in 1983 and are scheduled to be completed in 1988. The project areas are situated in the New Jersey part of the Atlantic Coastal Plain in and near Atlantic City, Camden, and South River. They range in size from 400 to 1,200 mil (1,040 to 3,120 km2). The studies are designed to define the geology, hydrology, and geochemistry of the local ground-water systems. The results of these studies will enable the State to address more effectively major problems in these areas such as declining water levels, overpumping, saltwater intrusion, and ground-water contamination resulting from the improper disposal of hazardous wastes. Specific objectives of these studies by the U.S. Geological Survey are to (1) develop an accurate and up-to-date hydrogeologic data base, (2) design and implement a data-collection program and establish a computerized information management system, (3) refine the conceptualization of the ground-water flow system, and (4) define the geochemistry of the aquifer system by conducting a water-quality appraisal. The objectives are accomplished by standard hydrogeologic methods. Information concerning hydrogeologic framework, ground-water levels, water use, hydraulic characteristics, and water quality in the study areas is compiled from all available sources. Additional data needed are collected through well inventories, surface geophysical surveys, water-quality samplings, water-level measurements, and a well-drilling program. Interpretation of the flow system is based on the use of standard analytical techniques and digital flow modeling. Calibrated flow models will provide ground-water managers with a mechanism to develop and test regional water-supply strategies. Definition of the geochemistry of the aquifer system is accomplished through a variety of methods which depend on the problems and available data in the particular study area. The approach includes statistical analysis of water-quality data, reaction-path modeling, and determination of the movement of chemical constituents using analytical and numerical modeling techniques. A combined staff of 25 to 30 professionals and technicians from the New Jersey District office of the U.S. Geological Survey is committed to the three studies. The staff has specialists in geohydrology, numerical modeling, geochemistry, geophysics, and computer science. The findings of these studies will be published in data reports, interpretive reports, instructional manuals and journal articles.

New Jersey↗
USGS2011

An analytical framework to assist decision makers in the use of forest ecosystem model predictions

The predictions from most forest ecosystem models originate from deterministic simulations. However, few evaluation exercises for model outputs are performed by either model developers or users. This issue has important consequences for decision makers using these models to develop natural resource management policies, as they cannot evaluate the extent to which predictions stemming from the simulation of alternative management scenarios may result in significant environmental or economic differences. Various numerical methods, such as sensitivity/uncertainty analyses, or bootstrap methods, may be used to evaluate models and the errors associated with their outputs. However, the application of each of these methods carries unique challenges which decision makers do not necessarily understand; guidance is required when interpreting the output generated from each model. This paper proposes a decision flow chart in the form of an analytical framework to help decision makers apply, in an orderly fashion, different steps involved in examining the model outputs. The analytical framework is discussed with regard to the definition of problems and objectives and includes the following topics: model selection, identification of alternatives, modelling tasks and selecting alternatives for developing policy or implementing management scenarios. Its application is illustrated using an on-going exercise in developing silvicultural guidelines for a forest management enterprise in Ontario, Canada.

Environmental Modelling and Software↗
USGS2005

Baseline models of trace elements in major aquifers of the United States

Trace-element concentrations in baseline samples from a survey of aquifers used as potable-water supplies in the United States are summarized using methods appropriate for data with multiple detection limits. The resulting statistical distribution models are used to develop summary statistics and estimate probabilities of exceeding water-quality standards. The models are based on data from the major aquifer studies of the USGS National Water Quality Assessment (NAWQA) Program. These data were produced with a nationally-consistent sampling and analytical framework specifically designed to determine the quality of the most important potable groundwater resources during the years 1991-2001. The analytical data for all elements surveyed contain values that were below several detection limits. Such datasets are referred to as multiply-censored data. To address this issue, a robust semi-parametric statistical method called regression on order statistics (ROS) is employed. Utilizing the 90th-95th percentile as an arbitrary range for the upper limits of expected baseline concentrations, the models show that baseline concentrations of dissolved Ba and Zn are below 500 ??g/L. For the same percentile range, dissolved As, Cu and Mo concentrations are below 10 ??g/L, and dissolved Ag, Be, Cd, Co, Cr, Ni, Pb, Sb and Se are below 1-5 ??g/L. These models are also used to determine the probabilities that potable ground waters exceed drinking water standards. For dissolved Ba, Cr, Cu, Pb, Ni, Mo and Se, the likelihood of exceeding the US Environmental Protection Agency standards at the well-head is less than 1-1.5%. A notable exception is As, which has approximately a 7% chance of exceeding the maximum contaminant level (10 ??g/L) at the well head.

Applied Geochemistry↗
USGS2015

Developing analytical approaches to explore the connection between endocrine-active pharmaceuticals in water to effects in fish

The emphasis of this research project was to develop and optimize a solid-phase extraction method and highperformance liquid chromatography-electrospray ionizationmass spectrometry method, such that a linkage between the detection of endocrine-active pharmaceuticals (EAPs) in the aquatic environment and subsequent effects on fish populations could eventually be studied. Four EAPs were studied: tamoxifen (TAM), exemestane (EXE), letrozole (LET), anastrozole (ANA); and three TAM metabolites: 4- hydroxytamoxifen, e/z endoxifen, and n-desmethyl tamoxifen. In aqueous matrices, the use of isotopically labeled standards for the EAPs allowed for the generation of good recoveries, greater than 80 %, and low relative standard deviations (% RSDs) (3 to 27 %). TAM metabolites had lower recoveries in the spiked water matrices: 35 to 93 % in waste/source water compared to 58 to 110 % in DI water. The precision in DI water was acceptable ranging from 8 to 38 % RSD. However, the precision in real environmental wastewaters could be poor, ranging from 15 to 120 % RSD, dependent upon unique matrix effects. In plasma, the overall recoveries of the EAPs were acceptable: 88 to 110 %, with %RSDs of 6 to 18 % (Table 3). The spiked recoveries of the TAM metabolites from plasma were good, ranging from 77 to 120 %, with %RSDs ranging from 27 to 32 %. Two of the TAM metabolites, 4- hydroxytamoxifen and n-desmethyl tamoxifen, were confirmed in most of the environmental aqueous samples. The discovery of TAM metabolites demonstrates that the source of the TAM metabolites, TAM, is constant, introducing a pseudo-persistence of this chemical into the environment.

Analytical and Bioanalytical Chemistry↗
USGS2002

Measurement of the bed material of gravel-bed rivers

The measurement of the physical properties of a gravel-bed river is important in the calculation of sediment transport and physical habitat values for aquatic animals. These properties are not always easy to measure. One recent report on flushing of fines from the Klamath River did not contain information on one location because the grain size distribution of the armour could not be measured on a dry river bar. The grain size distribution could have been measured using a barrel sampler and converting the measurements to the same as would have been measured if a dry bar existed at the site. In another recent paper the porosity was calculated from an average value relation from the literature. The results of that paper may be sensitive to the actual value of porosity. Using the bulk density sampling technique based on a water displacement process presented in this paper the porosity could have been calculated from the measured bulk density. The principle topics of this paper are the measurement of the size distribution of the armour, and measurement of the porosity of the substrate. The 'standard' method of sampling of the armour is to do a Wolman-type count of the armour on a dry section of the river bed. When a dry bar does not exist the armour in an area of the wet streambed is to sample and the measurements transformed analytically to the same type of results that would have been obtained from the standard Wolman procedure. A comparison of the results for the San Miguel River in Colorado shows significant differences in the median size of the armour. The method use to determine the porosity is not 'high-tech' and there is a need improve knowledge of the porosity because of the importance of porosity in the aquatic ecosystem. The technique is to measure the in-situ volume of a substrate sample by measuring the volume of a frame over the substrate and then repeated the volume measurement after the sample is obtained from within the frame. The difference in the volumes is the volume of the sample.

Conference Paper↗
USGS2016

Detection limits of quantitative and digital PCR assays and their influence in presence-absence surveys of environmental DNA

A set of universal guidelines is needed to determine the limit of detection (LOD) in PCR-based analyses of low concentration DNA. In particular, environmental DNA (eDNA) studies require sensitive and reliable methods to detect rare and cryptic species through shed genetic material in environmental samples. Current strategies for assessing detection limits of eDNA are either too stringent or subjective, possibly resulting in biased estimates of species’ presence. Here, a conservative LOD analysis grounded in analytical chemistry is proposed to correct for overestimated DNA concentrations predominantly caused by the concentration plateau, a nonlinear relationship between expected and measured DNA concentrations. We have used statistical criteria to establish formal mathematical models for both quantitative and droplet digital PCR. To assess the method, a new Grass Carp ( Ctenopharyngodon idella ) TaqMan assay was developed and tested on both PCR platforms using eDNA in water samples. The LOD adjustment reduced Grass Carp occupancy and detection estimates while increasing uncertainty – indicating that caution needs to be applied to eDNA data without LOD correction. Compared to quantitative PCR, digital PCR had higher occurrence estimates due to increased sensitivity and dilution of inhibitors at low concentrations. Without accurate LOD correction, species occurrence and detection probabilities based on eDNA estimates are prone to a source of bias that cannot be reduced by an increase in sample size or PCR replicates. Other applications also could benefit from a standardized LOD such as GMO food analysis, and forensic and clinical diagnostics.

Molecular Ecology Resources↗
USGS2013

A wetting and drying scheme for ROMS

The processes of wetting and drying have many important physical and biological impacts on shallow water systems. Inundation and dewatering effects on coastal mud flats and beaches occur on various time scales ranging from storm surge, periodic rise and fall of the tide, to infragravity wave motions. To correctly simulate these physical processes with a numerical model requires the capability of the computational cells to become inundated and dewatered. In this paper, we describe a method for wetting and drying based on an approach consistent with a cell-face blocking algorithm. The method allows water to always flow into any cell, but prevents outflow from a cell when the total depth in that cell is less than a user defined critical value. We describe the method, the implementation into the three-dimensional Regional Oceanographic Modeling System (ROMS), and exhibit the new capability under three scenarios: an analytical expression for shallow water flows, a dam break test case, and a realistic application to part of a wetland area along the Georgia Coast, USA.

Georgia↗
USGS2020

An international code comparison study on coupled thermal, hydrologic and geomechanical processes of natural gas hydrate-bearing sediments

Geologic reservoirs containing gas hydrate occur beneath permafrost environments and within marine continental slope sediments, representing a potentially vast natural gas source. Numerical simulators provide scientists and engineers with tools for understanding how production efficiency depends on the numerous, interdependent (coupled) processes associated with potential production strategies for these gas hydrate reservoirs. Confidence in the modeling and forecasting abilities of these gas hydrate reservoir simulators (GHRSs) grows with successful comparisons against laboratory and field test results, but such results are rare, particularly in natural settings. The hydrate community recognized another approach to building confidence in the GHRS: comparing simulation results between independently developed and executed computer codes on structured problems specifically tailored to the interdependent processes relevant for gas hydrate-bearing systems. The United States Department of Energy, National Energy Technology Laboratory (DOE/NETL), sponsored the first international gas hydrate code comparison study, IGHCCS1, in the early 2000s. IGHCCS1 focused on coupled thermal and hydrologic processes associated with producing gas hydrates from geologic reservoirs via depressurization and thermal stimulation. Subsequently, GHRSs have advanced to model more complex production technologies and incorporate geomechanical processes into the existing framework of coupled thermal and hydrologic modeling. This paper contributes to the validation of these recent GHRS developments by providing results from a second GHRS code comparison study, IGHCCS2, also sponsored by DOE/NETL. IGHCCS2 includes participants from an international collection of universities, research institutes, industry, national laboratories, and national geologic surveys. Study participants developed a series of five benchmark problems principally involving gas hydrate processes with geomechanical components. The five problems range from simple geometries with analytical solutions to a representation of the world’s first offshore production test of methane hydrates, which was conducted with the depressurization method off the coast of Japan. To identify strengths and limitations in the various GHRSs, study participants submitted solutions for the benchmark problems and discussed differing results via teleconferences. The GHRSs evolved over the course of IGHCCS2 as researchers modified their simulators to reflect new insights, lessons learned, and suggested performance enhancements. The five benchmark problems, final sample solutions, and lessons learned that are presented here document the study outcomes and serve as a reference guide for developing and testing gas hydrate reservoir simulators.

Journal of Marine and Petroleum Geology↗
USGS2012

Adjustment of total suspended solids data for use in sediment studies

The U.S. Environmental Protection Agency identifies fluvial sediment as the single most widespread pollutant in the Nation's rivers and streams, affecting aquatic habitat, drinking water treatment processes, and recreational uses of rivers, lakes, and estuaries. A significant amount of suspended-sediment data has been produced using the total suspended solids (TSS) laboratory analysis method. An evaluation of data collected and analyzed by the U.S. Geological Survey and others has shown that the variation in TSS analytical results is considerably larger than that for traditional suspended-sediment concentration analyses (SSC) and that the TSS data show a negative bias when compared to SSC data. This paper presents the initial results of a continuing investigation into the differences between TSS and SSC results. It explores possible relations between these differences and other hydrologic data collected at the same stations. A general equation was developed to relate TSS data to SSC data. However, this general equation is not applicable for data from individual stations. Based on these analyses, there appears to be no simple, straightforward way to relate TSS and SSC data unless pairs of TSS and SSC results are available for a station.

Conference Paper↗
USGS2023

Geospatial standard operating procedures of the Chesapeake Bay Program

Introduction The Chesapeake Bay Program (CBP) has operated a geographic information system (GIS) program since the early 1990s to address the established and growing need for and use of geospatial data, maps, and analysis within the CBP Partnership. This report is intended to detail the standard operating procedures of the CBP GIS program and address the quality assurance, quality control, and other technical activities that CBP will implement to ensure the commitment of the CBP GIS Team to performance standards (U.S. Environmental Protection Agency, 2003). The report is intended as an update to the 2011 Quality Assurance Project Plan (QAPP). For specialized tasks or analytical projects beyond the scope of this QAPP, a separate specialized QAPP with details on quality control, assurance procedures, and the geospatial methods associated with all aspects of the project may be required.

Open-File Report↗
USGS2006

An evaluation of a reagentless method for the determination of total mercury in aquatic life

Multiple treatment (i.e., drying, chemical digestion, and oxidation) steps are often required during preparation of biological matrices for quantitative analysis of mercury; these multiple steps could potentially lead to systematic errors and poor recovery of the analyte. In this study, the Direct Mercury Analyzer (Milestone Inc., Monroe, CT) was utilized to measure total mercury in fish tissue by integrating steps of drying, sample combustion and gold sequestration with successive identification using atomic absorption spectrometry. We also evaluated the differences between the mercury concentrations found in samples that were homogenized and samples with no preparation. These results were confirmed with cold vapor atomic absorbance and fluorescence spectrometric methods of analysis. Finally, total mercury in wild captured largemouth bass (n = 20) were assessed using the Direct Mercury Analyzer to examine internal variability between mercury concentrations in muscle, liver and brain organs. Direct analysis of total mercury measured in muscle tissue was strongly correlated with muscle tissue that was homogenized before analysis (r = 0.81, p < 0.0001). Additionally, results using this integrated method compared favorably (p < 0.05) with conventional cold vapor spectrometry with atomic absorbance and fluorescence detection methods. Mercury concentrations in brain were significantly lower than concentrations in muscle (p < 0.001) and liver (p < 0.05) tissues. This integrated method can measure a wide range of mercury concentrations (0-500 ??g) using small sample sizes. Total mercury measurements in this study are comparative to the methods (cold vapor) commonly used for total mercury analysis and are devoid of laborious sample preparation and expensive hazardous waste. ?? Springer 2006.

Water, Air, & Soil Pollution↗
USGS2024

Methods of analysis—Determination of pesticides in filtered water and suspended sediment using liquid chromatography- and gas chromatography-tandem mass spectrometry

The widespread application of pesticides in agricultural and urban areas leads to their presence in surface waters. Presence of these biologically active chemicals in environmental waters potentially has adverse effects on nontarget organisms. To better understand the environmental fate of these contaminants, a robust method to capture chemicals with wide-ranging physicochemical properties has been developed. The method was developed by the U.S. Geological Survey’s Organic Chemistry Research Laboratory to monitor pesticides, pesticide degradates, and other agrochemicals in environmental surface waters throughout the country. The analysis involves a multiresidue method to determine 183 pesticides and pesticide degradates in filtered water samples and 178 pesticides and pesticide degradates in paired suspended sediment samples. After the filtration of whole water, contaminants are individually measured in the filtered water and the collected suspended sediment. Filtered water is extracted via solid-phase extraction, whereas suspended sediment is extracted using an ultrasonication, solid-liquid extraction. Samples are analyzed by liquid chromatography-tandem mass spectrometry using an electrospray ionization source in positive and negative modes and analyzed by gas chromatography-tandem mass spectrometry using an advanced electron ionization source in positive mode. Instrument parameters were optimized for the highest sensitivity, and at least two transitions (quantifier and qualifier) were monitored for each analyte. Recoveries in test filtered water ( n =9; 183 analytes) from the American River, California, and suspended sediment ( n =9; 178 analytes) samples fortified at 15 nanograms per liter (ng/L) ranged from 70.1 to 121.0 and 71.1 to 117.0 percent in water and suspended sediment filter samples, respectively. Method detection limits of pesticides and pesticide degradates ranged from 0.5 to 10.6 ng/L in water and 0.7 to 11.8 ng/L in suspended sediment filters. Reporting limits were 1.1–21.1 ng/L and 1.5–23.7 ng/L in water and filter samples, respectively. The developed method is applied to surface-water samples for the analysis of pesticides, pesticide degradates, and other agrochemicals.

Techniques and Methods↗
USGS1999

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of arsenic and selenium in water and sediment by graphite furnace atomic absorption spectrometry

Graphite furnace-atomic absorption spectrometry (GF-AAS) is a sensitive, precise, and accurate technique that can be used to determine arsenic and selenium in samples of water and sediment. The GF-AAS method has been developed to replace the hydride generation-atomic absorption spectrometry (HG-AAS) methods because the method detection limits are similar, bias and variability are comparable, and interferences are minimal. Advantages of the GF-AAS method include shorter sample preparation time, increased sample throughput from simultaneous multielement analysis, reduced amount of chemical waste, reduced sample volume requirements, increased linear concentration range, and the use of a more accurate digestion procedure. The linear concentration range for arsenic and selenium is 1 to 50 micrograms per liter in solution; the current method detection limit for arsenic in solution is 0.9 microgram per liter; the method detection limit for selenium in solution is 1 microgram per liter. This report describes results that were obtained using stop-flow and low-flow conditions during atomization. The bias and variability of the simultaneous determination of arsenic and selenium by GF-AAS under both conditions are supported with results from standard reference materials--water and sediment, real water samples, and spike recovery measurements. Arsenic and selenium results for all Standard Reference Water Samples analyzed were within one standard deviation of the most probable values. Long-term spike recoveries at 6.25, 25.0, 37.5 micrograms per liter in reagent-, ground-, and surface-water samples for arsenic averaged 103 plus or minus 2 percent using low-flow conditions and 104 plus or minus 4 percent using stop-flow conditions. Corresponding recoveries for selenium were 98 plus or minus 13 percent using low-flow conditions and 87 plus or minus 24 percent using stop-flow conditions. Spike recoveries at 25 micrograms per liter in 120 water samples ranged from 97 to 99 percent for arsenic and from 82 to 93 percent for selenium, depending on the flow conditions used. Statistical analysis of dissolved and whole-water recoverable analytical results for the same set of water samples indicated that there is no significant difference between the GF-AAS and HG-AAS methods. Interferences related to various chemical constituents were also identified. Although sulfate and chloride in association with various cations might interfere with the determination of arsenic and selenium by GF-AAS, the use of a magnesium nitrate/palladium matrix modifier and low-flow argon during atomization helped to minimize such interferences. When using stabilized temperature platform furnace conditions where stop flow is used during atomization, the addition of hydrogen (5 percent volume/volume) to the argon minimized chemical interferences. Nevertheless, stop flow during atomization was found to be less effective than low flow in reducing interference effects.

Open-File Report↗