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At least 1,063 records · Page 59Linked to original sources
USGS2002

Quercetin as colorimetric reagent for determination of zirconium

Methods described in the literature for the determination of zirconium are generally designed for relatively large amounts of this element. A good procedure using colorimetric reagent for the determination of trace amounts is desirable. Quercetin has been found to yield a sensitive color reaction with zirconium suitable for the determination of from 0.1 to 50 of zirconium dioxide. The procedure developed involves the separation of zirconium from interfering elements by precipitation with p-dimethylaminoazophenylarsonic acid prior to its estimation with quercetin. The quercetin reaction is carried out in 0.5N hydrochloric acid solution. Under the operating conditions it is indicated that quercetin forms a 2 to 1 complex with zirconium; however, a 2 to 1 and a 1 to 1 complex can coexist under special conditions. Approximate values for the equilibrium constants of the complexes are K 1 = 0.33 x 10 -5 and K 2 = 1.3 x 10 -9 . Seven Bureau of Standards samples of glass sands and refractories were analyzed with excellent results. The method described should find considerable application in the analysis of minerals and other materials for macro as well as micro amounts of zirconium.

Analytical Chemistry↗
USGS2016

Determination of polydimethylsiloxane–water partition coefficients for ten 1-chloro-4-[2,2,2-trichloro-1-(4-chlorophenyl)ethyl]benzene-related compounds and twelve polychlorinated biphenyls using gas chromatography/mass spectrometry

Polymer-water partition coefficients (Kpw) of ten DDT-related compounds were determined in pure water at 25 °C using commercial polydimethylsiloxane-coated optical fiber. Analyte concentrations were measured by thermal desorption-gas chromatography/full scan mass spectrometry (TD–GC/MSFS; fibers) and liquid injection-gas chromatography/selected ion monitoring mass spectrometry (LI–GC/MSSIM; water). Equilibrium was approached from two directions (fiber uptake and depletion) as a means of assessing data concordance. Measured compound-specific log Kpw values ranged from 4.8 to 6.1 with an average difference in log Kpw between the two approaches of 0.05 log units (∼12% of Kpw). Comparison of the experimentally-determined log Kpw values with previously published data confirmed the consistency of the results and the reliability of the method. A second experiment was conducted with the same ten DDT-related compounds and twelve selected PCB (polychlorinated biphenyl) congeners under conditions characteristic of a coastal marine field site (viz., seawater, 11 °C) that is currently under investigation for DDT and PCB contamination. Equilibration at lower temperature and higher ionic strength resulted in an increase in log Kpw for the DDT-related compounds of 0.28–0.49 log units (61–101% of Kpw), depending on the analyte. The increase in Kpw would have the effect of reducing by approximately half the calculated freely dissolved pore-water concentrations (Cfree). This demonstrates the importance of determining partition coefficients under conditions as they exist in the field.

Journal of Chromatography A↗
USGS2023

Creating oriented and precisely sectioned mineral mounts for in situ chemical analyses—An example using olivine for diffusion chronometry studies

Diffusion chronometry is now a widely applied methodology for determining the rates and timescales of geologic processes from the chemical zoning observed in minerals. Despite the popularity of the method, several challenges still remain during its application, including: (1) the random sectioning of minerals either in thin sections or grain mounts in which both off-center and oblique sections contribute substantial uncertainty to modeled timescales and (2) diffusion anisotropy needs to be accounted for in models, which generally requires determining the principal crystallographic axes of the mineral using electron backscatter diffraction, a technique that is both challenging and limiting because few scanning electron microscopes have an electron backscatter detector. This guide developed by the U.S. Geological Survey focuses on a step-by-step methodology for mounting individually oriented minerals that are sectioned through their cores prior to polishing for analytical work. Using this technique, one can significantly reduce the uncertainties associated with off-center sections and minimize or completely remove the need for determining crystallographic orientation via electron backscatter diffraction analyses. This report is presented as a guide for using the technique on olivine crystals but can be applied to any minerals that can be extracted for analysis. Two variations of the methodology are included here: (1) The individual crystal method that entails mounting individually sectioned single crystals and crystal groups and (2) the whole mount method in which multiple single crystals or crystal clusters are mounted and sectioned at the same time.

Techniques and Methods↗
USGS2016

Regional oxygen reduction and denitrification rates in groundwater from multi-model residence time distributions, San Joaquin Valley, USA

Rates of oxygen and nitrate reduction are key factors in determining the chemical evolution of groundwater. Little is known about how these rates vary and covary in regional groundwater settings, as few studies have focused on regional datasets with multiple tracers and methods of analysis that account for effects of mixed residence times on apparent reaction rates. This study provides insight into the characteristics of residence times and rates of O 2 reduction and denitrification (NO 3 − reduction) by comparing reaction rates using multi-model analytical residence time distributions (RTDs) applied to a data set of atmospheric tracers of groundwater age and geochemical data from 141 well samples in the Central Eastern San Joaquin Valley, CA. The RTD approach accounts for mixtures of residence times in a single sample to provide estimates of in-situ rates. Tracers included SF 6 , CFCs, 3 H, He from 3 H (tritiogenic He), 14 C, and terrigenic He. Parameter estimation and multi-model averaging were used to establish RTDs with lower error variances than those produced by individual RTD models. The set of multi-model RTDs was used in combination with NO 3 − and dissolved gas data to estimate zero order and first order rates of O 2 reduction and denitrification. Results indicated that O 2 reduction and denitrification rates followed approximately log-normal distributions. Rates of O 2 and NO 3 − reduction were correlated and, on an electron milliequivalent basis, denitrification rates tended to exceed O 2 reduction rates. Estimated historical NO 3 − trends were similar to historical measurements. Results show that the multi-model approach can improve estimation of age distributions, and that relatively easily measured O 2 rates can provide information about trends in denitrification rates, which are more difficult to estimate.

California↗
USGS1999

Double-disk solid-phase extraction--Simultaneous cleanup and trace enrichment of herbicides and metabolites from environmental samples

Phenylurea and triazine herbicides, including some metabolites, were isolated from water and soil extracts by solid-phase extraction using a layered system of two extraction disks, a method called double-disk solid-phase extraction. The first disk consisted of strong anion exchange (SAX) of 10-μm styrene divinylbenzene (SDB) particles embedded in Teflon, and the second disk was a C 18 disk of 10-μm particles also embedded in Teflon. A volume of 500 mL of water or aqueous soil extract is passed through the layered system with the SAX disk first. The purpose of the SAX disk is to remove the humic and fulvic acids from the water or aqueous soil extract by ion exchange through their carboxyl groups. Even during methanol elution of herbicides, the humic substances remain bound to the SAX disk with >85% retention. Elution with methanol results in more than 90% recovery of the herbicides from the layered extraction disks. Removal of the humic and fulvic acids results in greater sensitivity for diode array detection quantitation (0.05 μg/L for herbicides) by substantially reducing the absorbance of the humic peak on the LC chromatogram. The herbicides adsorb to the SAX disk either through hydrogen bonding to the anion-exchange sites or by hydrophobic interaction with the SDB surface of the anion-exchange disk. The method was tested for the analysis of natural water samples from the Mississippi Embayment, a cotton-growing area of the southeastern United States.

Analytical Chemistry↗
USGS2012

Advances in the simulation and automated measurement of well-sorted granular material: 2. Direct measures of particle properties

1. In this, the second of a pair of papers on the structure of well-sorted natural granular material (sediment), new methods are described for automated measurements from images of sediment, of: 1) particle-size standard deviation (arithmetic sorting) with and without apparent void fraction; and 2) mean particle size in material with void fraction. A variety of simulations of granular material are used for testing purposes, in addition to images of natural sediment. Simulations are also used to establish that the effects on automated particle sizing of grains visible through the interstices of the grains at the very surface of a granular material continue to a depth of approximately 4 grain diameters and that this is independent of mean particle size. Ensemble root-mean squared error between observed and estimated arithmetic sorting coefficients for 262 images of natural silts, sands and gravels (drawn from 8 populations) is 31%, which reduces to 27% if adjusted for bias (slope correction between observed and estimated values). These methods allow non-intrusive and fully automated measurements of surfaces of unconsolidated granular material. With no tunable parameters or empirically derived coefficients, they should be broadly universal in appropriate applications. However, empirical corrections may need to be applied for the most accurate results. Finally, analytical formulas are derived for the one-step pore-particle transition probability matrix, estimated from the image's autocorrelogram, from which void fraction of a section of granular material can be estimated directly. This model gives excellent predictions of bulk void fraction yet imperfect predictions of pore-particle transitions.

Journal of Geophysical Research F: Earth Surface↗
USGS2014

Interrelations among the soil-water retention, hydraulic conductivity, and suction-stress characteristic curves

The three fundamental constitutive relations that describe fluid flow, strength, and deformation behavior of variably saturated soils are the soil-water retention curve (SWRC), hydraulic conductivity function (HCF), and suction-stress characteristic curve (SSCC). Until recently, the interrelations among the SWRC, HCF, and SSCC have not been well established. This work sought experimental confirmation of interrelations among these three constitutive functions. Results taken from the literature for six soils and those obtained for 11 different soils were used. Using newly established analytical relations among the SWRC, HCF, and SSCC and these test results, the authors showed that these three constitutive relations can be defined by a common set of hydromechanical parameters. The coefficient of determination for air-entry pressures determined independently using hydraulic and mechanical methods is >0.99, >0.98 for the pore size parameter, and 0.94 for the residual degree of saturation. One practical implication is that one of any of the four experiments (axis-translation, hydraulic, shear-strength, or deformation) is sufficient to quantify all three constitutive relations.

Journal of Geotechnical and Geoenvironmental Engin↗
USGS2018

Book review: Analytical groundwater mechanics

Encapsulating almost 50 years of experience applying mathematics to groundwater flow problems, this latest textbook from Otto Strack ( 2017 ) is a tour de force for analytical groundwater approaches. It is comprised of 10 chapters, spanning topics from the basics of groundwater mechanics, to steady state, three‐dimensional, and transient flow, as well as particle tracking and solute transport. The book concludes with a chapter on finite‐difference and finite‐element methods, but the treatment is cursory, focusing on basic principles. The book is high quality, especially with respect to the presentation, due perhaps in no small part to the keen eye of the author's longtime publication resource (and clearly supportive wife) Andrine!

Groundwater↗
USGS2000

Update and revisions for Open-File Report 98-624, synthetic precipitation leaching procedure (SPLP) leachate chemistry data for solid mine-waste composite samples from the Silverton and Leadville districts in Colorado

This report supersedes, revises, and updates information and data previously released in Open-File Report 98-624 (Montour and others, 1998). Data for this report were derived from leaching of mine-waste composite samples using a modification of E.P. A. Method 1312, Synthetic Precipitation Leaching Procedure (SPLP). In 1997, members of the U.S. Geological Survey Mine Waste Characterization Project collected four mine-waste composite samples from mining districts near Silverton, Colorado (MAY and YUK), and near Leadville, Colorado (VEN and SUN). This report presents analytical results from these sites.

Open-File Report↗
USGS2011

Lithogeochemistry of mineralized and altered rock samples from the northern Talkeetna Mountains, south-central Alaska

Mineralized and altered rock samples collected from the northern Talkeetna Mountains, Alaska, were analyzed by two different inductively coupled plasma atomic-emission spectrometry (ICP-AES) methods for as many as 44 elements; by fire assay and either direct-coupled plasma (DCP) or atomic absorption spectrophotometry (AAS) for gold (Au); by cold vapor atomic absorption (CVAA) for mercury (Hg); and by irradiated neutron activation analysis (INAA) for tungsten (W). The analytical results showed that some samples contain high values of multiple elements and may be potential indicators of hydrothermal mineralization in the area.

Alaska↗
USGS1953

Determination of traces of cobalt in soils: A field method

The growing use of geochemical prospecting methods in the search for ore deposits has led to the development of a field method for the determination of cobalt in soils. The determination is based on the fact that cobalt reacts with 2-nitroso-1-naphthol to yield a pink compound that is soluble in carbon tetrachloride. The carbon tetrachloride extract is shaken with dilute cyanide to complex interfering elements and to remove excess reagent. The cobalt content is estimated by comparing the pink color in the carbon tetrachloride with a standard series prepared from standard solutions. The cobalt 2-nitroso-1-naphtholate system in carbon tetrachloride follows Beer's law. As little as 1 p.p.m. can be determined in a 0.1-gram sample. The method is simple and fast and requires only simple equipment. More than 40 samples can be analyzed per man-day with an accuracy within 30% or better.

Analytical Chemistry↗
USGS1989

Graphical method for determining the coefficient of consolidation c from a flow-pump permeability test

A graphical method has been developed for determining the coefficient of consolidation from the transient phases of a flow-pump permeability test. The flow pump can be used to infuse fluid into or withdraw fluid from a laboratory sediment specimen at a constant volumetric rate in order to obtain data that can be used to calculate permeability using Darcy's law. When the initial transient-response curve (hydraulic head as a function of time) generated by this test is examined analytically in terms of a one-dimensional consolidation process, representative type-curve solutions to the associated forced-flow and pressure-decay models are derived. These curves provide the basis for graphically evaluating the permeability k , the coefficient of consolidation c v , and the coefficient of volume change m v . The curve-matching technique is easy and rapid, and it can be applied to results of forced-flow tests, both infusion and withdrawal, as well as to subsequent pressure-decay records. Values of k, c v , and m v for a laterally confined kaolinite specimen were determined by this graphical method and appear to be in reasonably good agreement with numerically derived estimates (within 20%). Discrepancies between the two sets of results seem to be largely a function of data quality rather than of method of analysis. Where responses of hydraulic head as a function of time are apparently unaffected by experimental sources of error, agreement is excellent (within 4%). Application of this graphical method to triaxial testing has inherent uncertainties, because the solution curves that describe one-dimensional deformation are used to analyze a three-dimensional process.

Geotechnical Testing Journal↗
USGS2024

Earth’s free surface complicates inference of absolute stress from earthquake-Induced stress rotations

The stress redistribution from an earthquake can produce localized measurable rotations of the principal stress axes if the absolute level of differential stress in the crust in on the order of the earthquake stress drop. Two simple analytic solutions have been developed to estimate the differential stress from an observed stress rotation. However, each has assumptions that may not be accurate near Earth’s free surface. I model synthetic earthquakes in an elastic half-space, and show that the assumptions of the methods are accurate for strike-slip earthquakes, and for deep dip-slip earthquakes. However, they are incorrect for shallow dip-slip earthquakes. I introduce a free surface correction for one of the methods for dip-slip earthquakes. I revise an analysis of stress rotations due to great subduction zone earthquakes, including this correction. The results support the original conclusion of near complete stress drop for many shallow subduction zone earthquakes.

Geophysical Research Letters↗
USGS1991

Unified theory on power laws for flow resistance

Two general power formulas, one for hydraulically smooth flows and the other for fully rough flows, are derived in a rational way from the widely accepted logarithmic formulas for the velocity profile and the Darcy‐Weisbach friction factor. A regression analysis based on the method of least squares is used to determine the valid range of the local velocity (or normal distance from the wall) in the power formula. Some older empirical formulas, such as Lacey's, Manning's, Blasius', and Hazen‐Williams', and their valid ranges, are actually explained analytically by the results. Incomplete self‐similarity of the power law, in which the exponent and the associated coefficient vary with the similarity parameters, such as the Reynolds number and the relative roughness, is elucidated through the parametric representations of the power formulas and their counterparts based on the logarithmic law. This paper examines the concept and rationale behind the power formulation of uniform turbulent shear flows, thereby addressing some critical issues in the modeling of flow resistance based on the power law.

Journal of Hydraulic Engineering↗
USGS2016

An investigation of soil-structure interaction effects observed at the MIT Green Building

The soil-foundation impedance function of the MIT Green Building is identified from its response signals recorded during an earthquake. Estimation of foundation impedance functions from seismic response signals is a challenging task, because: (1) the foundation input motions (FIMs) are not directly measurable, (2) the as-built properties of the super-structure are only approximately known, and (3) the soil-foundation impedance functions are inherently frequency-dependent. In the present study, aforementioned difficulties are circumvented by using, in succession, a blind modal identification (BMID) method, a simplified Timoshenko beam model (TBM), and a parametric updating of transfer functions (TFs). First, the flexible-base modal properties of the building are identified from response signals using the BMID method. Then, a flexible-base TBM is updated using the identified modal data. Finally, the frequency-dependent soil-foundation impedance function is estimated by minimizing the discrepancy between TFs (of pairs instrumented floors) that are (1) obtained experimentally from earthquake data and (2) analytically from the updated TBM. Using the fully identified flexible-base TBM, the FIMs as well as building responses at locations without instruments can be predicted, as demonstrated in the present study.

Massachussets↗
USGS2008

Development of a standard reference material for Cr(vi) in contaminated soil

Over the last several decades, considerable contamination by hexavalent chromium has resulted from the land disposal of Chromite Ore Processing Residue (COPR). COPR contains a number of hexavalent chromium-bearing compounds that were produced in high temperature industrial processes. Concern over the carcinogenic potential of this chromium species, and its environmental mobility, has resulted in efforts to remediate these waste sites. To provide support to analytical measurements of hexavalent chromium, a candidate National Institute of Standards and Technology (NIST) Standard Reference Material?? (SRM 2701), having a hexavalent chromium content of approximately 500 mg kg -1, has been developed using material collected from a waste site in Hudson County, New Jersey, USA. The collection, processing, preparation and preliminary physico-chemical characterization of the material are discussed. A two-phase multi-laboratory testing study was carried out to provide data on material homogeneity and to assess the stability of the material over the duration of the study. The study was designed to incorporate several United States Environmental Protection Agency (USEPA) determinative methods for hexavalent chromium, including Method 6800 which is based on speciated isotope dilution mass spectrometry (SIDMS), an approach which can account for chromium species inter-conversion during the extraction and measurement sequence. This journal is ?? The Royal Society of Chemistry 2008.

Journal of Analytical Atomic Spectrometry↗
USGS1951

Determination of molybenum in soils and rocks: A geochemical semimicro field method

Reconnaissance work in geochemical prospecting requires a simple, rapid, and moderately accurate method for the determination of small amounts of molybdenum in soils and rocks. The useful range of the suggested procedure is from 1 to 32 p.p.m. of molybdenum, but the upper limit can be extended. Duplicate determinations on eight soil samples containing less than 10 p.p.m. of molybdenum agree within 1 p.p.m., and a comparison of field results with those obtained by a conventional laboratory procedure shows that the method is sufficiently accurate for use in geochemical prospecting. The time required for analysis and the quantities of reagents needed have been decreased to provide essentially a "test tube" method for the determination of molybdenum in soils and rocks. With a minimum amount of skill, one analyst can make 30 molybdenum determinations in an 8-hour day.

Analytical Chemistry↗
USGS1982

Near-station terrain corrections for gravity data by a surface-integral technique

A new method of computing gravity terrain corrections by use of a digitizer and digital computer can result in substantial savings in the time and manual labor required to perform such corrections by conventional manual ring-chart techniques. The method is typically applied to estimate terrain effects for topography near the station, for example within 3 km of the station, although it has been used successfully to a radius of 15 km to estimate corrections in areas where topographic mapping is poor. Points (about 20) that define topographic maxima, minima, and changes in the slope gradient are picked on the topographic map, within the desired radius of correction about the station. Particular attention must be paid to the area immediately surrounding the station to ensure a good topographic representation. The horizontal and vertical coordinates of these points are entered into the computer, usually by means of a digitizer. The computer then fits a multiquadric surface to the input points to form an analytic representation of the surface. By means of the divergence theorem, the gravity effect of an interior closed solid can be expressed as a surface integral, and the terrain correction is calculated by numerical evaluation of the integral over the surfaces of a cylinder, The vertical sides of which are at the correction radius about the station, the flat bottom surface at the topographic minimum, and the upper surface given by the multiquadric equation. The method has been tested with favorable results against models for which an exact result is available and against manually computed field-station locations in areas of rugged topography. By increasing the number of points defining the topographic surface, any desired degree of accuracy can be obtained. The method is more objective than manual ring-chart techniques because no average compartment elevations need be estimated ?

Open-File Report↗