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USGS Reference Materials Program: Serving the Needs of the Global Analytical Community

Every year in the United States, millions of measurements are made on the chemical composition of items that affect us on a daily basis. The accuracy of these measurements is routinely determined by the analysis of appropriate reference materials. In the field of earth science, reference materials are particularly important because they help us develop a better understanding of the processes that have shaped, and continue to shape the world around us. USGS reference materials are distributed internationally to organizations involved in geochemical and environmental analysis, instrumentation and methods development, and industrial research and quality assurance. Reference materials are widely used in the development and validation of geochemical models used by the USGS.

Fact Sheet↗

Ground-water sampling methods and quality-control data for the Red River of the North basin, Minnesota, North Dakota, and South Dakota, 1993-95

Ground-water-quality samples were collected for the intensive data-collection phase of the Red River of the P Torth Basin study unit, one of 60 study units of the National Water Quality Assessment (NAWQA) Program throughout the United States. The sampling protocols used were designed for the NAWQA Program. The protocols include sampling equipment, cleaning procedures, sample-collection methods, and quality-control plans to monitor the accuracy of the data collected. One of the goals of the NAWQA Program was to collect data using similar methcds to build a nationally consistent water-quality data base. Quality-control data demonstrated that most constituents measured for this study yielded reproducible data, with low to undetectable contamination from the sampling and analytical procedures. Several constituents were occasionally or frequently detected in blank samples at levels similar to low-concentration ground-water-quality samples. For example, iron was detected in 75 percent of the blank samples, with a maximum concentration of 27 [ig/L, indicating that iron contamination may interfere with its determination at low levels in ground waters. Copper, aluminum, and dissolved organic carbon concentrations in blank samples overlap those determined in ground-waterquality samples, thereby precluding quantitative reporting of those constituents. Most pesticide data are reproducible, with minimal bias. Some pesticides had low but consistent recoveries; these data may be useful if spike and surrogate data are carefully considered. Data for some pesticides measured in this study should not be quantitatively reported or used, because they may underestimate the concentrations of those pesticides in ground waters.

Minnesota, North Dakota, South Dakota↗

Population fragmentation and inter-ecosystem movements of grizzly bears in Western Canada and the Northern United States

Population fragmentation compromises population viability, reduces a species ability to respond to climate change, and ultimately may reduce biodiversity. We studied the current state and potential causes of fragmentation in grizzly bears over approximately 1,000,000 km 2 of western Canada, the northern United States (US), and southeast Alaska. We compiled much of our data from projects undertaken with a variety of research objectives including population estimation and trend, landscape fragmentation, habitat selection, vital rates, and response to human development. Our primary analytical techniques stemmed from genetic analysis of 3,134 bears, supplemented with radiotelemetry data from 792 bears. We used 15 locus microsatellite data coupled withmeasures of genetic distance, isolation-by-distance (IBD) analysis, analysis of covariance (ANCOVA), linear multiple regression, multi-factorial correspondence analysis (to identify population divisions or fractures with no a priori assumption of group membership), and population-assignment methods to detect individual migrants between immediately adjacent areas. These data corroborated observations of inter-area movements from our telemetry database. In northern areas, we found a spatial genetic pattern of IBD, although there was evidence of natural fragmentation from the rugged heavily glaciated coast mountains of British Columbia (BC) and the Yukon. These results contrasted with the spatial pattern of fragmentation in more southern parts of their distribution. Near the Canada-US border area, we found extensive fragmentation that corresponded to settled mountain valleys andmajor highways. Genetic distances across developed valleys were elevated relative to those across undeveloped valleys in central and northern BC. In disturbed areas, most inter-area movements detected were made by male bears, with few female migrants identified. North-south movements within mountain ranges (Mts) and across BC Highway 3 were more common than east-west movements across settled mountain valleys separating Mts. Our results suggest that relatively distinct subpopulations exist in this region, including the Cabinet, Selkirk South, and the decadesisolated Yellowstone populations. Current movement rates do not appear sufficient to consider the subpopulations we identify along the Canada-US border as 1 inter-breeding unit. Although we detected enough male movement to mediate gene flow, the current low rate of female movement detected among areas is insufficient to provide a demographic rescue effect between areas in the immediate future (0-15 yr). In Alberta, we found fragmentation corresponded to major east-west highways (Highways 3, 11, 16, and 43) and most inter-area movements were made by males. Gene flow and movement rates between Alberta and BC were highest across the Continental Divide south of Highway 1 and north of Highway 16. In the central region between Highways 1 and 11, we found evidence of natural fragmentation associated with the extensive glaciers and icefields along the Continental Divide. The discontinuities that we identified would form appropriate boundaries formanagement units. We related sex-specific movement rates between adjacent areas to several metrics of human use (highway traffic, settlement, and humancaused mortality) to understand the causes of fragmentation. This analysis used data from 1,508 bears sampled over a 161,500-km 2 area in southeastern BC, western Alberta, northern Idaho, and northern Montana during 1979-2007. This area was bisected by numerous human transportation and settlement corridors of varying intensity and complexity. We used multiple linear regression and ANCOVA to document the responses of female and male bears to disturbance. Males and females both demonstrated reduced movement rates with increasing settlement and traffic. However, females reduced their movement rates dramatically when settlement increased to >20% of the fracture zone. At this same

Wildlife Monographs↗

Metrics for comparing dynamic earthquake rupture simulations

Earthquakes are complex events that involve a myriad of interactions among multiple geologic features and processes. One of the tools that is available to assist with their study is computer simulation, particularly dynamic rupture simulation. A dynamic rupture simulation is a numerical model of the physical processes that occur during an earthquake. Starting with the fault geometry, friction constitutive law, initial stress conditions, and assumptions about the condition and response of the near‐fault rocks, a dynamic earthquake rupture simulation calculates the evolution of fault slip and stress over time as part of the elastodynamic numerical solution (Ⓔ see the simulation description in the electronic supplement to this article). The complexity of the computations in a dynamic rupture simulation make it challenging to verify that the computer code is operating as intended, because there are no exact analytic solutions against which these codes’ results can be directly compared. One approach for checking if dynamic rupture computer codes are working satisfactorily is to compare each code’s results with the results of other dynamic rupture codes running the same earthquake simulation benchmark. To perform such a comparison consistently, it is necessary to have quantitative metrics. In this paper, we present a new method for quantitatively comparing the results of dynamic earthquake rupture computer simulation codes.

Seismological Research Letters↗

1980 water quality laboratory services catalog

The information in this catalog is provided to assist Water Resources Division personnel in the selection of analytical determinations, estimation of cost, calculation of sample volume requirements, identification of the necessary sample treatment, and selection of laboratory precision for samples to be submitted to Central Laboratories. The catalog contains 18 tables. Tables 1-4 are arranged alphabetically by constituent or schedule, and where available, include parameter name, unit of measurement, lab code or schedule code, applicable range and precision of the method, parameter code, method number and name, and a page index. Tables 1 and 2 list inorganic and organic constituents determined in water samples, table 3 provides information on determinations of chemical and physical properties of sediments, and table 4 lists biological determinations. Page references in these first four tables refer to the tables of determinations (tables 5 through 8) or to the tables of calculations (tables 9 through 12). Constituents that are found in more than one category are cross-referenced (e.g. nitrogen, organic is found in the inorganic table and is cross indexed in the organic table). Tables 13 through 16 list sample containers, sample preservations, and sample designations for each determination. Table 17 lists materials (bottles, preservatives, standardized solutions, and so forth) which may be purchased from the Central Laboratories. Table 18 lists agency codes which can be used to indicate the agency collecting or analyzing samples. Although the catalog is being released now, its effective date is September 11, 1979 to September 10, 1980. The early release is for program planning only.

Open-File Report↗

Geochemical field method for determination of nickel in plants

The use of biogeochemical data in prospecting for nickel emphasizes the need for a simple, moderately accurate field method for the determination of nickel in plants. In order to follow leads provided by plants of unusual nickel content without loss of time, the plants should be analyzed and the results given to the field geologist promptly. The method reported in this paper was developed to meet this need. Speed is acquired by elimination of the customary drying and controlled ashing; the fresh vegetation is ashed in an open dish over a gasoline stove. The ash is put into solution with hydrochloric acid and the solution buffered. A chromograph is used to make a confined spot with an aliquot of the ash solution on dimethylglyoxime reagent paper. As little as 0.025% nickel in plant ash can be determined. With a simple modification, 0.003% can be detected. Data are given comparing the results obtained by an accepted laboratory procedure. Results by the field method are within 30% of the laboratory values. The field method for nickel in plants meets the requirements of biogeochemical prospecting with respect to accuracy, simplicity, speed, and ease of performance in the field. With experience, an analyst can make 30 determinations in an 8-hour work day in the field.

Analytical Chemistry↗

Groundwater contaminant plume maps and volumes, 100-K and 100-N Areas, Hanford Site, Washington

This study provides an independent estimate of the areal and volumetric extent of groundwater contaminant plumes which are affected by waste disposal in the 100-K and 100-N Areas (study area) along the Columbia River Corridor of the Hanford Site. The Hanford Natural Resource Trustee Council requested that the U.S. Geological Survey perform this interpolation to assess the accuracy of delineations previously conducted by the U.S. Department of Energy and its contractors, in order to assure that the Natural Resource Damage Assessment could rely on these analyses. This study is based on previously existing chemical (or radionuclide) sampling and analysis data downloaded from publicly available Hanford Site Internet sources, geostatistically selected and interpreted as representative of current (from 2009 through part of 2012) but average conditions for groundwater contamination in the study area. The study is limited in scope to five contaminants—hexavalent chromium, tritium, nitrate, strontium-90, and carbon-14, all detected at concentrations greater than regulatory limits in the past. All recent analytical concentrations (or activities) for each contaminant, adjusted for radioactive decay, non-detections, and co-located wells, were converted to log-normal distributions and these transformed values were averaged for each well location. The log-normally linearized well averages were spatially interpolated on a 50 × 50-meter (m) grid extending across the combined 100-N and 100-K Areas study area but limited to avoid unrepresentative extrapolation, using the minimum curvature geostatistical interpolation method provided by SURFER ® data analysis software. Plume extents were interpreted by interpolating the log-normally transformed data, again using SURFER ® , along lines of equal contaminant concentration at an appropriate established regulatory concentration . Total areas for each plume were calculated as an indicator of relative environmental damage. These plume extents are shown graphically and in tabular form for comparison to previous estimates. Plume data also were interpolated to a finer grid (10 × 10 m) for some processing, particularly to estimate volumes of contaminated groundwater. However, hydrogeologic transport modeling was not considered for the interpolation. The compilation of plume extents for each contaminant also allowed estimates of overlap of the plumes or areas with more than one contaminant above regulatory standards. A mapping of saturated aquifer thickness also was derived across the 100-K and 100–N study area, based on the vertical difference between the groundwater level (water table) at the top and the altitude of the top of the Ringold Upper Mud geologic unit, considered the bottom of the uppermost unconfined aquifer. Saturated thickness was calculated for each cell in the finer (10 × 10 m) grid. The summation of the cells’ saturated thickness values within each polygon of plume regulatory exceedance provided an estimate of the total volume of contaminated aquifer, and the results also were checked using a SURFER ® volumetric integration procedure. The total volume of contaminated groundwater in each plume was derived by multiplying the aquifer saturated thickness volume by a locally representative value of porosity (0.3). Estimates of the uncertainty of the plume delineation also are presented. “Upper limit” plume delineations were calculated for each contaminant using the same procedure as the “average” plume extent except with values at each well that are set at a 95-percent upper confidence limit around the log-normally transformed mean concentrations, based on the standard error for the distribution of the mean value in that well; “lower limit” plumes are calculated at a 5-percent confidence limit around the geometric mean. These upper- and lower-limit estimates are considered unrealistic because the statistics were increased or decreased at each well simultaneously and were not adjusted for correlation among the well distributions (i.e., it is not realistic that all wells would be high simultaneously). Sources of the variability in the distributions used in the upper- and lower-extent maps include time varying concentrations and analytical errors. The plume delineations developed in this study are similar to the previous plume descriptions developed by U.S. Department of Energy and its contractors. The differences are primarily due to data selection and interpolation methodology. The differences in delineated plumes are not sufficient to result in the Hanford Natural Resource Trustee Council adjusting its understandings of contaminant impact or remediation.

Washington↗

Can machine learning accelerate process understanding and decision-relevant predictions of river water quality?

The global decline of water quality in rivers and streams has resulted in a pressing need to design new watershed management strategies. Water quality can be affected by multiple stressors including population growth, land use change, global warming, and extreme events, with repercussions on human and ecosystem health. A scientific understanding of factors affecting riverine water quality and predictions at local to regional scales, and at sub-daily to decadal timescales are needed for optimal management of watersheds and river basins. Here, we discuss how machine learning (ML) can enable development of more accurate, computationally tractable, and scalable models for analysis and predictions of river water quality. We review relevant state-of-the art applications of ML for water quality models and discuss opportunities to improve the use of ML for emerging computational and mathematical methods for model selection, hyperparameter optimization, incorporating process knowledge into ML models, improving explainablity, uncertainty quantification, and model-data integration. We then present considerations for using ML to address water quality problems given their scale and complexity, available data and computational resources, and stakeholder needs. When combined with decades of process understanding, interdisciplinary advances in knowledge-guided ML, information theory, data integration, and analytics can help address fundamental science questions and enable decision-relevant predictions of riverine water quality.

Hydrological Processes↗

Leveraging invasive mussel contaminant survey data for stepwise prioritization of chemicals of potential concern in the Great Lakes basin

Historical and ongoing anthropogenic activities coupled with advancements in analytical techniques have led to the detection of large numbers of contaminants in the Laurentian Great Lakes. Consequently, identifying and prioritizing chemicals likely to cause ecological harm represents a challenge for natural resource managers. Previous prioritization efforts have focused on contaminants in sediment, water, and passive samplers, which may not be representative of compounds that bioaccumulate in aquatic organisms. Consequently, this study adopted a stepwise method to prioritize chemicals of potential concern detected in dreissenid mussels from samples collected across the Great Lakes from 2009–2018. The stepwise method considered environmental fate, detection frequency, and exceedance of toxicity quotients based on ecotoxicological effect concentrations. Overall, 153 compounds out of 267 analyzed were detected in dreissenid mussels, 47 of which had water quality effect concentrations, 56 had apical effect concentrations (Tier 1 ECOTOX or apical screening), 17 had nonapical effect concentrations (Tier 2 ECOTOX, Cytotoxic Burst, and ToxCast) and 33 had estimated effect concentrations (quantitative structure-activity relationship, estimated screening, and pharmacological potency). Of the compounds with water quality effect concentrations, nine were designated as high priority, including the herbicide atrazine and five polycyclic aromatic hydrocarbons that were previously identified as potentially hazardous within other matrices. Similar contaminants were identified as high priority in a related study of native unionid mussels in the Great Lakes. A total of 27 compounds were low priority, suggesting that these contaminants do not warrant further action based on this dataset. Overall, these findings will facilitate the development of management strategies to mitigate the effects of contaminants on aquatic organisms within the Great Lakes.

Great Lakes basin↗

Studies of a peatified angiosperm log cross section from Indonesia by nuclear magnetic resonance spectroscopy and analytical pyrolysis

Samples from a 10 cm cross-sectional radius of a peatified angiosperm log from Sumatra, Indonesia, were examined by 13 C nuclear magnetic resonance and pyrolysis-gas chromatography in order to understand chemical changes due to the peatification process. NMR results show degradation by selective loss of carbohydrates in all parts of the log section compared with fresh wood; however, the degree of degradation is less near the center of the log section. The degree of ring substitution of aromatic lignin monomeric units, as measured by dipolar dephasing NMR methods, appears to be less at the center of the log section than at the periphery. The methoxyl carbon content of lignin in the log is lower than in unaltered angiospermous lignin but does not appear to change as a function of either radial position or the degree of aromatic ring substitution. Pyrolysis-gas chromatography indicates higher yields of catechols in the outer areas relative to the heartwood. Other than the variations in catechol contents and in the yields of carbohydrate-derived pyrolysis products (e.g. levoglucosan, angelicalactones), the pyrolysis results do not show significant changes related to radial position, indicating that the lignin is not significantly altered across the log section.

Organic Geochemistry↗

Effect of dynamical phase on the resonant interaction among tsunami edge wave modes

Different modes of tsunami edge waves can interact through nonlinear resonance. During this process, edge waves that have very small initial amplitude can grow to be as large or larger than the initially dominant edge wave modes. In this study, the effects of dynamical phase are established for a single triad of edge waves that participate in resonant interactions. In previous studies, Jacobi elliptic functions were used to describe the slow variation in amplitude associated with the interaction. This analytical approach assumes that one of the edge waves in the triad has zero initial amplitude and that the combined phase of the three waves φ = θ 1 + θ 2 − θ 3 is constant at the value for maximum energy exchange ( φ = 0). To obtain a more general solution, dynamical phase effects and non-zero initial amplitudes for all three waves are incorporated using numerical methods for the governing differential equations. Results were obtained using initial conditions calculated from a subduction zone, inter-plate thrust fault geometry and a stochastic earthquake slip model. The effect of dynamical phase is most apparent when the initial amplitudes and frequencies of the three waves are within an order of magnitude. In this case, non-zero initial phase results in a marked decrease in energy exchange and a slight decrease in the period of the interaction. When there are large differences in frequency and/or initial amplitude, dynamical phase has less of an effect and typically one wave of the triad has very little energy exchange with the other two waves. Results from this study help elucidate under what conditions edge waves might be implicated in late, large-amplitude arrivals.

Pure and Applied Geophysics↗

Remote-sensing methods for monitoring surface coal mining in the northern Great Plains

Recent studies at a large surface coal mine in southern Montana confirm that remote sensing is both feasible and effective for gathering land-use and environmental data (spatial, dynamic, and seasonal) for large-scale surface mines in the northern Great Plains. The Western Energy Co.'s Rosebud mine near Colstrip, Mont., was selected as a test site because it typifies surface operations in the Powder River Basin of Montana and Wyoming and elsewhere in the northern Great Plains. Several basic interpretive and analytical remote-sensing techniques were used to identify and delineate various categories of surface-mining operations and concurrent stages of reclamation that characterize most, if not all, such mining operations. Color infrared and black-and-white aerial photographs and a black-and-white band 5 Landsat image were used to identify (1) high wall and bench areas, (2) ungraded spoils, (3) graded and recontoured areas, (4) revegetated recontoured areas, (5) natural and impounded surface water, and (6) miscellaneous areas. Over the lifespan of an extensive surface mine, cultural and natural processes and cumulative environmental effects can be monitored by capitalizing on the close correlation between enhanced satellite imagery, infrared and (or) black-and-white aerial photography, standard large-scale topographic maps (such as U.S. Geological Survey 7½-minute quadrangle maps), and results of onsite inspection of mining and reclamation by Federal or State agencies.

Montana↗

Application of effective discharge analysis to environmental flow decision-making

Well-informed river management decisions rely on an explicit statement of objectives, repeatable analyses, and a transparent system for assessing trade-offs. These components may then be applied to compare alternative operational regimes for water resource infrastructure (e.g., diversions, locks, and dams). Intra- and inter-annual hydrologic variability further complicates these already complex environmental flow decisions. Effective discharge analysis (developed in studies of geomorphology) is a powerful tool for integrating temporal variability of flow magnitude and associated ecological consequences. Here, we adapt the effectiveness framework to include multiple elements of the natural flow regime (i.e., timing, duration, and rate-of-change) as well as two flow variables. We demonstrate this analytical approach using a case study of environmental flow management based on long-term (60 years) daily discharge records in the Middle Oconee River near Athens, GA, USA. Specifically, we apply an existing model for estimating young-of-year fish recruitment based on flow-dependent metrics to an effective discharge analysis that incorporates hydrologic variability and multiple focal taxa. We then compare three alternative methods of environmental flow provision. Percentage-based withdrawal schemes outcompete other environmental flow methods across all levels of water withdrawal and ecological outcomes.

Environmental Management↗

The U.S. Geological Survey coal quality (COALQUAL) database version 3.0

Since the mid-1970s, the U.S. Geological Survey (USGS) has maintained a coal quality database of national scope named USCHEM, which currently contains data for over 13,000 samples. A subset of the USCHEM database called COALQUAL Version 1.3 was initially published in 1994 and was followed by Version 2.0 in 1997. Version 3.0 of the COALQUAL database represents a major editing effort to resolve some of the DOS software limitations used by earlier versions of the database. Because of database size limits during the development of COALQUAL Version 1.3, many analyses of individual bench samples were merged into whole coal bed averages. The methodology for making these composite intervals was not consistent. Size limits also restricted the amount of georeferencing information and forced removal of qualifier notations such as "less than detection limit" (<) information, which can cause problems when using the data. A review of the original data sheets revealed that COALQUAL Version 2.0 was missing information that was needed for a complete understanding of a coal section. Another important database issue to resolve was the USGS "remnant moisture" problem. Prior to 1998, tests for remnant moisture (as-determined moisture in the sample at the time of analysis) were not performed on any USGS major, minor, or trace element coal analyses. Without the remnant moisture, it is impossible to convert the analyses to a usable basis (as-received, dry, etc.). Based on remnant moisture analyses of hundreds of samples of different ranks (and known residual moisture) reported after 1998, it was possible to develop a method to provide reasonable estimates of remnant moisture for older data to make it more useful in COALQUAL Version 3.0. In addition, COALQUAL Version 3.0 is improved by (1) adding qualifiers, including statistical programming to deal with the qualifiers; (2) clarifying the sample compositing problems; and (3) adding associated samples. Version 3.0 of COALQUAL also represents the first attempt to incorporate data verification by mathematically crosschecking certain analytical parameters. Finally, a new database system was designed and implemented to replace the outdated DOS program used in earlier versions of the database.

Data Series↗

Water quality and hydrology of the Silver River Watershed, Baraga County, Michigan, 2005-08

The Silver River Watershed comprises about 69 square miles and drains part of northeastern Baraga County, Michigan. For generations, tribal members of the Keweenaw Bay Indian Community have hunted and fished in the watershed. Tribal government and members of Keweenaw Bay Indian Community are concerned about the effect of any development within the watershed, which is rural, isolated, and lightly populated. For decades, the area has been explored for various minerals. Since 2004, several mineral-exploration firms have been actively investigating areas within the watershed; property acquisition, road construction, and subsurface drilling have taken place close to tributary streams of the Silver River. The U.S. Geological Survey, in cooperation with Keweenaw Bay Indian Community, conducted a multi-year water-resources investigation of the Silver River Watershed during 2005-08. Methods of investigation included analyses of streamflow, water-quality sampling, and ecology at eight discrete sites located throughout the watershed. In addition, three continuous-record streamgages located within the watershed provided stage, discharge, specific conductance, and water-temperature data on an hourly basis. Water quality of the Silver River Watershed is typical of many streams in undeveloped areas of Upper Michigan. Concentrations of most analytes typically were low, although several exceeded applicable surface-water-quality standards. Seven samples had concentrations of copper that exceeded the Michigan Department of Environmental Quality standards for wildlife, and one sample had concentrations of cyanide that exceeded the same standards. Concentrations of total mercury at all eight sampling sites exceeded the Great Lakes Basin water-quality standard, but the ratio of methylmercury to total mercury was similar to the 5 to 10 percent found in most natural waters. Concentrations of arsenic and chromium in bed sediments were near the threshold-effect concentration. A qualitative ecological assessment of fishes and macroinvertebrates showed that intolerant salmonids were present at most sampled sites, and macroinvertebrate communities were indicative of near-excellent or excellent conditions at all eight sites. This baseline information will aid in an ongoing monitoring effort designed to protect the water resources of the

Scientific Investigations Report↗

Synthetic calibration of a Rainfall-Runoff Model

A method for synthetically calibrating storm-mode parameters for the U.S. Geological Survey's Precipitation-Runoff Modeling System is described. Synthetic calibration is accomplished by adjusting storm-mode parameters to minimize deviations between the pseudo-probability disributions represented by regional regression equations and actual frequency distributions fitted to model-generated peak discharge and runoff volume. Results of modeling storm hydrographs using synthetic and analytic storm-mode parameters are presented. Comparisons are made between model results from both parameter sets and between model results and observed hydrographs. Although mean storm runoff is reproducible to within about 26 percent of the observed mean storm runoff for five or six parameter sets, runoff from individual storms is subject to large disparities. Predicted storm runoff volume ranged from 2 percent to 217 percent of commensurate observed values. Furthermore, simulation of peak discharges was poor. Predicted peak discharges from individual storm events ranged from 2 percent to 229 percent of commensurate observed values. The model was incapable of satisfactorily executing storm-mode simulations for the study watersheds. This result is not considered a particular fault of the model, but instead is indicative of deficiencies in similar conceptual models.

Conference Paper↗

Determination of lead, uranium, thorium, and thallium in silicate glass standard materials by isotope dilution mass spectrometry

A set of four standard glasses has been prepared which have been doped with 61 different elements at the 500-, 50-, 1-, and 0.02-ppm level. The concentrations of lead, uranium, thorium, and thallium have been determined by isotope dilution mass spectrometry at a number of points in each of the glasses. The results obtained from independent determinations in two laboratories demonstrate the homogeneity of the samples and that precision of the order of 0.5% (95% L.E.) may be obtained by the method even at the 20-ppb level for these elements. The chemical and mass spectrometric procedures necessary are presented.

Analytical Chemistry↗

UV identification and quantitative measurement of quinaldine residues in fish

A method for the confirmatory analysis of quinaldine residue in fish is described. The method utilizes the same extraction and cleanup procedure as the GLC method reported previously. The lower limit of sensitivity for quinaldine residue in fish muscle is 0.01 ppm. Identification is accomplished by comparing the UV spectra of the sample and a standard solution of quinaldine.

Journal of the Association of Official Analytical ↗