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Sample records for solid samples rock

  1. A new method for determining the uranium and thorium distribution in volcanic rock samples using solid state nuclear track detectors

    International Nuclear Information System (INIS)

    Misdaq, M.A.; Bakhchi, A.; Ktata, A.; Koutit, A.; Lamine, J.; Ait nouh, F.; Oufni, L.

    2000-01-01

    A method based on using solid state nuclear track detectors (SSNTD) CR- 39 and LR-115 type II and calculating the probabilities for the alpha particles emitted by the uranium and thorium series to reach and be registered on these films was utilized for uranium and thorium contents determination in various geological samples. The distribution of uranium and thorium in different volcanic rocks has been investigated using the track fission method. In this work, the uranium and thorium contents have been determined in different volcanic rock samples by using CR-39 and LR-115 type II solid state nuclear track detectors (SSNTD). The mean critical angles of etching of the solid state nuclear track detectors utilized have been calculated. A petrographical study of the volcanic rock thin layers studied has been conducted. The uranium and thorium distribution inside different rock thin layers has been studied. The mechanism of inclusion of the uranium and thorium nuclei inside the volcanic rock samples studied has been investigated. (author)

  2. Solid as a rock

    International Nuclear Information System (INIS)

    Pincus, H.J.

    1984-01-01

    Recent technologic developments have required a more comprehensive approach to the behavior of rock mass or rock substance plus discontinuities than was adequate previously. This work considers the inherent problems in such operations as the storage of hot or cold fluids in caverns and aquifers, underground storage of nuclear waste, underground recovery of heat from hydrocarbon fuels, tertiary recovery of oil by thermal methods, rapid excavation of large openings at shallow to great depths and in hostile environments, and retrofitting of large structures built on or in rock. The standardization of methods for determining rock properties is essential to all of the activities described, for use not only in design and construction but also in site selection and post-construction monitoring. Development of such standards is seen as a multidisciplinary effort

  3. Deposition behavior of polystyrene latex particles on solid surfaces during migration through an artificial fracture in a granite rock sample

    International Nuclear Information System (INIS)

    Chinju, Hirofumi; Tanaka, Satoru; Kuno, Yoshio

    2001-01-01

    The deposition behavior of colloids during transport through heterogeneous media was observed by conducting column experiments to study migration of polystyrene latex particles (diameter=309 nm) through columns packed with artificially fractured granite rock (length=300 and 150 mm). The experiments were conducted under conditions of different ionic strengths and flow rates. The results were similar to those for colloid deposition in columns packed with glass beads reported previously; the colloid breakthrough curves showed three stages, characterized by different rates of change in the concentration of effluent. Colloid deposition on the fracture surfaces was described by considering strong and weak deposition sites. Scanning Electron Microscopy (SEM) observations indicated the existence of strong and weak sites on the fracture surfaces regardless of mineral composition. The observations also showed that the strong deposition sites tended to exist on surface irregularities such as cracks or protrusions. The degree of colloid deposition increased with increasing ionic strength and decreasing flow rate. The dependencies on ionic strength and flow rate agreed qualitatively with the DLVO theory and the previous experimental results, respectively. (author)

  4. Rock pushing and sampling under rocks on Mars

    Science.gov (United States)

    Moore, H.J.; Liebes, S.; Crouch, D.S.; Clark, L.V.

    1978-01-01

    Viking Lander 2 acquired samples on Mars from beneath two rocks, where living organisms and organic molecules would be protected from ultraviolet radiation. Selection of rocks to be moved was based on scientific and engineering considerations, including rock size, rock shape, burial depth, and location in a sample field. Rock locations and topography were established using the computerized interactive video-stereophotogrammetric system and plotted on vertical profiles and in plan view. Sampler commands were developed and tested on Earth using a full-size lander and surface mock-up. The use of power by the sampler motor correlates with rock movements, which were by plowing, skidding, and rolling. Provenance of the samples was determined by measurements and interpretation of pictures and positions of the sampler arm. Analytical results demonstrate that the samples were, in fact, from beneath the rocks. Results from the Gas Chromatograph-Mass Spectrometer of the Molecular Analysis experiment and the Gas Exchange instrument of the Biology experiment indicate that more adsorbed(?) water occurs in samples under rocks than in samples exposed to the sun. This is consistent with terrestrial arid environments, where more moisture occurs in near-surface soil un- der rocks than in surrounding soil because the net heat flow is toward the soil beneath the rock and the rock cap inhibits evaporation. Inorganic analyses show that samples of soil from under the rocks have significantly less iron than soil exposed to the sun. The scientific significance of analyses of samples under the rocks is only partly evaluated, but some facts are clear. Detectable quantities of martian organic molecules were not found in the sample from under a rock by the Molecular Analysis experiment. The Biology experiments did not find definitive evidence for Earth-like living organisms in their sample. Significant amounts of adsorbed water may be present in the martian regolith. The response of the soil

  5. Lead isotope analyses of standard rock samples

    International Nuclear Information System (INIS)

    Koide, Yoshiyuki; Nakamura, Eizo

    1990-01-01

    New results on lead isotope compositions of standard rock samples and their analytical procedures are reported. Bromide form anion exchange chromatography technique was adopted for the chemical separation lead from rock samples. The lead contamination during whole analytical procedure was low enough to determine lead isotope composition of common natural rocks. Silica-gel activator method was applied for emission of lead ions in the mass spectrometer. Using the data reduction of 'unfractionated ratios', we obtained good reproducibility, precision and accuracy on lead isotope compositions of NBS SRM. Here we present new reliable lead isotope compositions of GSJ standard rock samples and USGS standard rock, BCR-1. (author)

  6. Controlled sample program publication No. 1: characterization of rock samples

    International Nuclear Information System (INIS)

    Ames, L.L.

    1978-10-01

    A description is presented of the methodology used and the geologic parameters measured on several rocks which are being used in round-robin laboratory and nuclide adsorption methodology experiments. Presently investigators from various laboratories are determining nuclide distribution coefficients utilizing numerous experimental techniques. Unfortunately, it appears that often the resultant data are dependent not only on the type of groundwater and rock utilized, but also on the experimentor or method used. The Controlled Sample Program is a WISAP (Waste Isolation Safety Assessment Program) attempt to resolve the apparent method and dependencies and to identify individual experimenter's bias. The rock samples characterized in an interlaboratory Kd methodology comparison program include Westerly granite, Argillaceous shale, Oolitic limestone, Sentinel Gap basalt, Conasauga shale, Climax Stock granite, anhydrite, Magenta dolomite and Culebra dolomite. Techniques used in the characterization include whole rock chemical analysis, X-ray diffraction, optical examination, electron microprobe elemental mapping, and chemical analysis of specific mineral phases. Surface areas were determined by the B.E.T. and ethylene glycol sorption methods. Cation exchange capacities were determined with 85 Sr, but were of questionable value for the high calcium rocks. A quantitative mineralogy was also estimated for each rock. Characteristics which have the potential of strongly affecting radionuclide Kd values such as the presence of sulfides, water-soluble, pH-buffering carbonates, glass, and ferrous iron were listed for each rock sample

  7. Digital Rock Simulation of Flow in Carbonate Samples

    Science.gov (United States)

    Klemin, D.; Andersen, M.

    2014-12-01

    Reservoir engineering has becomes more complex to deal with current challenges, so core analysts must understand and model pore geometries and fluid behaviors at pores scales more rapidly and realistically. We introduce an industry-unique direct hydrodynamic pore flow simulator that operates on pore geometries from digital rock models obtained using microCT or 3D scanning electron microscope (SEM) images. The PVT and rheological models used in the simulator represent real reservoir fluids. Fluid-solid interactions are introduced using distributed micro-scale wetting properties. The simulator uses density functional approach applied for hydrodynamics of complex systems. This talk covers selected applications of the simulator. We performed microCT scanning of six different carbonate rock samples from homogeneous limestones to vuggy carbonates. From these, we constructed digital rock models representing pore geometries for the simulator. We simulated nonreactive tracer flow in all six digital models using a digital fluid description that included a passive tracer solution. During the simulation, we evaluated the composition of the effluent. Results of tracer flow simulations corresponded well with experimental data of nonreactive tracer floods for the same carbonate rock types. This simulation data of the non-reactive tracer flow can be used to calculate the volume of the rock accessible by the fluid, which can be further used to predict response of a porous medium to a reactive fluid. The described digital core analysis workflow provides a basis for a wide variety of activities, including input to design acidizing jobs and evaluating treatment efficiency and EOR economics. Digital rock multiphase flow simulations of a scanned carbonate rock evaluated the effect of wettability on flow properties. Various wetting properties were tested: slightly oil wet, slightly water wet, and water wet. Steady-state relative permeability simulations yielded curves for all three

  8. Zirconium determination in rocks by solid-phase spectrophotometry

    International Nuclear Information System (INIS)

    Brykina, G.D.; Lebedeva, G.G.; Agapova, G.F.; AN SSSR, Moscow

    1990-01-01

    A method was developed for determination of zirconium in rocks by solid-phase spectrophotometry using AV-17x8-Cl anion exchanger modified with xylenol orange. Relative standard deviation at the level of (2-4.9)x10 -3 % ZrO 2 was about 0.245

  9. Summary of Test Results for Daya Bay Rock Samples

    International Nuclear Information System (INIS)

    Onishi, Celia Tiemi; Dobson, Patrick; Nakagawa, Seiji

    2004-01-01

    A series of analytical tests was conducted on a suite of granitic rock samples from the Daya Bay region of southeast China. The objective of these analyses was to determine key rock properties that would affect the suitability of this location for the siting of a neutrino oscillation experiment. This report contains the results of chemical analyses, rock property measurements, and a calculation of the mean atomic weight

  10. Astronaut Neil Armstrong studies rock samples during geological field trip

    Science.gov (United States)

    1969-01-01

    Astronaut Neil Armstrong, commander of the Apollo 11 lunar landing mission, studies rock samples during a geological field trip to the Quitman Mountains area near the Fort Quitman ruins in far west Texas.

  11. Rock solid: the geology of nuclear waste disposal

    International Nuclear Information System (INIS)

    Reid, Elspeth.

    1990-01-01

    With a number of nuclear submarines and power stations due to be decommissioned in the next decade, stores of radioactive waste, and arguments about storage increase. Whatever the direction taken by the nuclear industry in Britain, the legacy of waste remains for the foreseeable future. Geology is at the heart of the safety argument for nuclear wastes. It is claimed that rocks should act as the main safety barrier, protecting present and future generations from radiation. Rock Solid presents a clear, accessible and up to date account of the geological problems involved in building a nuclear waste repository. The author describes the geology of some of the possible UK repository sites (Sellafield, Dounreay, Altnabreac, Billingham), explains how sites are investigated (including computer models), and finally considers the crucial question: 'would geological containment of radioactive waste actually work?'. (author)

  12. Characterization of rock samples and mineralogical controls on leachates

    Science.gov (United States)

    Hammarstrom, Jane M.; Cravotta, Charles A.; Galeone, Daniel G.; Jackson, John C.; Dulong, Frank T.; Hornberger, Roger J.; Brady, Keith B.C.

    2009-01-01

    Rocks associated with coal beds typically include shale, sandstone, and (or) limestone. In addition to common rock-forming minerals, all of these rock types may contain sulfide and sulfate minerals, various carbonate minerals, and organic material. These different minerals have inherently different solubility characteristics, as well as different acid-generating or acid-neutralizing potentials. The abundance and composition of sulfur- and carbonate-bearing minerals are of particular interest in interpreting the leaching column data because (1) pyrite and carbonate minerals are the primary controls on the acid-base account of a sample, (2) these minerals incorporate trace metals that can be released during weathering, and (3) these minerals readily react during weathering due to mineral dissolution and oxidation of iron.Rock samples were collected by the Pennsylvania Department of Environmental Protection (PaDEP) from five different sites to assess the draft standardized leaching column method (ADTI-WP2) for the prediction of weathering rates and water quality at coal mines. Samples were sent to USGS laboratories for mineralogical characterization and to ActLabs for chemical analysis. The samples represent a variety of rock types (shales, sandstones, and coal refuse) that are typical of coal overburden in the eastern United States. These particular samples were chosen for testing the weathering protocols because they represent a range of geochemical and lithologic characteristics, sulfur contents, and acid-base accounting characteristics (Hornberger et al., 2003). The rocks contain variable amounts of pyrite and carbonate minerals and vary in texture.This chapter includes bulk rock chemical data and detailed mineralogical and textural data for unweathered starting materials used in the interlaboratory validation study, and for two samples used in the early phases of leaching column tests (Wadesville Sandstone, Leechburg Coal Refuse). We also characterize some of the

  13. Sample Results from MCU Solids Outage

    Energy Technology Data Exchange (ETDEWEB)

    Peters, T.; Washington, A.; Oji, L.; Coleman, C.; Poirier, M.

    2014-09-22

    Savannah River National Laboratory (SRNL) has received several solid and liquid samples from MCU in an effort to understand and recover from the system outage starting on April 6, 2014. SRNL concludes that the presence of solids in the Salt Solution Feed Tank (SSFT) is the likely root cause for the outage, based upon the following discoveries: A solids sample from the extraction contactor #1 proved to be mostly sodium oxalate; A solids sample from the scrub contactor#1 proved to be mostly sodium oxalate; A solids sample from the Salt Solution Feed Tank (SSFT) proved to be mostly sodium oxalate; An archived sample from Tank 49H taken last year was shown to contain a fine precipitate of sodium oxalate; A solids sample from ; A liquid sample from the SSFT was shown to have elevated levels of oxalate anion compared to the expected concentration in the feed. Visual inspection of the SSFT indicated the presence of precipitated or transferred solids, which were likely also in the Salt Solution Receipt Tank (SSRT). The presence of the solids coupled with agitation performed to maintain feed temperature resulted in oxalate solids migration through the MCU system and caused hydraulic issues that resulted in unplanned phase carryover from the extraction into the scrub, and ultimately the strip contactors. Not only did this carryover result in the Strip Effluent (SE) being pushed out of waste acceptance specification, but it resulted in the deposition of solids into several of the contactors. At the same time, extensive deposits of aluminosilicates were found in the drain tube in the extraction contactor #1. However it is not known at this time how the aluminosilicate solids are related to the oxalate solids. The solids were successfully cleaned out of the MCU system. However, future consideration must be given to the exclusion of oxalate solids into the MCU system. There were 53 recommendations for improving operations recently identified. Some additional considerations or

  14. Performance improvement of ionic surfactant flooding in carbonate rock samples by use of nanoparticles

    Directory of Open Access Journals (Sweden)

    Mohammad Ali Ahmadi

    2016-07-01

    Full Text Available Abstract Various surfactants have been used in upstream petroleum processes like chemical flooding. Ultimately, the performance of these surfactants depends on their ability to reduce the interfacial tension between oil and water. The surfactant concentration in the aqueous solution decreases owing to the loss of the surfactant on the rock surface in the injection process. The main objective of this paper is to inhibit the surfactant loss by means of adding nanoparticles. Sodium dodecyl sulfate and silica nanoparticles were used as ionic surfactant and nanoparticles in our experiments, respectively. AEROSIL® 816 and AEROSIL® 200 are hydrophobic and hydrophilic nanoparticles. To determine the adsorption loss of the surfactant onto rock samples, a conductivity approach was used. Real carbonate rock samples were used as the solid phase in adsorption experiments. It should be noted that the rock samples were water wet. This paper describes how equilibrium adsorption was investigated by examining adsorption behavior in a system of carbonate sample (solid phase and surfactant solution (aqueous phase. The initial surfactant and nanoparticle concentrations were 500–5000 and 500–2000 ppm, respectively. The rate of surfactant losses was extremely dependent on the concentration of the surfactant in the system, and the adsorption of the surfactant decreased with an increase in the nanoparticle concentration. Also, the hydrophilic nanoparticles are more effective than the hydrophobic nanoparticles.

  15. Astronauts Armstrong and Aldrin study rock samples during field trip

    Science.gov (United States)

    1969-01-01

    Astronaut Neil Armstrong, commander of the Apollo 11 lunar landing mission, and Astronaut Edwin Aldrin, Lunar module pilot for Apollo 11, study rock samples during a geological field trip to the Quitman Mountains area near the Fort Quitman ruins in far west Texas.

  16. Rock sampling. [method for controlling particle size distribution

    Science.gov (United States)

    Blum, P. (Inventor)

    1971-01-01

    A method for sampling rock and other brittle materials and for controlling resultant particle sizes is described. The method involves cutting grooves in the rock surface to provide a grouping of parallel ridges and subsequently machining the ridges to provide a powder specimen. The machining step may comprise milling, drilling, lathe cutting or the like; but a planing step is advantageous. Control of the particle size distribution is effected primarily by changing the height and width of these ridges. This control exceeds that obtainable by conventional grinding.

  17. Apollo Lunar Sample Photographs: Digitizing the Moon Rock Collection

    Science.gov (United States)

    Lofgren, Gary E.; Todd, Nancy S.; Runco, S. K.; Stefanov, W. L.

    2011-01-01

    The Acquisition and Curation Office at JSC has undertaken a 4-year data restoration project effort for the lunar science community funded by the LASER program (Lunar Advanced Science and Exploration Research) to digitize photographs of the Apollo lunar rock samples and create high resolution digital images. These sample photographs are not easily accessible outside of JSC, and currently exist only on degradable film in the Curation Data Storage Facility

  18. Assessing total and volatile solids in municipal solid waste samples.

    Science.gov (United States)

    Peces, M; Astals, S; Mata-Alvarez, J

    2014-01-01

    Municipal solid waste is broadly generated in everyday activities and its treatment is a global challenge. Total solids (TS) and volatile solids (VS) are typical control parameters measured in biological treatments. In this study, the TS and VS were determined using the standard methods, as well as introducing some variants: (i) the drying temperature for the TS assays was 105°C, 70°C and 50°C and (ii) the VS were determined using different heating ramps from room tempature to 550°C. TS could be determined at either 105°C or 70°C, but oven residence time was tripled at 70°C, increasing from 48 to 144 h. The VS could be determined by smouldering the sample (where the sample is burnt without a flame), which avoids the release of fumes and odours in the laboratory. However, smouldering can generate undesired pyrolysis products as a consequence of carbonization, which leads to VS being underestimated. Carbonization can be avoided using slow heating ramps to prevent the oxygen limitation. Furthermore, crushing the sample cores decreased the time to reach constant weight and decreased the potential to underestimate VS.

  19. An ultrasonic corer for planetary rock sample retrieval

    International Nuclear Information System (INIS)

    Harkness, P; Cardoni, A; Lucas, M

    2009-01-01

    Several recent and planned space projects have been focussed on surface rovers for planetary missions, such as the U.S. Mars Exploration Rovers and the European ExoMars. The main functions of similar extraterrestrial vehicles in the future will be moving across planetary surfaces and retrieving rock samples. This paper presents a novel ultrasonic rock sampling tool tuned in a longitudinal-torsional mode along with the conceptual design of a full coring apparatus for preload delivery and core removal. Drilling and coring bits have been designed so that a portion of the longitudinal motion supplied by the ultrasonic transducer is converted into torsional motion. Results of drilling/coring trials are also presented.

  20. Rb/Sr dating of rock samples from Antarctica

    International Nuclear Information System (INIS)

    Ahmed, A.; Awan, M.A.; Mehjabeen, A.; Jabeen, N.; Majid, C.A.

    1996-01-01

    Soon after the discovery of radioactivity in 1896 by Becquerel, the phenomenon was applied to geochronology. From 1902 onwards, rapid advances were made in this field of science. Using radiometric techniques of Rb/Sr the whole rock granitic pegmatite samples from two localities in the North Eastern Antarctica have been dated. The rock samples have yielded Rb/Sr ages around 200 nd 173 million year. The ages around 200 million year have been correlated to the orogenic/epeirogenic activities associated with the breaking up of the Pangaea which led to the dispersion of the continents to form Gondwanaland and Laurasia which subsequently gave rise to the present day configuration of the globe. The younger age of 173 million year corresponds to Jurassic dole rites from Western queens Maud Land and other areas of Antarctica. (author)

  1. Rock sample brought to earth from the Apollo 12 lunar landing mission

    Science.gov (United States)

    1969-01-01

    A scientist's gloved hand holds one of the numerous rock samples brought back to Earth from the Apollo 12 lunar landing mission. This sample is a highly shattered basaltic rock with a thin black-glass coating on five of its six sides. Glass fills fractures and cements the rock together. The rock appears to have been shattered and thrown out by a meteorite impact explosion and coated with molten rock material before the rock fell to the surface.

  2. Characteristics of core sampling from crumbing Paleozoic rock

    Energy Technology Data Exchange (ETDEWEB)

    Barabashkin, I I; Edelman, Y A; Filippov, V N; Lychev, V N

    1981-01-01

    The results of analysis of core sampling using standard core sampling tools with small and medium inside diameter are cited. It is demonstrated that when using these tools loss of core in Paleozoic deposits promising with regard to oil and gas content does not exceed 25 - 30%. The use of a new core sampling tool with a large inside diameter which includes drill bits of different types and a core lifter ''Krembriy'' SKU-172/100 made it possible to increase core removal approximately 52%. A representative core from a highly crumbling and vesicular rock belinging to groups III - IV in terms of difficulty of core sampling was obtained first. A description of a new core sampling tool is given. The characteristics of the technology of its use which promote preservation of the core are cited. Means of continued improvement of this tool are noted.

  3. Solid images for geostructural mapping and key block modeling of rock discontinuities

    Science.gov (United States)

    Assali, Pierre; Grussenmeyer, Pierre; Villemin, Thierry; Pollet, Nicolas; Viguier, Flavien

    2016-04-01

    Rock mass characterization is obviously a key element in rock fall hazard analysis. Managing risk and determining the most adapted reinforcement method require a proper understanding of the considered rock mass. Description of discontinuity sets is therefore a crucial first step in the reinforcement work design process. The on-field survey is then followed by a structural modeling in order to extrapolate the data collected at the rock surface to the inner part of the massif. Traditional compass survey and manual observations can be undoubtedly surpassed by dense 3D data such as LiDAR or photogrammetric point clouds. However, although the acquisition phase is quite fast and highly automated, managing, handling and exploiting such great amount of collected data is an arduous task and especially for non specialist users. In this study, we propose a combined approached using both 3D point clouds (from LiDAR or image matching) and 2D digital images, gathered into the concept of ''solid image''. This product is the connection between the advantages of classical true colors 2D digital images, accessibility and interpretability, and the particular strengths of dense 3D point clouds, i.e. geometrical completeness and accuracy. The solid image can be considered as the information support for carrying-out a digital survey at the surface of the outcrop without being affected by traditional deficiencies (lack of data and sampling difficulties due to inaccessible areas, safety risk in steep sectors, etc.). Computational tools presented in this paper have been implemented into one standalone software through a graphical user interface helping operators with the completion of a digital geostructural survey and analysis. 3D coordinates extraction, 3D distances and area measurement, planar best-fit for discontinuity orientation, directional roughness profiles, block size estimation, and other tools have been experimented on a calcareous quarry in the French Alps.

  4. Frictional sliding tests on combined coal-rock samples

    Directory of Open Access Journals (Sweden)

    Tao Wang

    2014-06-01

    Full Text Available A test system was developed to understand the sliding mechanism of coal-rock structure. The test system was composed by a double-shear testing model and an acousto-optic monitoring system in association with a digital camera and an acoustic emission (AE instrument. The tests can simulate the movement of activated faults and the sliding in coal-rock structure. In this regard, instable sliding conditions of coal-rock samples, sliding types under different conditions, displacement evolution law, and AE characteristics during sliding process were investigated. Several sliding types were monitored in the tests, including unstable continuous sliding, unstable discontinuous sliding, and stable sliding. The sliding types have close relation with the axial loads and loading rates. Larger axial load and smaller loading rate mean that unstable sliding is less likely to occur. The peak shear stress was positively correlated with the axial load when sliding occurred, whereas the displacement induced by unstable sliding was uncorrelated with the axial load. A large number of AE events occurred before sliding, and the AE rate decreased after stable sliding. The results show that the tests can well simulate the process of structural instability in a coal bump, and are helpful in the understanding of fault activation and the physical processes during squeezing process of roof and floor.

  5. Air sampling with solid phase microextraction

    Science.gov (United States)

    Martos, Perry Anthony

    There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

  6. Rock samples from LEP/LHC tunnel excavation

    CERN Multimedia

    1985-01-01

    Rock samples taken from 0 to 170 m below ground on the CERN site when the LEP (Large Electron Positron collider) pit number 6 was drilled in Bois-chatton (Versonnex). The challenges of LHC civil engineering: A mosaic of works, structures and workers of differents crafts and origins. Three consulting consortia for the engineering and the follow-up of the works. Four industrial consortia for doing the job. A young team of 25 CERN staff, 30 surface buildings, 32 caverns of all sizes, 170 000 m3 of concrete, 420 000 m3 excavated. 1998-2004 : six years of work and 340 millions Swiss Francs.

  7. Mineralogical, chemical, and petrographic analysis of selected rock samples

    International Nuclear Information System (INIS)

    Roy, D.M.

    1976-01-01

    I. The majority of rocks examined from the NTS were found to be siltstones, varying from coarse into the very fine siltstone range, and containing > 60% quartz, usually much higher. Samples of the UEIL series of cores, in contrast, had a large clay mineral fraction, as well as some carbonate present. A few were intermediate silty claystones or argillites. Microphotographs are included to illustrate the variations in texture observed, while most of the data obtained are summarized in tabular form. II. Seven Michigan Salina evaporite specimens were analyzed

  8. Sampling of solid particles in clouds

    International Nuclear Information System (INIS)

    Feuillebois, F.; Lasek, A.; Scibilia, M.F.

    1986-01-01

    This paper is concerned with the sampling of small solid particles from clouds by an airborne apparatus to be mounted on an airplane for meteorological investigations. In the airborne experiment the particles entering the test tube should be as representative as possible of the upstream conditions ahead of the plane, in the real cloud. Due to the inertia of the particles, the proportion of the different sizes of particles entering the test tube depends on the location of the tube mouth. We present a method of calculating the real concentration in particles of different sizes, using the results of measurements executed during the flight of an airplane in a cloud. Two geometries are considered: the nose of the airplane, represented schematically by a hemisphere, and a wing represented by a (2D) Joukowski profile which matches well a NACA 0015 profile on its leading edge

  9. Transient diffusion from a waste solid into fractured porous rock

    International Nuclear Information System (INIS)

    Ahn, J.; Chambre, P.L.; Pigford, T.H.

    1988-01-01

    Previous analytical studies of the advective transport of dissolved contaminants through fractured rock have emphasized the effect of molecular diffusion in the rock matrix in affecting the space-time-dependent concentration of the contaminant as it moves along the fracture. Matrix diffusion only in the direction normal to the fracture surface was assumed. Contaminant sources were constant-concentration surfaces of width equal to the fracture aperture and of finite or infinite extent in the transverse direction. Such studies illustrate the far-field transport features of fractured media. To predict the time-dependent mass transfer from a long waste cylinder surrounded by porous rock and intersected by a fracture, the present study includes diffusion from the waste surface directly into porous rock, as well as the more realistic geometry. Here the authors present numerical results from Chambre's analytical solution for the time-dependent mass transfer from the cylinder for the low-flow conditions wherein near-field mass transfer is expected to be controlled by molecular diffusion

  10. Attempt of groundwater dating using the drilled rock core. 1. Development of the rock sampling method for measurement of noble gases dissolved in interstitial water in rock

    International Nuclear Information System (INIS)

    Mahara, Yasunori

    2002-01-01

    Groundwater dating in low permeable rock is very difficult and impracticable, because we take a very long time to collect groundwater sample in a borehole and have to invest much fund in production of the in-situ groundwater sampler and in operation of it. If we can directly measure noble gases dissolved in interstitial groundwater in rock core, we have a big merit to estimate groundwater resident time easy. In this study, we designed and produced a high vacuum container to let dissolved noble gases diffuse until reaching in equilibrium, and we made a handling manual of the rock core into the container and a procedure to vacuum out air from the sealed container. We compared data sets of noble gas concentration obtained from rock cores and groundwater sample collected from boreholes in-situ. The measured rocks are pumice-tuff rock, mud rock and hornfels, which have their permeabilities of 10 -6 cm/s, 10 -9 cm/s and 10 -11 cm/s, respectively. Consequently, we evaluated the rock core method is better than the in-situ groundwater sampling method for low permeable rock. (author)

  11. Sampling and treatment of rock cores and groundwater under reducing environments of deep underground

    International Nuclear Information System (INIS)

    Ebashi, Katsuhiro; Yamaguchi, Tetsuji; Tanaka, Tadao

    2005-01-01

    A method of sampling and treatment of undisturbed rock cores and groundwater under maintained reducing environments of deep underground was developed and demonstrated in a Neogene's sandy mudstone layer at depth of GL-100 to -200 m. Undisturbed rock cores and groundwater were sampled and transferred into an Ar gas atmospheric glove box with minimized exposure to the atmosphere. The reducing conditions of the sampled groundwater and rock cores were examined in the Ar atmospheric glove box by measuring pH and Eh of the sampled groundwater and sampled groundwater contacting with disk type rock samples, respectively. (author)

  12. Three wave mixing test of hyperelasticity in highly nonlinear solids: sedimentary rocks.

    Science.gov (United States)

    D'Angelo, R M; Winkler, K W; Johnson, D L

    2008-02-01

    Measurements of three-wave mixing amplitudes on solids whose third order elastic constants have also been measured by means of the elasto-acoustic effect are reported. Because attenuation and diffraction are important aspects of the measurement technique results are analyzed using a frequency domain version of the KZK equation, modified to accommodate an arbitrary frequency dependence to the attenuation. It is found that the value of beta so deduced for poly(methylmethacrylate) (PMMA) agrees quite well with that predicted from the stress-dependent sound speed measurements, establishing that PMMA may be considered a hyperelastic solid, in this context. The beta values of sedimentary rocks, though they are typically two orders of magnitude larger than, e.g., PMMA's, are still a factor of 3-10 less than those predicted from the elasto-acoustic effect. Moreover, these samples exhibit significant heterogeneity on a centimeter scale, which heterogeneity is not apparent from a measurement of the position dependent sound speed.

  13. Imaging fluid/solid interactions in hydrocarbon reservoir rocks.

    Science.gov (United States)

    Uwins, P J; Baker, J C; Mackinnon, I D

    1993-08-01

    The environmental scanning electron microscope (ESEM) has been used to image liquid hydrocarbons in sandstones and oil shales. Additionally, the fluid sensitivity of selected clay minerals in hydrocarbon reservoirs was assessed via three case studies: HCl acid sensitivity of authigenic chlorite in sandstone reservoirs, freshwater sensitivity of authigenic illite/smectite in sandstone reservoirs, and bleach sensitivity of a volcanic reservoir containing abundant secondary chlorite/corrensite. The results showed the suitability of using ESEM for imaging liquid hydrocarbon films in hydrocarbon reservoirs and the importance of simulating in situ fluid-rock interactions for hydrocarbon production programmes. In each case, results of the ESEM studies greatly enhanced prediction of reservoir/borehole reactions and, in some cases, contradicted conventional wisdom regarding the outcome of potential engineering solutions.

  14. Inorganic mass spectrometry of solid samples

    International Nuclear Information System (INIS)

    Adams, F.; Vertes, A.

    1990-01-01

    In this review some recent developments in the field of inorganic mass spectrometry of solids are described with special emphasis on the actual state of understanding of the ionization processes. It concentrates on the common characteristics of methods such as spark source-, laser-, secondary ion-, inductively coupled plasma- and glow discharge mass spectrometry. (orig.)

  15. Microstructural controls on the macroscopic behavior of geo-architected rock samples

    Science.gov (United States)

    Mitchell, C. A.; Pyrak-Nolte, L. J.

    2017-12-01

    Reservoir caprocks, are known to span a range of mechanical behavior from elastic granitic units to visco-elastic shale units. Whether a rock will behave elastically, visco-elastically or plastically depends on both the compositional and textural or microsctructural components of the rock, and how these components are spatially distributed. In this study, geo-architected caprock fabrication was performed to develop synthetic rock to study the role of rock rheology on fracture deformations, fluid flow and geochemical alterations. Samples were geo-architected with Portland Type II cement, Ottawa sand, and different clays (kaolinite, illite, and Montmorillonite). The relative percentages of these mineral components are manipulated to generate different rock types. With set protocols, the mineralogical content, texture, and certain structural aspects of the rock were controlled. These protocols ensure that identical samples with the same morphological and mechanical characteristics are constructed, thus overcoming issues that may arise in the presence of heterogeneity and high anisotropy from natural rock samples. Several types of homogeneous geo-architected rock samples were created, and in some cases the methods were varied to manipulate the physical parameters of the rocks. Characterization of rocks that the samples exhibit good repeatability. Rocks with the same mineralogical content generally yielded similar compressional and shear wave velocities, UCS and densities. Geo-architected rocks with 10% clay in the matrix had lower moisture content and effective porosities than rocks with no clay. The process by which clay is added to the matrix can strongly affect the resulting compressive strength and physical properties of the geo-architected sample. Acknowledgment: This material is based upon work supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, Geosciences Research Program under Award Number (DE-FG02-09ER16022).

  16. Correlations fo Sc, rare earths and other elements in selected rock samples from Arrua-i

    Energy Technology Data Exchange (ETDEWEB)

    Facetti, J F; Prats, M [Asuncion Nacional Univ. (Paraguay). Inst. de Ciencias

    1972-01-01

    The Sc and Eu contents in selected rocks samples from the stock of Arrua-i have been determined and correlations established with other elements and with the relative amount of some rare earths. These correlations suggest metasomatic phenomena for the formation of the rock samples.

  17. Correlations fo Sc, rare earths and other elements in selected rock samples from Arrua-i

    International Nuclear Information System (INIS)

    Facetti, J.F.; Prats, M.

    1972-01-01

    The Sc and Eu contents in selected rocks samples from the stock of Arrua-i have been determined and correlations established with other elements and with the relative amount of some rare earths. These correlations suggest metasomatic phenomena for the formation of the rock samples

  18. Paraffin scintillator for radioassay of solid support samples

    International Nuclear Information System (INIS)

    Fujii, Haruo; Takiue, Makoto

    1989-01-01

    A new paraffin scintillator used for solid support sample counting has been proposed, and its composition and various characteristics are described. The solid support sample treated with this scintillator can be easily handled because of rigid sample conditions. This technique provides great advantages such as the elimination of a large volume of scintillator and little radioactive waste material by using an economical polyethylene bag instead of the conventional counting vial. (author)

  19. Determination of 210Pb and 210Po in soil or rock samples containing refractory matrices

    International Nuclear Information System (INIS)

    Jia Guogang; Torri, Giancarlo

    2007-01-01

    A new method has been developed for determination of 21 Pb and 21 Po in soil or rock samples containing refractory matrices. The samples were first fused with Na 2 CO 3 and Na 2 O 2 at 600 o C for pre-treatment and then 210 Pb and 210 Po were sequentially leached out at 200-250 o C with HNO 3 +HF, HClO 4 and HCl. About 10% of the leaching solution was used for 21 Po determination, carried out by spontaneous deposition of polonium on a silver disc from a weakly acidic solution that contained hydroxylamine hydrochloride, sodium citrate and 209 Po tracer, measurement being made by α-spectrometry. The remains of the leaching solution were used for determination of 21 Pb, conducted by precipitation as sulphate, purification with Na 2 S as PbS in 6 M ammonium acetate, separation from α-emitters by an anion-exchange resin column, source preparation as PbSO 4 , and measurement with a β-counter. The procedure has been checked with two certified IAEA reference materials, showing good agreement with the recommended values. The lower limits of detection for 1 g of analysed soil or rock samples were found to be 0.75 Bq kg -1 for 210 Po and 2.2 Bq kg -1 for 210 Pb. A variety of solid sample species analysed through use of the procedure gave average yields of 90.0±9.8% for 210 Po and 88.4±7.1% for 210 Pb

  20. Fast sampling calorimetry with solid argon ionization chambers

    International Nuclear Information System (INIS)

    Clark, E.; Linn, S.; Piekarz, H.; Wahl, H.; Womersley, J.; Hansen, S.; Hurh, P.; Rivetta, C.; Sanders, R.; Schmitt, R.; Stanek, R.; Stefanik, A.

    1992-01-01

    A proposal for the fast sampling calorimetry with solid argon as active medium and the preliminary results from the solid argon test cell are presented. The proposed test calorimeter module structure, the signal routing and the mechanical and cryogenic arrangements are also discussed

  1. Laser solid sampling for a solid-state-detector ICP emission spectrometer

    International Nuclear Information System (INIS)

    Noelte, J.; Moenke-Blankenburg, L.; Schumann, T.

    1994-01-01

    Solid sampling with laser vaporization has been coupled to an ICP emission spectrometer with an Echelle optical system and a solid-state-detector for the analysis of steel and soil samples. Pulsation of the vaporized material flow was compensated by real-time background correction and internal standardization, resulting in good accuracy and precision. (orig.)

  2. Measurement of solid flow rates and sampling

    International Nuclear Information System (INIS)

    Caillot, A.

    1984-01-01

    Given the fact that very fine sediments are carriers of numerous pollutant products, in order to be able to ensure realistic and vigilant control of the aquatic environment we have to take into account sedimentary transport. The movement of sediments may be due to natural events (currents, swell, winds), or to human intervention (dredging, emptying of dam reservoirs, release of wastes and so forth). Their circulation, at times highly complex, especially in estuaries, may alternate with periods of rest - and therefore periods of accumulation of pollutants - which may be fairly long. Despite the plethora of available methods and techniques, the amounts of sediment transported by drift or in suspension are very difficult to assess. The physico-chemical nature and the behaviour of these substances in water makes it awkward to select samples, in space and time, for the purpose of analysis. The sampling should be carried out with the mechanical means suited to the circumstances and to the aim in mind. However, by taking into consideration the hydrosedimentary mechanisms known by the hydrologists and sedimentologists it is possible to improve the selection of the sites to be monitored as well as to choose more carefully (and therefore to limit) the samples to be analysed. Environmental monitoring may thus be performed more efficiently and at lower cost. (author)

  3. Solid images generated from UAVs to analyze areas affected by rock falls

    Science.gov (United States)

    Giordan, Daniele; Manconi, Andrea; Allasia, Paolo; Baldo, Marco

    2015-04-01

    The study of rock fall affected areas is usually based on the recognition of principal joints families and the localization of potential instable sectors. This requires the acquisition of field data, although as the areas are barely accessible and field inspections are often very dangerous. For this reason, remote sensing systems can be considered as suitable alternative. Recently, Unmanned Aerial Vehicles (UAVs) have been proposed as platform to acquire the necessary information. Indeed, mini UAVs (in particular in the multi-rotors configuration) provide versatility for the acquisition from different points of view a large number of high resolution optical images, which can be used to generate high resolution digital models relevant to the study area. By considering the recent development of powerful user-friendly software and algorithms to process images acquired from UAVs, there is now a need to establish robust methodologies and best-practice guidelines for correct use of 3D models generated in the context of rock fall scenarios. In this work, we show how multi-rotor UAVs can be used to survey areas by rock fall during real emergency contexts. We present two examples of application located in northwestern Italy: the San Germano rock fall (Piemonte region) and the Moneglia rock fall (Liguria region). We acquired data from both terrestrial LiDAR and UAV, in order to compare digital elevation models generated with different remote sensing approaches. We evaluate the volume of the rock falls, identify the areas potentially unstable, and recognize the main joints families. The use on is not so developed but probably this approach can be considered the better solution for a structural investigation of large rock walls. We propose a methodology that jointly considers the Structure from Motion (SfM) approach for the generation of 3D solid images, and a geotechnical analysis for the identification of joint families and potential failure planes.

  4. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    OpenAIRE

    Helena Prosen

    2014-01-01

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several...

  5. Preparation of rock samples for measurement of the thermal neutron macroscopic absorption cross-section

    International Nuclear Information System (INIS)

    Czubek, J.A.; Burda, J.; Drozdowicz, K.; Igielski, A.; Kowalik, W.; Krynicka-Drozdowicz, E.; Woznicka, U.

    1986-03-01

    Preparation of rock samples for the measurement of the thermal neutron macroscopic absorption cross-section in small cylindrical two-region systems by a pulsed technique is presented. Requirements which should be fulfilled during the preparation of the samples due to physical assumptions of the method are given. A cylindrical vessel is filled with crushed rock and saturated with a medium strongly absorbing thermal neutrons. Water solutions of boric acid of well-known macroscopic absorption cross-section are used. Mass contributions of the components in the sample are specified. This is necessary for the calculation of the thermal neutron macroscopic absorption cross-section of the rock matrix. The conditions necessary for assuring the required accuracy of the measurement are given and the detailed procedure of preparation of the rock sample is described. (author)

  6. Proceedings of a technical session on rock mechanics ''Advance in laboratory sample testing''

    International Nuclear Information System (INIS)

    Come, B.

    1984-01-01

    This report brings together a series of papers about rock mechanics. The meeting was divided into three sessions, which dealt with the three main types of rock formation currently considered in the CEC Programme: granite, clay and salt. Safe disposal of high-level radioactive waste involves the proper design of deep underground repositories. This necessitates an in-depth knowledge of the mechanical properties of the rock mass. The behaviour of the rock mass must be known both for the construction and the operation (heating effects) of the repository. Usually, the dominant factor for designing an underground structure is the fracturing of the rock mass. In the present case, the rock is chosen with a very low fracturing. Therefore, the mechanical properties of the formation are mainly those of the rock matrix. These properties are obtained, at least in a first exploratory step, by laboratory testing of rock samples obtained by core-drilling from surface. This aspect of rock characterization was thought to deserve a special technical meeting, in order to bring together most of the results obtained in this field by contracting partners of the CEC for the years 1980-82

  7. Solid Phase Characterization of Tank 241-C-105 Grab Samples

    International Nuclear Information System (INIS)

    Ely, T. M.; LaMothe, M. E.; Lachut, J. S.

    2016-01-01

    The solid phase characterization (SPC) of three grab samples from single-shell Tank 241-C-105 (C-105) that were received at the laboratory the week of October 26, 2015, has been completed. The three samples were received and broken down in the 11A hot cells.

  8. Solid-phase microextraction for the analysis of biological samples

    NARCIS (Netherlands)

    Theodoridis, G; Koster, EHM; de Jong, GJ

    2000-01-01

    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

  9. Study on natural radioactive elements in soil and rock samples around Mandya district, India

    International Nuclear Information System (INIS)

    Shivakumara, B.C.; Paramesh, L.; Shashikumar, T.S.; Chandrashekara, M.S.

    2012-01-01

    The soil is a complex mixture of different compounds and rocks. In the natural environment, it is an important source of exposure to radiation due to naturally occurring, gamma emitting radionuclides which include 226 Ra, 232 Th and 40 K present in the soil. The study of distribution of these radionuclides in soil and rock is of great importance for radiation protection and measurements. The activity concentrations of 226 Ra, 232 Th, and 40 K in soil and rock samples collected in Mandya District, Karnataka state, India have been measured by gamma ray spectrometry. The average activity concentrations of 226 Ra, 232 Th, and 40 K (Bq/kg) are found to be 40.2, 62.3, and 317.5 Bq/kg, respectively, in soil samples and 30.5, 34.4, and 700.2 Bq/kg, respectively, in rock samples. The concentrations of radionuclides in soil samples are found to higher than in rock samples. The concentrations of radionuclides in soil and rock samples in the study area are slightly higher than Indian average and world average values. (author)

  10. A new method for automatic discontinuity traces sampling on rock mass 3D model

    Science.gov (United States)

    Umili, G.; Ferrero, A.; Einstein, H. H.

    2013-02-01

    A new automatic method for discontinuity traces mapping and sampling on a rock mass digital model is described in this work. The implemented procedure allows one to automatically identify discontinuity traces on a Digital Surface Model: traces are detected directly as surface breaklines, by means of maximum and minimum principal curvature values of the vertices that constitute the model surface. Color influence and user errors, that usually characterize the trace mapping on images, are eliminated. Also trace sampling procedures based on circular windows and circular scanlines have been implemented: they are used to infer trace data and to calculate values of mean trace length, expected discontinuity diameter and intensity of rock discontinuities. The method is tested on a case study: results obtained applying the automatic procedure on the DSM of a rock face are compared to those obtained performing a manual sampling on the orthophotograph of the same rock face.

  11. Thermal neutron absorption cross-section measured on rock samples and brines in the Institute of Nuclear Physics

    International Nuclear Information System (INIS)

    Czubek, J.A.; Drozdowicz, K.; Krynicka-Drozdowicz, E.; Igielski, A.; Woznicka, U.

    1983-01-01

    In consecutive measurements the rock sample (having a fixed and well known shape -in our case it is a sphere or a cylinder and the sample is powdered or liquid) is enveloped in shells of a plexiglass moderator (the neutron parameters of which are known) of variable thickness and irradiated with the pulsed beam of fast neutrons. The die-away rate of thermal neutrons escaping from the whole system is measured. The absorption cross-section of the sample is found as the intersection of the experimental curve (i.e. die -away rate vs thickness of the moderator) with the theoretical one. The theoretical curve is calculated for a given moderator under the assumption of a constant value of the neutron flux inside the sample. This method is independent of the value of the transport cross-section of the sample. It has been checked on artificial materials with a well known elemental composition (liquid or solid) and on the natural brines and rock samples (basalts and dolomite). A special method of calculation of the variance of the measurement has been established. It is based on the multiple computer simulations of all experimental data used in the computation. The one standard deviation of our methods is of the order of 1 up to 3 capture units (1 c.u. = 10 -3 cm -1 ). The volume of the sample needed is of the order of 500ccm. (author)

  12. Procedures for sampling and sample-reduction within quality assurance systems for solid biofuels

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2005-04-15

    The bias introduced when sampling solid biofuels from stockpiles or containers instead of from moving streams is assessed as well as the number and size of samples required to represent accurately the bulk sample, variations introduced when reducing bulk samples into samples for testing, and the usefulness of sample reduction methods. Details are given of the experimental work carried out in Sweden and Denmark using sawdust, wood chips, wood pellets, forestry residues and straw. The production of a model European Standard for quality assurance of solid biofuels is examined.

  13. Solid-Gas Coupling Model for Coal-Rock Mass Deformation and Pressure Relief Gas Flow in Protection Layer Mining

    OpenAIRE

    Zhu, Zhuohui; Feng, Tao; Yuan, Zhigang; Xie, Donghai; Chen, Wei

    2018-01-01

    The solid-gas coupling model for mining coal-rock mass deformation and pressure relief gas flow in protection layer mining is the key to determine deformation of coal-rock mass and migration law of pressure relief gas of protection layer mining in outburst coal seams. Based on the physical coupling process between coal-rock mass deformation and pressure-relief gas migration, the coupling variable of mining coal-rock mass, a part of governing equations of gas seepage field and deformation fiel...

  14. A new sampling technique for surface exposure dating using a portable electric rock cutter

    Directory of Open Access Journals (Sweden)

    Yusuke Suganuma

    2012-07-01

    Full Text Available Surface exposure dating using in situ cosmogenic nuclides has contributed to our understanding of Earth-surface processes. The precision of the ages estimated by this method is affected by the sample geometry; therefore, high accuracy measurements of the thickness and shape of the rock sample (thickness and shape is crucial. However, it is sometimes diffi cult to meet these requirements by conventional sampling methods with a hammer and chisel. Here, we propose a new sampling technique using a portable electric rock cutter. This sampling technique is faster, produces more precisely shaped samples, and allows for a more precise age interpretation. A simple theoretical modeldemonstrates that the age error due to defective sample geometry increases as the total sample thickness increases, indicating the importance of precise sampling for surface exposure dating.

  15. Rock Gripper for Sampling, Mobility, Anchoring, and Manipulation

    Science.gov (United States)

    Parness, Aaron

    2013-01-01

    A new gripper mechanism can be used as an end effector for a long arm that reaches out from a nearby spacecraft for a touch-and-go type of mission. The gripper would stabilize the arm and allow samples to be collected and in situ science to be done from a fixed platform. In the long term, this style of gripper could even be used as handholds for astronauts trying to move about on/near small asteroids. The prototype developed has demonstrated a 120 N gripping force, and improvements continue to be made.

  16. An axisymmetric diffusion experiment for the determination of diffusion and sorption coefficients of rock samples.

    Science.gov (United States)

    Takeda, M; Hiratsuka, T; Ito, K; Finsterle, S

    2011-04-25

    Diffusion anisotropy is a critical property in predicting migration of substances in sedimentary formations with very low permeability. The diffusion anisotropy of sedimentary rocks has been evaluated mainly from laboratory diffusion experiments, in which the directional diffusivities are separately estimated by through-diffusion experiments using different rock samples, or concurrently by in-diffusion experiments in which only the tracer profile in a rock block is measured. To estimate the diffusion anisotropy from a single rock sample, this study proposes an axisymmetric diffusion test, in which tracer diffuses between a cylindrical rock sample and a surrounding solution reservoir. The tracer diffusion between the sample and reservoir can be monitored from the reservoir tracer concentrations, and the tracer profile could also be obtained after dismantling the sample. Semi-analytical solutions are derived for tracer concentrations in both the reservoir and sample, accounting for an anisotropic diffusion tensor of rank two as well as the dilution effects from sampling and replacement of reservoir solution. The transient and steady-state analyses were examined experimentally and numerically for different experimental configurations, but without the need for tracer profiling. These experimental configurations are tested for in- and out-diffusion experiments using Koetoi and Wakkanai mudstones and Shirahama sandstone, and are scrutinized by a numerical approach to identify favorable conditions for parameter estimation. The analysis reveals the difficulty in estimating diffusion anisotropy; test configurations are proposed for enhanced identifiability of diffusion anisotropy. Moreover, it is demonstrated that the axisymmetric diffusion test is efficient in obtaining the sorption parameter from both steady-state and transient data, and in determining the effective diffusion coefficient if isotropic diffusion is assumed. Moreover, measuring reservoir concentrations in an

  17. An asixymmetric diffusion experiment for the determination of diffusion and sorption coefficients of rock samples

    Energy Technology Data Exchange (ETDEWEB)

    Takeda, M.; Hiratsuka, T.; Ito, K.; Finsterle, S.

    2011-02-01

    Diffusion anisotropy is a critical property in predicting migration of substances in sedimentary formations with very low permeability. The diffusion anisotropy of sedimentary rocks has been evaluated mainly from laboratory diffusion experiments, in which the directional diffusivities are separately estimated by through-diffusion experiments using different rock samples, or concurrently by in-diffusion experiments in which only the tracer profile in a rock block is measured. To estimate the diffusion anisotropy from a single rock sample, this study proposes an axisymmetric diffusion test, in which tracer diffuses between a cylindrical rock sample and a surrounding solution reservoir. The tracer diffusion between the sample and reservoir can be monitored from the reservoir tracer concentrations, and the tracer profile could also be obtained after dismantling the sample. Semi-analytical solutions are derived for tracer concentrations in both the reservoir and sample, accounting for an anisotropic diffusion tensor of rank two as well as the dilution effects from sampling and replacement of reservoir solution. The transient and steady-state analyses were examined experimentally and numerically for different experimental configurations, but without the need for tracer profiling. These experimental configurations are tested for in- and out-diffusion experiments using Koetoi and Wakkanai mudstones and Shirahama sandstone, and are scrutinized by a numerical approach to identify favorable conditions for parameter estimation. The analysis reveals the difficulty in estimating diffusion anisotropy; test configurations are proposed for enhanced identifiability of diffusion anisotropy. Moreover, it is demonstrated that the axisymmetric diffusion test is efficient in obtaining the sorption parameter from both steady-state and transient data, and in determining the effective diffusion coefficient if isotropic diffusion is assumed. Moreover, measuring reservoir concentrations in an

  18. NASA Lunar Sample Education Disk Program - Space Rocks for Classrooms, Museums, Science Centers and Libraries

    Science.gov (United States)

    Allen, J. S.

    2009-12-01

    NASA is eager for students and the public to experience lunar Apollo rocks and regolith soils first hand. Lunar samples embedded in plastic are available for educators to use in their classrooms, museums, science centers, and public libraries for education activities and display. The sample education disks are valuable tools for engaging students in the exploration of the Solar System. Scientific research conducted on the Apollo rocks has revealed the early history of our Earth-Moon system. The rocks help educators make the connections to this ancient history of our planet as well as connections to the basic lunar surface processes - impact and volcanism. With these samples educators in museums, science centers, libraries, and classrooms can help students and the public understand the key questions pursued by missions to Moon. The Office of the Curator at Johnson Space Center is in the process of reorganizing and renewing the Lunar and Meteorite Sample Education Disk Program to increase reach, security and accountability. The new program expands the reach of these exciting extraterrestrial rocks through increased access to training and educator borrowing. One of the expanded opportunities is that trained certified educators from science centers, museums, and libraries may now borrow the extraterrestrial rock samples. Previously the loan program was only open to classroom educators so the expansion will increase the public access to the samples and allow educators to make the critical connections of the rocks to the exciting exploration missions taking place in our solar system. Each Lunar Disk contains three lunar rocks and three regolith soils embedded in Lucite. The anorthosite sample is a part of the magma ocean formed on the surface of Moon in the early melting period, the basalt is part of the extensive lunar mare lava flows, and the breccias sample is an important example of the violent impact history of the Moon. The disks also include two regolith soils and

  19. Assessment of two kinetic tests to predict the acid mine drainage in waste rock samples of a uranium mine

    OpenAIRE

    Abreu,Adriana Trópia de; Faria,Efigênia Miranda de; Chaves,Carla Thamilis Fonseca; Leite,Adilson do Lago; Lena,Jorge Carvalho de

    2014-01-01

    Acid mine drainage is the result of the oxidation process of sulfide bearing rocks. This process occurs when the sulfide material is exposed to atmospheric conditions. Under these conditions, successive oxidation reactions yield sulfuric acid generating acidic waters. This problem becomes more serious when the surrounding rocks are not able to neutralize the acid. The low pH condition of the drained water accelerates the solubility process of solid materials (rocks, soils and sediments) and f...

  20. Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  1. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  2. Cr(VI) generation during sample preparation of solid samples – A ...

    African Journals Online (AJOL)

    Cr(VI) generation during sample preparation of solid samples – A chromite ore case study. R.I Glastonbury, W van der Merwe, J.P Beukes, P.G van Zyl, G Lachmann, C.J.H Steenkamp, N.F Dawson, M.H Stewart ...

  3. PDS Archive Release of Apollo 11, Apollo 12, and Apollo 17 Lunar Rock Sample Images

    Science.gov (United States)

    Garcia, P. A.; Stefanov, W. L.; Lofgren, G. E.; Todd, N. S.; Gaddis, L. R.

    2013-01-01

    Scientists at the Johnson Space Center (JSC) Lunar Sample Laboratory, Information Resources Directorate, and Image Science & Analysis Laboratory have been working to digitize (scan) the original film negatives of Apollo Lunar Rock Sample photographs [1, 2]. The rock samples, and associated regolith and lunar core samples, were obtained during the Apollo 11, 12, 14, 15, 16 and 17 missions. The images allow scientists to view the individual rock samples in their original or subdivided state prior to requesting physical samples for their research. In cases where access to the actual physical samples is not practical, the images provide an alternate mechanism for study of the subject samples. As the negatives are being scanned, they have been formatted and documented for permanent archive in the NASA Planetary Data System (PDS). The Astromaterials Research and Exploration Science Directorate (which includes the Lunar Sample Laboratory and Image Science & Analysis Laboratory) at JSC is working collaboratively with the Imaging Node of the PDS on the archiving of these valuable data. The PDS Imaging Node is now pleased to announce the release of the image archives for Apollo missions 11, 12, and 17.

  4. Localisation and identification of radioactive particles in solid samples by means of a nuclear track technique

    International Nuclear Information System (INIS)

    Boehnke, Antje; Treutler, Hanns-Christian; Freyer, Klaus; Schubert, Michael; Holger Weiss

    2005-01-01

    This study is aimed to develop a generally applicable methodology of investigation that can be used for the localisation of single alpha-active particles in solid samples, such as industrial dust or natural soils, sediments and rocks by autoradiography using solid-state nuclear track detectors. The developed technique allows the detection of local enrichments of alpha-emitters in any solid material. The results of such an investigation are of interest from technical, biological and environmental points of view. The idea behind the methodology is to locate the position of alpha-active spots in a sample by attaching the track detector to the sample in a defined manner, thoroughly described in the paper. The located alpha-active particles are subsequently analysed by an electron microscope and an electron microprobe. An example of the application of this methodology is also given. An ultra-fine -grained ore-processing residue, which causes serious environmental pollution in the respective mining district and thus limits possible land use and affects quality of life in the area, was examined using the described technique. The investigation revealed considerable amounts of alpha-active particles in this material

  5. Determination of uranium and thorium in rock samples from Harargaj Anticline by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Rahman, M.; Molla, N.I.; Sharif, A.K.M.; Basunia, S.; Islam, S.; Miah, R.U.; Hossain, S.M.; Chowdhury, M.I.; Bhuiyan, A.D.; Stegnar, P.

    1993-01-01

    Uranium and thorium were determined in geological materials such as radioactive rock samples collected from the Harargaj Anticline in Moulavi Bazar. The pure instrumental neutron activation analysis (INAA) technique was used in qualitative and quantitative analysis of the rock samples for U and Th. The samples were properly prepared together with their standards and simultaneously irradiated in a neutron flux of the order of 10 12 n*cm -2 *s -1 using the TRIGA MARK II research reactor facility at the AERE, Savar, Dhaka. After activation the samples were subjected to γ-ray spectrometry using a high purity germanium detection system. As a result of the analysis, U and Th could be determined. The data are consistent with the values reported by the ground radiometric survey group for some of the samples. (author) 7 refs.; 1 fig.; 2 tabs

  6. Permeability measurements on rock samples from Unzen Scientific Drilling Project Drill Hole 4 (USDP-4)

    Science.gov (United States)

    Watanabe, Tohru; Shimizu, Yuhta; Noguchi, Satoshi; Nakada, Setsuya

    2008-07-01

    Permeability measurement was made on five rock samples from USDP-4 cores. Rock samples were collected from the conduit zone and its country rock. One sample (C14-1-1) is considered as a part of the feeder dyke for the 1991-1995 eruption. The transient pulse method was employed under confining pressure up to 50 MPa. Compressional wave velocity was measured along with permeability. The measured permeability ranges from 10 - 19 to 10 - 17 m 2 at the atmospheric pressure, and is as low as that reported for tight rocks such as granite. The permeability decreases with increasing confining pressure, while the compressional wave velocity increases. Assuming that pores are parallel elliptical tubes, the pressure dependence of permeability requires aspect ratio of 10 - 4 -10 - 2 at the atmospheric pressure. The pore aperture is estimated to be less than 1 μm. The estimated aspect ratio and pore aperture suggest that connectivity of pores is maintained by narrow cracks. The existence of cracks is supported by the pressure dependence of compressional wave velocity. Narrow cracks (< 1 μm) are observed in dyke samples, and they must have been created after solidification. Dyke samples do not provide us information of pore structures during degassing, since exsolved gas has mostly escaped and pores governing the gas permeable flow should have been lost. Both dyke and country rock samples provide us information of materials around ascending magma. Although the measured small-scale permeability cannot be directly applied to geological-scale processes, it gives constrains on studies of large-scale permeability.

  7. Data Validation Package September 2016 Groundwater and Surface Water Sampling at the Slick Rock, Colorado, Processing Sites January 2017

    Energy Technology Data Exchange (ETDEWEB)

    Traub, David [Navarro Research and Engineering, Inc., Oak Ridge, TN (United States); Nguyen, Jason [US Department of Energy, Washington, DC (United States)

    2017-01-04

    The Slick Rock, Colorado, Processing Sites are referred to as the Slick Rock West Processing Site (SRK05) and the Slick Rock East Processing Site (SRK06). This annual event involved sampling both sites for a total of 16 monitoring wells and 6 surface water locations as required by the 2006 Draft Final Ground Water Compliance Action Plan for the Slick Rock, Colorado, Processing Sites (GCAP). A domestic well was also sampled at a property adjacent to the Slick Rock East site at the request of the landowner.

  8. Acoustic emission of quasi-isotropic rock samples initiated by temperature gradients

    Czech Academy of Sciences Publication Activity Database

    Vasin, R.N.; Nikitin, A. N.; Lokajíček, Tomáš; Rudajev, Vladimír

    2006-01-01

    Roč. 42, č. 10 (2006), s. 815-823 ISSN 1069-3513 Institutional research plan: CEZ:AV0Z30460519; CEZ:AV0Z30130516 Keywords : seismoacoustic emission * rock sample * temperature gradient Subject RIV: DB - Geology ; Mineralogy Impact factor: 0.092, year: 2006

  9. Mapping of uranium and thorium in radioactive rocks using nuclear track solid detectors

    International Nuclear Information System (INIS)

    Bouch, C.M.

    1982-01-01

    α-Autoradiography and studies of induced fission in a research nuclear reactor (IEA-R1, IPEN, Sao Paulo) were done, employing Solid-State Nuclear Track detectors, in order to study the distribution of α-emitters, U and Th in rocks. Polished sections of rocks were prepared and photographed. Etching conditions were studied in order to adapt the detectors to the studies of microdistribution and macrodistribution of tracks. Polycarbonate foils (Bayer, Makrofol) were chosen as fission-fragments detectors and the technique of fission induced with reactor neutrons to obtain the distribution of U and Th were studied. Uranium and thorium standards evaporated on the surface of the detectors, as well as thorite and uraninite grains, were irradiated in order to measure the integrated flux of neutrons, the effective cross sections for fission with reactor neutrons for 232 Th(0,05b) and 238 U(0,30b) and to study the contribution of 238 U fission in thorium mapping. A technique for determination of uranium and thorium in minerals was studied and applied to Mica, for which were determined the contents of 4,2 ppb U e 58 ppb Th. (Author) [pt

  10. Disposal of low- and intermediate-level solid radioactive wastes in rock cavities

    International Nuclear Information System (INIS)

    1983-01-01

    This Guidebook summarizes the factors to be considered and the activities to be undertaken in the overall planning and development of a disposal system for solid or solidified low- and intermediate-level wastes in rock cavities. Aspects related to repository site selection, design, construction, operation, shutdown, surveillance, regulation and safety assessment are discussed here in general terms. They will be covered in greater technical detail in a separate document. This report considers the emplacement of wastes in categories II, III, IV and V, as defined in Table 3.1, in different kinds of cavities located at various depths from just below the surface to deep continental rock. The choice of the type of cavity and its depth and of the disposal site itself is related to the radiological protection requirements for the wastes concerned. The repositories considered include natural caves and abandoned mines as well as specially excavated cavities in various geological formations. Consideration is also given to hydrogeological, environmental and societal factors. The guidelines given in the report are made sufficiently general to cover a broad variety of different circumstances. Consequently, the practical application of these guidelines needs a case-by-case consideration which takes into account the local conditions, e.g. natural circumstances, the characteristics of the wastes and national and international regulations and practices

  11. Disposal of low- and intermediate-level solid radioactive wastes in rock cavities. A guidebook

    Energy Technology Data Exchange (ETDEWEB)

    1983-01-01

    This Guidebook summarizes the factors to be considered and the activities to be undertaken in the overall planning and development of a disposal system for solid or solidified low- and intermediate-level wastes in rock cavities. Aspects related to repository site selection, design, construction, operation, shutdown, surveillance, regulation and safety assessment are discussed here in general terms. They will be covered in greater technical detail in a separate document. This report considers the emplacement of wastes in categories II, III, IV and V, as defined in Table 3.1, in different kinds of cavities located at various depths from just below the surface to deep continental rock. The choice of the type of cavity and its depth and of the disposal site itself is related to the radiological protection requirements for the wastes concerned. The repositories considered include natural caves and abandoned mines as well as specially excavated cavities in various geological formations. Consideration is also given to hydrogeological, environmental and societal factors. The guidelines given in the report are made sufficiently general to cover a broad variety of different circumstances. Consequently, the practical application of these guidelines needs a case-by-case consideration which takes into account the local conditions, e.g. natural circumstances, the characteristics of the wastes and national and international regulations and practices.

  12. GANSEKI: JAMSTEC Deep Seafloor Rock Sample Database Emerging to the New Phase

    Science.gov (United States)

    Tomiyama, T.; Ichiyama, Y.; Horikawa, H.; Sato, Y.; Soma, S.; Hanafusa, Y.

    2013-12-01

    Japan Agency for Marine-Earth Science and Technology (JAMSTEC) collects a lot of substantial samples as well as various geophysical data using its research vessels and submersibles. These samples and data, which are obtained by spending large amounts of human and physical resources, are precious wealth of the world scientific community. For the better use of these samples and data, it is important that they are utilized not only for initial purpose of each cruse but also for other general scientific and educational purposes of second-hand users. Based on the JAMSTEC data and sample handling policies [1], JAMSTEC has systematically stored samples and data obtained during research cruises, and provided them to domestic/foreign activities on research, education, and public relation. Being highly valued for second-hand usability, deep seafloor rock samples are one of the most important types of samples obtained by JAMSTEC, as oceanic biological samples and sediment core samples are. Rock samples can be utilized for natural history sciences and other various purposes; some of these purposes are connected to socially important issues such as earthquake mechanisms and mineral resource developments. Researchers and educators can access to JAMSTEC rock samples and associated data through 'GANSEKI [2]', the JAMSTEC Deep Seafloor Rock Sample Database. GANSEKI was established on the Internet in 2006 and its contents and functions have been continuously enriched and upgraded since then. GANSEKI currently provides 19 thousands of sample metadata, 9 thousands of collection inventory data and 18 thousands of geochemical data. Most of these samples are recovered from the North-western Pacific Ocean, although samples from other area are also included. The major update of GANSEKI held in May 2013 involved a replacement of database core system and a redesign of user interface. In the new GANSEKI, users can select samples easily and precisely using multi-index search, numerical

  13. Porosity, permeability and 3D fracture network characterisation of dolomite reservoir rock samples.

    Science.gov (United States)

    Voorn, Maarten; Exner, Ulrike; Barnhoorn, Auke; Baud, Patrick; Reuschlé, Thierry

    2015-03-01

    With fractured rocks making up an important part of hydrocarbon reservoirs worldwide, detailed analysis of fractures and fracture networks is essential. However, common analyses on drill core and plug samples taken from such reservoirs (including hand specimen analysis, thin section analysis and laboratory porosity and permeability determination) however suffer from various problems, such as having a limited resolution, providing only 2D and no internal structure information, being destructive on the samples and/or not being representative for full fracture networks. In this paper, we therefore explore the use of an additional method - non-destructive 3D X-ray micro-Computed Tomography (μCT) - to obtain more information on such fractured samples. Seven plug-sized samples were selected from narrowly fractured rocks of the Hauptdolomit formation, taken from wellbores in the Vienna basin, Austria. These samples span a range of different fault rocks in a fault zone interpretation, from damage zone to fault core. We process the 3D μCT data in this study by a Hessian-based fracture filtering routine and can successfully extract porosity, fracture aperture, fracture density and fracture orientations - in bulk as well as locally. Additionally, thin sections made from selected plug samples provide 2D information with a much higher detail than the μCT data. Finally, gas- and water permeability measurements under confining pressure provide an important link (at least in order of magnitude) towards more realistic reservoir conditions. This study shows that 3D μCT can be applied efficiently on plug-sized samples of naturally fractured rocks, and that although there are limitations, several important parameters can be extracted. μCT can therefore be a useful addition to studies on such reservoir rocks, and provide valuable input for modelling and simulations. Also permeability experiments under confining pressure provide important additional insights. Combining these and

  14. Analysis of mercury in rock varnish samples in areas impacted by coal-fired power plants

    International Nuclear Information System (INIS)

    Nowinski, Piotr; Hodge, Vernon F.; Gerstenberger, Shawn; Cizdziel, James V.

    2013-01-01

    Rock varnish is a manganese–iron rich coating that forms on rocks, most often in arid climates. To assess its utility as an environmental monitor of mercury contamination, cold vapor atomic absorption spectrometry (CVAAS) was used for analysis. Samples were collected in the fallout patterns of two coal-fired power plants in southern Nevada: the defunct Mohave Power Plant (MPP) and the operating Reid Gardner Power Plant (RGPP). The resultant Hg concentrations in rock varnishes were plotted as a function of the distance from each power plant. The highest concentrations of Hg occurred at locations that suggest the power plants are the main source of pollutants. In addition, past tracer plume studies carried out at MPP show that the highest tracer concentrations coincide with the highest rock varnish Hg concentrations. However, additional samples are required to further demonstrate that power plants are indeed the sources of mercury in varnishes. -- Highlights: •We analyze desert varnish samples collected in the fallout patterns of two coal-fired and analyzed for Hg by CVAA. •The resultant Hg concentrations in the desert varnish samples were plotted as a function of the distance from each power plant. •The highest concentrations of Hg occurred at locations that suggest the power plants are the main source of pollutants. •Data indicate the utility of desert varnish as a passive environmental monitor for Hg atmospheric pollution. -- Cold vapor atomic absorption spectrometry (CVAAS) was used for analysis of mercury in varnished rocks collected in the fallout zones of two coal-fired power plants

  15. SESAR: Addressing the need for unique sample identification in the Solid Earth Sciences

    Science.gov (United States)

    Lehnert, K. A.; Goldstein, S. L.; Lenhardt, C.; Vinayagamoorthy, S.

    2004-12-01

    The study of solid earth samples is key to our knowledge of Earth's dynamical systems and evolution. The data generated provide the basis for models and hypotheses in all disciplines of the Geosciences from tectonics to magmatic processes to mantle dynamics to paleoclimate research. Sample-based data are diverse ranging from major and trace element abundances, radiogenic and stable isotope ratios of rocks, minerals, fluid or melt inclusions, to age determinations and descriptions of lithology, texture, mineral or fossil content, stratigraphic context, physical properties. The usefulness of these data is critically dependent on their integration as a coherent data set for each sample. If different data sets for the same sample cannot be combined because the sample cannot be unambiguously recognized, valuable information is lost. The ambiguous naming of samples has been a major problem in the geosciences. Different samples are often given identical names, and there is a tendency for different people analyzing the same sample to rename it in their publications according to local conventions. This situation has generated significant confusion, with samples often losing their "history", making it difficult or impossible to link available data. This has become most evident through the compilation of geochemical data in relational databases such as PetDB, NAVDAT, and GEOROC. While the relational data structure allows linking of disparate data for samples published in different references, linkages cannot be established due to ambiguous sample names. SESAR is a response to this problem of ambiguous naming of samples. SESAR will create a common clearinghouse that provides a centralized registry of sample identifiers, to avoid ambiguity, to systematize sample designation, and ensure that all information associated with a sample would in fact be unique. The project will build a web-based digital registry for solid earth samples that will provide for the first time a way to

  16. Permeability Measurements of Rock Samples from Conduit Drilling at Unzen Volcano, Japan

    Science.gov (United States)

    Watanabe, T.; Shimizu, Y.; Noguchi, S.; Nakada, S.

    2006-12-01

    The last eruption of Unzen Volcano (1990-1995) was effusive to form lava domes, though magmas at depths are estimated to have contained volatile materials enough to cause explosive eruptions [e.g., Sato et al., 1995]. Most of volatile materials should have escaped from ascending magmas. The escape of gas is controlled by permeability of magmas and country rocks. Unzen Scientific Drilling Project sampled both the latest conduit and its country rock (USDP-4). In order to understand degassing processes, we have measured the permeability of these rock samples. Four cube samples with edges of 25 mm were cut from USDP-4 cores C1, C12 (country rock), C13 and C14 (conduit). Sample C1 is considered as Old Unzen Lava, and Sample C12 volcanic breccia. The transient pulse method was employed to measure the permeability. It applies a step of the fluid pressure difference across a specimen, and measures the decay rate of the fluid pressure difference. This method can be applied to samples with very low permeability, since it determines the permeability without measuring the fluid flux. Nitrogen gas was used as a pore fluid. Our permeametry system is built in a pressure vessel, and the confining pressure and the pore fluid pressure can be controlled independently. The temperature of the measurement system is kept constant within 0.1 degree. The temperature control and the background leak rate limit the measurable permeability to be higher than 10^{-20} m2. Measurements were first conducted under the atmospheric pressure. The permeability in a rock sample varies with the direction by a factor less than 5. Sample C1 has the lowest permeability (10^{-19} m2), and Sample C12 the highest value (10^{-17 m2). The permeability of C13 and C14 is of the order of 10^{- 18} m2. Though only a trace of vesicles can be seen in conduit samples, the interconnection is still maintained. The pressure dependence of the permeability is now investigated up to 50 MPa. The permeability of C13 and C14

  17. The electrical signature of rock samples exposed to hydrostatic and triaxial pressures

    Energy Technology Data Exchange (ETDEWEB)

    Heikamp, S.; Nover, G. [Bonn Univ., Bonn (Germany). Mineralogical Institute

    2001-04-01

    The electrical signature of sedimentary (carbonate) and crystalline rock samples was studied in hydrostatic and triaxial pressure experiments up to 300 MPa. The aim was to establish a relation between an electrical signal stimulated by an external pressure acting on the sample and the mechanical stability of the rock. Natural open fractures tend to be closed under hydrostatic pressure conditions, whereas in triaxial pressure experiments new fractures are generated. These contrary processes of either decrease or increase in crack density and geometry, cause a decrease or increase in the inner surface of the sample. Such pressure induced variations in pore geometry were investigated by an interpretation and modelling of the frequency dependence of the complex electrical conductivity. In a series of hydrostatic pressure experiments crack-closure was found in the electrical signature by decrease of the model capacitor C being related to crack geometry. This capacitor increases in the triaxial experiments where new fractures were formed.

  18. Mineralogy, petrology and whole-rock chemistry data compilation for selected samples of Yucca Mountain tuffs

    International Nuclear Information System (INIS)

    Connolly, J.R.

    1991-12-01

    Petrologic, bulk chemical, and mineralogic data are presented for 49 samples of tuffaceous rocks from core holes USW G-1 and UE-25a number-sign 1 at Yucca Mountain, Nevada. Included, in descending stratigraphic order, are 11 samples from the Topopah Spring Member of the Paintbrush Tuff, 12 samples from the Tuffaceous Beds of Calico Hills, 3 samples from the Prow Pass Member of the Crater Flat Tuff, 20 samples from the Bullfrog Member of the Crater Flat Tuff and 3 samples from the Tram Member of the Crater Flat Tuff. The suite of samples contains a wide variety of petrologic types, including zeolitized, glassy, and devitrified tuffs. Data vary considerably between groups of samples, and include thin section descriptions (some with modal analyses for which uncertainties are estimated), electron microprobe analyses of mineral phases and matrix, mineral identifications by X-ray diffraction, and major element analyses with uncertainty estimates

  19. Sorption of Cs, Eu and U(VI) onto rock samples from Nizhnekansky massive

    Energy Technology Data Exchange (ETDEWEB)

    Petrov, V.; Vlasova, I.; Kalmykov, S. [Lomonosov Moscow State University (Russian Federation); Kuzmenkova, N. [Vernadsky Institute of Geochemistry and Analytical Chemistry, Russian Academy of Science (Russian Federation); Petrov, V.; Poluektov, V. [Institute of Geology of Ore Deposits, Petrography, Mineralogy and Geochemistry, Russian Academy of Sciences - IGEM RAS (Russian Federation)

    2014-07-01

    The accepted in Russia concept for high level wastes (HLW) and spent nuclear fuel (SNF) disposal is based on their isolation into the deep underground crystalline rock formations. The 'Eniseysky' area (Nizhnekansky massive) is supposed as the most perspective location for the future HLW and SNF repository. Core materials from different areas of Nizhnekasnsky massive have been studied in terms of petrographic and mineralogical characterization; definition of filtration, elastic, petro-physical and strength properties; estimation of hydrothermal-metasomatic transformation of rocks. We used both undisturbed sliced cores and crushed material for the sorption experiments. Preliminary results of uranium sorption show some significant differences between used rock samples from different depth in sorption rate and pH-dependence. In all cases maximum sorption (more than 90%) is reached in 2-3 weeks. The pH-dependence of sorbed uranium fraction has typical hump-shape: increase of sorption percentage with increasing pH values to 6, plateau (90-98 % of uranium sorbed), decrease of sorption percentage with increasing pH values from 8 due to U(VI) hydrolysis. In the case of cesium the sorption maximum is reached within 10-12 days and in the case of europium - about 5 days. All radionuclides sorbed preferentially onto dark minerals. Local distribution and preferential sorption of cesium, europium and uranium (VI) onto different minerals within the sample were studied by radiography, SEM-EDX, etc. These data accompanying with rock sample composition will allow the development of quantitative model for Cs, Eu and U(VI) sorption onto investigated rocks. Document available in abstract form only. (authors)

  20. Atomic absorption determination of ultratrace tellurium in rocks utilizing high sensitivity sampling systems

    International Nuclear Information System (INIS)

    Beaty, R.D.

    1973-01-01

    The sampling boat and the graphite furnace were shown to possess the required sensitivity to detect tellurium at ultratrace levels, in a variety of sample types, by atomic absorption. In the sampling boat approach, tellurium in sample solutions is chemically separated and concentrated by extraction into methyl isobutyl ketone before measurement. For samples exhibiting extraction interferences or excessively high background absorption, a preliminary separation of tellurium by coprecipitation with selenium is described. Using this technique, tellurium can be quantitatively detected down to 5 nanograms and linear response is observed to 100 nanograms. Relative standard deviations of better than 7 percent are achieved for 50 nanograms of tellurium. For samples that have a tellurium content below the detection limits of the sampling boat, the graphite furnace is used for atomization. By this method, as little as 0.07 nanograms of tellurium can be detected, and a precision of 1 percent relative standard deviation is achievable at the 5 nanogram level. A routinely applicable procedure was developed for determining tellurium in rocks, using the graphite furnace, after a hydrofluoric acid decomposition of the sample. Using this procedure, tellurium data were obtained on 20 different rocks, and the significance of this new information is discussed. (Diss. Abstr. Int., B)

  1. Sampling and specimen preparation of rocks from the Asse mine, for sorption studies

    International Nuclear Information System (INIS)

    Bode, W.

    1986-01-01

    Within the framework of siting exploratory work in the Asse salt mine, five deep holes have been brought down, a series of hydrogeological wells (up to a depth of 300 m), and some gauge wells (up to 110 m). Most of the borings are core drills with a diameter of 100 mm. In addition to the usual experiments for rock property determination, samples for the determination of sorption properties have been taken. In order to reduce the effect of the O 2 in the air on the rocks during storage, the bore kernels have been put into O 2 -tight casks immediately after sampling and cleaning. Processing has been done by means of a jawbreaker, hammer milling, and a shaking device, all equipped with argon-conditioned boxes. The specimens have been shipped in Al-coated and Ar-conditioned polyethylene containers. (orig.) [de

  2. Analysis of Precious Stones Deposited in Various Rock Samples of Mogok Region by energy dispersive X-ray Fluorescence Spectrometry

    International Nuclear Information System (INIS)

    Kyi Kyi San; Soe Lwin; Win Win Thar; Sein Htoon

    2004-06-01

    The analysis of precious stones deposited in various rock samples of Mogok region were investigated by the energy dispersive x-ray fluorescence technique. The x-ray machine with Rh target was used to excite the characteristic x-ray from the sample. X-rays emitted from the sample were measured by a high resolution, cooled Si (Li) detector. The calibration was made by the measurement of minerals which composed in each kind of precious stones. The kind of precious stone deposited in the rocks sample was determined by the measurement of minerals from the rock samples compared with those obtained from each kind of precious stones

  3. Lunar and Meteorite Sample Education Disk Program - Space Rocks for Classrooms, Museums, Science Centers, and Libraries

    Science.gov (United States)

    Allen, Jaclyn; Luckey, M.; McInturff, B.; Huynh, P.; Tobola, K.; Loftin, L.

    2010-01-01

    NASA is eager for students and the public to experience lunar Apollo samples and meteorites first hand. Lunar rocks and soil, embedded in Lucite disks, are available for educators to use in their classrooms, museums, science centers, and public libraries for education activities and display. The sample education disks are valuable tools for engaging students in the exploration of the Solar System. Scientific research conducted on the Apollo rocks reveals the early history of our Earth-Moon system and meteorites reveal much of the history of the early solar system. The rocks help educators make the connections to this ancient history of our planet and solar system and the basic processes accretion, differentiation, impact and volcanism. With these samples, educators in museums, science centers, libraries, and classrooms can help students and the public understand the key questions pursued by many NASA planetary missions. The Office of the Curator at Johnson Space Center is in the process of reorganizing and renewing the Lunar and Meteorite Sample Education Disk Program to increase reach, security and accountability. The new program expands the reach of these exciting extraterrestrial rocks through increased access to training and educator borrowing. One of the expanded opportunities is that trained certified educators from science centers, museums, and libraries may now borrow the extraterrestrial rock samples. Previously the loan program was only open to classroom educators so the expansion will increase the public access to the samples and allow educators to make the critical connections to the exciting exploration missions taking place in our solar system. Each Lunar Disk contains three lunar rocks and three regolith soils embedded in Lucite. The anorthosite sample is a part of the magma ocean formed on the surface of Moon in the early melting period, the basalt is part of the extensive lunar mare lava flows, and the breccias sample is an important example of the

  4. Natural radioactivity measurements in rock samples of Cuihua Mountain National Geological Park (China))

    International Nuclear Information System (INIS)

    Lu, X.; Zhang, X.

    2008-01-01

    The concentrations of the natural radionuclides namely 40 K, 232 Th and 226 Ra in rock samples collected from Cuihua Mountain National Geological Park of China have been determined using a NaI(Tl) detector. The concentrations of 226 Ra, 232 Th and 40 K in the studied rock samples range from 10.7 to 34.8, 19.9 to 53.6 and 642.7 to 1609.9 Bq kg -1 with an average of 20.4, 30.1 and 1009.5 Bq kg -1 , respectively. The concentrations of these radionuclides are compared with the typical world values. To evaluate the radiological hazard of the natural radioactivity, the radium equivalent activity, the air absorbed dose rate, the annual effective dose rate, the representative level index and the values of both external and internal hazard indices were evaluated and compared with the internationally approved values. The radium equivalent activity values of all rock samples are lower than the limit of 370 Bq kg -1 . The values of H ex and H in are less than unity. The mean outdoor air absorbed dose rate is 69.7 nGy h -1 , and the corresponding outdoor effective dose rate is 0.086 mSv y -1 . (authors)

  5. Standard characterization of phosphate rock samples from the FAO/IAEA phosphate project

    International Nuclear Information System (INIS)

    Binh, Truong; Zapata, F.

    2002-01-01

    Phosphate rocks (PR) are phosphate-bearing minerals that vary widely in their inherent characteristics and consequently their agronomic potential. In the framework of a FAO/IAEA networked research project, the evaluation of the agronomic effectiveness of natural and modified PR products under a variety of soil climate and crop management conditions was carried out. The characterization of phosphate rocks is the first and essential step in evaluating their suitability for direct application. If several PR sources are utilized, standardized methods should be used for comparison purposes to determine their agronomic potential. This paper describes the standard characterization of phosphate rock products utilized in the project, in particular the mineralogical and crystallographic analyses, physical analyses, chemical composition and solubility in conventional reagents. A total of 28 phosphate rock samples from 15 countries were collected and analyzed in specialized laboratories. The data on mineralogy, chemical composition and solubility in conventional reagents are closely interrelated. An arbitrary classification of the reactivity of the PR samples was made based on the solubility indices in conventional reagents. On another hand, the results of the crystallographic parameters, calculated indices of absolute solubility, specific surface and porosity reflect the variability of the physical state and the sample pre-conditioning treatment of the analyzed products. A proper characterization of phosphate rock samples should provide the maximum of basic information that can be obtained in a cost-effective manner in normal chemical laboratories. Based on the results of this characterization, the following determinations are recommended: a description of the sample, major elemental (total P, Ca, Mg) composition, solubility in conventional reagents (neutral ammonium citrate, citric and formic acid) and particle size analysis. The classification of PR samples for direct

  6. Permeability and compression characteristics of municipal solid waste samples

    Science.gov (United States)

    Durmusoglu, Ertan; Sanchez, Itza M.; Corapcioglu, M. Yavuz

    2006-08-01

    Four series of laboratory tests were conducted to evaluate the permeability and compression characteristics of municipal solid waste (MSW) samples. While the two series of tests were conducted using a conventional small-scale consolidometer, the two others were conducted in a large-scale consolidometer specially constructed for this study. In each consolidometer, the MSW samples were tested at two different moisture contents, i.e., original moisture content and field capacity. A scale effect between the two consolidometers with different sizes was investigated. The tests were carried out on samples reconsolidated to pressures of 123, 246, and 369 kPa. Time settlement data gathered from each load increment were employed to plot strain versus log-time graphs. The data acquired from the compression tests were used to back calculate primary and secondary compression indices. The consolidometers were later adapted for permeability experiments. The values of indices and the coefficient of compressibility for the MSW samples tested were within a relatively narrow range despite the size of the consolidometer and the different moisture contents of the specimens tested. The values of the coefficient of permeability were within a band of two orders of magnitude (10-6-10-4 m/s). The data presented in this paper agreed very well with the data reported by previous researchers. It was concluded that the scale effect in the compression behavior was significant. However, there was usually no linear relationship between the results obtained in the tests.

  7. Investigation of trace uranium content in rock phosphate ore samples from Kurun-Uro area, Nuba Mountains, Sudan

    International Nuclear Information System (INIS)

    Ali, Abdel Majid Abdel Galil Mohammed

    1999-07-01

    This investigation was carried out mainly to test the trace uranium level content in rock phosphate, which was used as a low cost fertilizer. Two types of rock phosphate were examined, namely, Kurun and Uro rocks from Nuba Mountains in the Southern Kurdufan province, Sudan.This area has a high background natural radioactivity. Moreover, it contains a rock phosphate zone lying between J. Kurun and Uro. The work included analytical methods carried out for thr rock phosphate samples using spectrophotometric and X-ray fluorescence techniques. The results obtained were compared with the data from literature and they showed a good agreement.The data was statistically analyzed to compare the results by the two techniques. The results of uranium content determined by the two analytical methods were significantly similar.The instrumental analysis revealed that different. Uranium content in the rocks phosphate samples of Uro type was found to be 1.6 times higher than Kurun type. (Author)

  8. The results of experimental studies of VLF-ULF electromagnetic emission by rock samples due to mechanical action

    Science.gov (United States)

    Panfilov, A. A.

    2014-06-01

    The paper presents the results of laboratory experiments on electromagnetic emissions excitation (the electric component of electromagnetic fields) by rock samples due to different forms of mechanical stress applications. It was shown that samples generate electric impulses with different spectra when the impact action, gradual loading or dynamic friction is applied. It was ascertained that level and spectral compositions of signals, generated by rock samples, change with an increasing number of hits. It was found that strong electromagnetic signals, generated while rock samples were fracturing, were accompanied by repetitive weak but perceptible variations in the electric field intensity in short frequency ranges.

  9. OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

    Directory of Open Access Journals (Sweden)

    Maja Vrkljan

    2004-12-01

    Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

  10. Neutron emission from impacted solid LiD samples

    International Nuclear Information System (INIS)

    Kaushik, T.C.; Shyam, A.; Kulkarni, L.V.; Srinivasan, M.

    1993-01-01

    Nylon projectiles with 0.1 g to 0.3 g mass, accelerated to velocities of 0.2-1 km/s using a 60 cm long electromagnetic accelerator (railgun), have been impacted upon solid lithium deuteride (LiD) samples of 3 proportional counters. The output from the BF 3 set-up is monitored in several ways to characterize the possible neutron emission from the target. This includes a simple technique of counting the single channel analyser (SCA) output through a dead-time unit to identify bursts of < 100 μs duration. Counting is started after a delay of ∼ 1 ms to avoid the initial interference from the capacitor bank discharge. The signal is also recorded in a storage oscilloscope from the start of projectile acceleration along with a time marker just before the impact. From a number of shots taken with and without the samples, a significant evidence of neutron emission from the LiD samples appears to emerge. The experiments suggest that approximately 100 neutrons might be generated during every such impact in a duration of < 4 ms. (author). 7 refs., 3 figs

  11. Gastric emptying of solids: When should we sample

    International Nuclear Information System (INIS)

    Sfakianakis, G.; Spoliansky, G.; Cassady, J.; Barkin, J.; Serafini, A.

    1984-01-01

    Gastric emptying of solids has been studied for 20 normal volunteers using Tc-99m-sulfur-colloid labeled chicken liver or eggs. Residual gastric activity measured in 15 min intervals for 2 1/2 hrs was used to calculate gastric emptying. The procedure was proposed and is used to examine patients for suspected abnormal emptying. This approach however ties up one gamma camera and one technologist for a period of 2 1/2 - 3 hrs. Furthermore to classify any value more the 1SD below the mean as abnormal includes 16% of normals as abnormally low (false positives). In order to find the pattern of abnormalities and the best time to study patients we analyzed the results of 54 studies performed in patients with a variety of clinical problems. Gastric emptying was measured in 30 min intervals for 2 1/2 hrs after a standard meal of 2 scrambled eggs labeled with 1 mCi of Tc-99m-sulfur-colloid, 2 slices of bread and 300 ml of juice. To choose the point important to observe the authors studied the distribution of values at each time-point to determine when there is the greatest variability from the reported normal. When there is delayed emptying the 2 1/2 hr observation is the best discriminator and when there is accelerated emptying the 60 min observation is the best discriminator. In the group of patients the 150 min observation had no correlation with the age of the patients. It is possible that sampling at a later time could be more discriminatory. The authors propose sampling at 0, 60, and 150 min time as the most informative and cost effective approach to study the solid gastric emptying. The 2SD rather than 1SD below and above the mean should be used as the level to separate normal from abnormal results

  12. Gastric emptying of solids: When should we sample

    Energy Technology Data Exchange (ETDEWEB)

    Sfakianakis, G.; Spoliansky, G.; Cassady, J.; Barkin, J.; Serafini, A.

    1984-01-01

    Gastric emptying of solids has been studied for 20 normal volunteers using Tc-99m-sulfur-colloid labeled chicken liver or eggs. Residual gastric activity measured in 15 min intervals for 2 1/2 hrs was used to calculate gastric emptying. The procedure was proposed and is used to examine patients for suspected abnormal emptying. This approach however ties up one gamma camera and one technologist for a period of 2 1/2 - 3 hrs. Furthermore to classify any value more the 1SD below the mean as abnormal includes 16% of normals as abnormally low (false positives). In order to find the pattern of abnormalities and the best time to study patients we analyzed the results of 54 studies performed in patients with a variety of clinical problems. Gastric emptying was measured in 30 min intervals for 2 1/2 hrs after a standard meal of 2 scrambled eggs labeled with 1 mCi of Tc-99m-sulfur-colloid, 2 slices of bread and 300 ml of juice. To choose the point important to observe the authors studied the distribution of values at each time-point to determine when there is the greatest variability from the reported normal. When there is delayed emptying the 2 1/2 hr observation is the best discriminator and when there is accelerated emptying the 60 min observation is the best discriminator. In the group of patients the 150 min observation had no correlation with the age of the patients. It is possible that sampling at a later time could be more discriminatory. The authors propose sampling at 0, 60, and 150 min time as the most informative and cost effective approach to study the solid gastric emptying. The 2SD rather than 1SD below and above the mean should be used as the level to separate normal from abnormal results.

  13. Direct determination of uranium in soil, rock, ore and biological samples by laser-induced fluorometry

    International Nuclear Information System (INIS)

    Li Qingzhen; Zhang Yanan

    1993-03-01

    A laser-induced fluorometric method with modified J-22 anti-interferent fluorescent reagent for directly determining the uranium in soil, rock, ore, geochemical, biological and other samples has been studied. The effects of external ions and dilution law of sample are examined in detail. A method for correcting inner effect is proposed. A mixed solution of 0.25% NaOH-10% J-22 is prepared which can be added to the sample cuvette for direct measurement without any pre-adjustment of acidity. Therefore, it is much simpler for operation and reduces the loss and contamination of uranium. By changing the laser fluorometer sensitivity (400 ∼ 200), up to 3000 ng uranium in the cuvette can be detected. Thus, both analytical accuracy and detectable range are improved. This method is simple, rapid, accurate and applicable to various uranium-bearing samples. The detection limit is better than 0.05 μgU/g. The relative standard deviation is ≤+-5% for the rock reference samples of 0.95, 84.8, 669 and 7240 μgU/g

  14. The results of experimental studies of VLF–ULF electromagnetic emission by rock samples due to mechanical action

    OpenAIRE

    A. A. Panfilov

    2013-01-01

    The paper presents the results of laboratory experiments on electromagnetic emission excitation (electric component of electromagnetic field) by rock samples due to different forms of mechanical stress applications. It was shown that samples generate electric impulses with different spectra when the impact action, gradual loading or dynamic friction is applied. It was ascertained that level and spectral compositions of signals, generated by rock samples, cha...

  15. Physical properties and petrologic description of rock samples from an IOCG mineralized area in the northern Fennoscandian Shield, Sweden

    DEFF Research Database (Denmark)

    Sandrin, Alessandro; Edfelt, Å.; Waight, Tod Earle

    2009-01-01

    The Tjårrojåkka Fe-Cu prospect in northern Sweden is considered an example of a Fe-oxide Cu-Au (IOCG) deposit and is hosted in metamorphosed Paleoproterozoic volcanic and intrusive rocks. Rock samples from 24 outcrops were collected for petrophysical analysis (magnetic susceptibility, remanent ma...

  16. Liquid-solid extraction of uranium (VI) with TOPO - molten naphthalene and determination by laser fluorimetry in geological samples

    International Nuclear Information System (INIS)

    Kumar, Sanjay; Krishnakumar, M.; Patwardhan, A.A.

    2007-01-01

    A simple, rapid, sensitive, cost-effective and efficient method for separation of uranium using tri-n-octylphosphine oxide (TOPO)-molten naphthalene as solid phase extractant and its determination by laser fluorimetry in geological samples (rock, soil, sediment) was developed. Under optimum conditions, using 50 mg TOPO and 100 mg naphthalene, 50 - 5000 ng of uranium in 10 ml sample solution (3% (v/v) HNO 3 ) could be extracted quantitatively. The extracted uranium was stripped using tetra sodium pyrophosphate (5% (v/v) solution, pH adjusted to 7.0 with H 3 PO 4 ) and determined by laser fluorimetry. The influence of different acid concentrations, the amount of solid phase extractant, sample volumes, different stripping reagents, their volumes and effect of foreign ions on the extraction and determination of uranium (VI) were investigated. Synthetic samples of varying concentration as regards uranium were prepared and analysed. Recoveries ranging from 90% to 105% were obtained. The method was validated by analyzing four certified reference materials namely, BL-5, DH-1a, SY-2, SY-3 and the values obtained for uranium agreed well with the certified values. The method was also applied to the determination of uranium in geological samples (rock, soil and sediment) by laser fluorimetry and the results obtained compared favorably with those obtained from the pellet fluorimetry method. Following the proposed method, determination limit for uranium was found to be 1 μg/g with RSD ± 10%. (author)

  17. Rare earths analysis of rock samples by instrumental neutron activation analysis, internal standard method

    International Nuclear Information System (INIS)

    Silachyov, I.

    2016-01-01

    The application of instrumental neutron activation analysis for the determination of long-lived rare earth elements (REE) in rock samples is considered in this work. Two different methods are statistically compared: the well established external standard method carried out using standard reference materials, and the internal standard method (ISM), using Fe, determined through X-ray fluorescence analysis, as an element-comparator. The ISM proved to be the more precise method for a wide range of REE contents and can be recommended for routine practice. (author)

  18. Determination of uranium, thorium and potassium contents of rock samples in Yemen

    International Nuclear Information System (INIS)

    Abdulrahman Abdul-Hadi; Wedad Al-Qadhi; Enayat El-Zeen

    2011-01-01

    Uranium, thorium and potassium contents in 16 different rock samples from various sites in Republic of Yemen were determined using three different techniques of analysis: γ-spectrometry, Instrumental neutron activation analyses (INAA) and X-ray fluorescence (XRF). The concentration range for thorium, uranium and potassium were found to be from 9,810 ± 272 to 3.6 ± 1.3 ppm, 1,072 ± 40 to 1.2 ± 0.7 ppm and 11 ± 1 to 0.26 ± 0.05%, respectively. (author)

  19. Geothermal heat from solid rock - increased energy extraction through hydraulic pressurizing of drill wells

    International Nuclear Information System (INIS)

    Ramstad, Randi Kalskin; Hilmo, Bernt Olav; Skarphagen, Helge

    2005-01-01

    New equipment for hydraulic pressurizing, a double collar of the type FrakPak - AIP 410-550, is developed by the Broennteknologi AS. The equipment is tested in the laboratory and in the field at Lade in Trondheim. By the construction of two pilot plants for geothermal heat at Bryn and on the previous grounds of the energy company in Asker and Baerum (EAB) extensive studies connected to hydraulic pressurizing are carried out both with water and sand injection. The geothermal heat plants at Bryn and AEB were supposed to be based on pumped ground water from rock wells where increased effect was obtained through pumping up, returning and circulating the water. The aim of the study was to test and develop the methods for hydraulic pressurizing both with water and sand injection, document the effect of the various types of pressurizing as well as mapping the hydro- and rock geological conditions for this type of geothermal heat plants. In addition to stimulating 10 drill holes with hydraulic pressurizing with water and sand injection, the studies have carried out test pumping, water sampling, geophysical logging, measurements of alterations in the terrain, current and rock strain measurements and geothermal response tests. Furthermore an efficacy test and a theoretical model of the energy potential of the plants are carried out. The results from the pilot plant at Bryn show that the drill hole capacities are significantly increased both through hydraulic pressurizing with water and sand injection. There seems to be a greater need for sand as ''prepping agent'' or distance maker in cracks with high pressure resistance than in cracks with lower resistance. The grain size of the sand should be adapted to the resistance pressure and injection of coarser sand is recommended in cracks with lower resistance pressure. The rock strength and strain conditions determine the successes of hydraulic pressurizing at the reopening of existing or opening of new faults. Test pumping was

  20. Environmental impacts of waste produced from processing of different uraniferous rock samples

    Directory of Open Access Journals (Sweden)

    Ibrahim E. El Aassy

    2016-07-01

    Full Text Available Radon exhalation rates from five studied laboratory waste samples resulted from five different sedimentary rock types named sandy dolostone, siltstone –two samples-, marly claystone and black shale were measured using ‘‘Sealed Can technique”. These rates were found to vary between 0.005 and 0.015 Bq m−2 h−1. A positive correlation was found between the radon exhalation rates and the radium activities. The emanation coefficients were calculated for these laboratory waste samples which varied between 0.0004 and 0.0007 according to the physical and chemical characterize of the wastes. These results are partially in accordance with autonite acid leached tailings on laboratory scale (USA. These results led us to pay attention about the effect and impact of these wastes on the environment.

  1. Multielement determination of rare earth elements in rock sample by liquid chromatography / inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Hamanaka, Tadashi; Itoh, Akihide; Itoh, Shinya; Sawatari, Hideyuki; Haraguchi, Hiroki.

    1995-01-01

    Rare earth elements in geological standard rock sample JG-1 (granodiolite)issued from the Geological Survey of Japan have been determined by a combined system of liquid chromatography and inductively coupled plasma mass spectrometry. (author)

  2. The research of breaking rock with liquid-solid two-phase jet flow

    Science.gov (United States)

    Cheng, X. Z.; Ren, F. S.; Fang, T. C.

    2018-03-01

    Abstracts. Particle impact drilling is an efficient way of breaking rock, which is mainly used in deep drilling and ultra-deep drilling. The differential equation was established based on the theory of Hertz and Newton’s second law, through the analysis of particle impact rock, the depth of particles into the rock was obtained. The mathematical model was established based on the effect of water impact crack. The research results show when water jet speed is more than 40 m/s, rock stability coefficient is more than 1.0, the rock fracture appear. Through the experimental research of particle impact drilling facilities, analysis of cuttings and the crack size which was analyzed through Scanning electron microscope consistent with the theoretical calculation, the validity of the model was verified.

  3. An approach for sampling solid heterogeneous waste at the Hanford Site waste receiving and processing and solid waste projects

    International Nuclear Information System (INIS)

    Sexton, R.A.

    1993-03-01

    This paper addresses the problem of obtaining meaningful data from samples of solid heterogeneous waste while maintaining sample rates as low as practical. The Waste Receiving and Processing Facility, Module 1, at the Hanford Site in south-central Washington State will process mostly heterogeneous solid wastes. The presence of hazardous materials is documented for some packages and unknown for others. Waste characterization is needed to segregate the waste, meet waste acceptance and shipping requirements, and meet facility permitting requirements. Sampling and analysis are expensive, and no amount of sampling will produce absolute certainty of waste contents. A sampling strategy is proposed that provides acceptable confidence with achievable sampling rates

  4. Geochemical porosity values obtained in core samples from different clay-rocks

    International Nuclear Information System (INIS)

    Fernandez, A.M.

    2010-01-01

    Document available in extended abstract form only. Argillaceous formations of low permeability are considered in many countries as potential host rocks for the disposal of high level radioactive wastes (HLRW). In order to determine their suitability for waste disposal, evaluations of the hydro-geochemistry and transport mechanisms from such geologic formations to the biosphere must be undertaken. One of the key questions about radionuclide diffusion and retention is to know the chemistry and chemical reactions and sorption processes that will occur in the rock and their effects on radionuclide mobility. In this context, the knowledge of the pore water chemistry is essential for performance assessment purposes. This information allows to establish a reliable model for the main water-rock interactions, which control the physico-chemical parameters and the chemistry of the major elements of the system. An important issue in order to model the pore water chemistry in clayey media is to determine the respective volume accessible to cations and anions, i.e, the amount of water actually available for chemical reactions/solute transport. This amount is usually referred as accessible porosity or geochemical porosity. By using the anion inventories, i.e. the anion content obtained from aqueous leaching, and assuming that all Cl - , Br - and SO4 2- leached in the aqueous extracts originates from pore water, the concentration of a conservative ion can be converted into the real pore water concentration if the accessible porosity is known. In this work, the accessible porosity or geochemical porosity has been determined in core samples belonging to four different formations: Boom Clay from Hades URL (Belgium, BE), Opalinus Clay from Mont Terri (Switzerland, CH), and Callovo-Oxfordian argillite from Bure URL (France, FR). The geochemical or chloride porosity was defined as the ratio between the pore water volume containing Cl-bearing pore water and the total volume of a sample

  5. Irradiation and accretion of solids in space based on observations of lunar rocks and grains

    International Nuclear Information System (INIS)

    Lal, D.

    1977-01-01

    Clues to a wide range of questions relating to the origin and evolution of the solar system and dynamic physical and electromagnetic processes occurring concurrently and in the past in our galaxy have been provided by a study of the lunar samples. This information is deduced from a variety of complementary physical and chemical evidence. In this presentation greatest emphasis is laid on information based on effects arising from interactions of low energy cosmic rays with lunar surface materials. The present discussions concern the nature of experimental data to date and implications thereof to the charged particle environment of the Moon, ancient magnetic fields and the nature of time scales involved in the irradiation and accretion of solids in space, based on lunar regolith dynamics. It becomes clear that there does not yet exist any consensus on the absolute values of charged particle or the meteorite fluxes, and also about the details of the evolution of the lunar regolith. The complex history of evolution of lunar material is slowly being understood and it is hoped that a great deal of quantitative information will soon be available which will in turn allow discussion of evolution of solid bodies in the solar system. (author)

  6. Long-wave equivalent viscoelastic solids for porous rocks saturated by two-phase fluids

    Science.gov (United States)

    Santos, J. E.; Savioli, G. B.

    2018-04-01

    Seismic waves traveling across fluid-saturated poroelastic materials with mesoscopic-scale heterogeneities induce fluid flow and Biot's slow waves generating energy loss and velocity dispersion. Using Biot's equations of motion to model these type of heterogeneities would require extremely fine meshes. We propose a numerical upscaling procedure to determine the complex and frequency dependent P-wave and shear moduli of an effective viscoelastic medium long-wave equivalent to a poroelastic solid saturated by a two-phase fluid. The two-phase fluid is defined in terms of capillary pressure and relative permeability flow functions. The P-wave and shear effective moduli are determined using harmonic compressibility and shear experiments applied on representative samples of the bulk material. Each experiment is associated with a boundary value problem that is solved using the finite element method. Since a poroelastic solid saturated by a two-phase fluid supports the existence of two slow waves, this upscaling procedure allows to analyze their effect on the mesoscopic-loss mechanism in hydrocarbon reservoir formations. Numerical results show that a two-phase Biot medium model predicts higher attenuation than classic Biot models.

  7. Central Colorado Assessment Project (CCAP)-Geochemical data for rock, sediment, soil, and concentrate sample media

    Science.gov (United States)

    Granitto, Matthew; DeWitt, Ed H.; Klein, Terry L.

    2010-01-01

    This database was initiated, designed, and populated to collect and integrate geochemical data from central Colorado in order to facilitate geologic mapping, petrologic studies, mineral resource assessment, definition of geochemical baseline values and statistics, environmental impact assessment, and medical geology. The Microsoft Access database serves as a geochemical data warehouse in support of the Central Colorado Assessment Project (CCAP) and contains data tables describing historical and new quantitative and qualitative geochemical analyses determined by 70 analytical laboratory and field methods for 47,478 rock, sediment, soil, and heavy-mineral concentrate samples. Most samples were collected by U.S. Geological Survey (USGS) personnel and analyzed either in the analytical laboratories of the USGS or by contract with commercial analytical laboratories. These data represent analyses of samples collected as part of various USGS programs and projects. In addition, geochemical data from 7,470 sediment and soil samples collected and analyzed under the Atomic Energy Commission National Uranium Resource Evaluation (NURE) Hydrogeochemical and Stream Sediment Reconnaissance (HSSR) program (henceforth called NURE) have been included in this database. In addition to data from 2,377 samples collected and analyzed under CCAP, this dataset includes archived geochemical data originally entered into the in-house Rock Analysis Storage System (RASS) database (used by the USGS from the mid-1960s through the late 1980s) and the in-house PLUTO database (used by the USGS from the mid-1970s through the mid-1990s). All of these data are maintained in the Oracle-based National Geochemical Database (NGDB). Retrievals from the NGDB and from the NURE database were used to generate most of this dataset. In addition, USGS data that have been excluded previously from the NGDB because the data predate earliest USGS geochemical databases, or were once excluded for programmatic reasons

  8. Super resolution reconstruction of μ-CT image of rock sample using neighbour embedding algorithm

    Science.gov (United States)

    Wang, Yuzhu; Rahman, Sheik S.; Arns, Christoph H.

    2018-03-01

    X-ray computed tomography (μ-CT) is considered to be the most effective way to obtain the inner structure of rock sample without destructions. However, its limited resolution hampers its ability to probe sub-micro structures which is critical for flow transportation of rock sample. In this study, we propose an innovative methodology to improve the resolution of μ-CT image using neighbour embedding algorithm where low frequency information is provided by μ-CT image itself while high frequency information is supplemented by high resolution scanning electron microscopy (SEM) image. In order to obtain prior for reconstruction, a large number of image patch pairs contain high- and low- image patches are extracted from the Gaussian image pyramid generated by SEM image. These image patch pairs contain abundant information about tomographic evolution of local porous structures under different resolution spaces. Relying on the assumption of self-similarity of porous structure, this prior information can be used to supervise the reconstruction of high resolution μ-CT image effectively. The experimental results show that the proposed method is able to achieve the state-of-the-art performance.

  9. 238U And 232Th Concentration In Rock Samples using Alpha Autoradiography and Gamma Spectroscopy Techniques

    International Nuclear Information System (INIS)

    Hafez, A.F.; El-Farrash, A.H.; Yousef, H.A.

    2009-01-01

    The activity concentrations of uranium and thorium were measured for some rock samples selected from Dahab region in the south tip of Sinai. In order to detect any harmful radiation that would affect on the tourists and is becoming economic resource because Dahab have open fields of tourism in Egypt. The activity concentration of uranium and thorium in rocks samples was measured using two techniques. The first is .-autoradiography technique with LR-115 and CR-39 detectors and the second is gamma spectroscopic technique with NaI(Tl) detector. It was found that the average activity concentrations of uranium and thorium using .-autoradiography technique ranged from 6.41-49.31 Bqkg-1, 4.86- 40.87 Bqkg-1 respectively and by gamma detector are ranged from 6.70- 49.50 Bqkg-1, 4.47- 42.33 Bqkg-1 respectively. From the obtained data we can conclude that there is no radioactive healthy hazard for human and living beings in the area under investigation. It was found that there are no big differences between the calculated thorium to uranium ratios in both techniques

  10. Effect of simulated sampling disturbance on creep behaviour of rock salt

    Science.gov (United States)

    Guessous, Z.; Gill, D. E.; Ladanyi, B.

    1987-10-01

    This article presents the results of an experimental study of creep behaviour of a rock salt under uniaxial compression as a function of prestrain, simulating sampling disturbance. The prestrain was produced by radial compressive loading of the specimens prior to creep testing. The tests were conducted on an artifical salt to avoid excessive scattering of the results. The results obtained from several series of single-stage creep tests show that, at short-term, the creep response of salt is strongly affected by the preloading history of samples. The nature of this effect depends upon the intensity of radial compressive preloading, and its magnitude is a function of the creep stress level. The effect, however, decreases with increasing plastic deformation, indicating that large creep strains may eventually lead to a complete loss of preloading memory.

  11. Isotope identification of Saudi Arabian rock samples from Umm Al-Birak using neutron activation analysis

    International Nuclear Information System (INIS)

    Kahtani, S.A.

    1984-12-01

    Forty eight geological samples from Umm Al-Birak area in the northwest part of Saudi Arabia are analyzed qualitatively and quantitatively using the instrumental neutron activation analysis technique. Samples are properly prepared and irridiated in the reactor facilities of the National Tsing-Hue University in Taiwan. Gamma spectra from high resolution detector are analyzed using BRUTAL code. Final calculations are made by two independent programs, namely, ELCAL and SMPCL. Twenty trace elements are identified and their concentrations are used in the investigation of the geochemistry of the Umm Al-Birak microgranite site. These elements are: Co, Cr, Eu, Fe, Hf, K, La, Lu, Na, Rb, Sc, Sm, Ta, Tb, Th, U, Yb, Zn and Zr. It is shown that high grade area is a differentiated rock that crystallized in a late stage of Umm Al-Birak microgranite area. 43 Ref

  12. Electron microprobe analyses of selected samples from deep rock disposal experiment No. 1

    International Nuclear Information System (INIS)

    Hlava, P.F.; Chambers, W.F.

    1976-04-01

    Deep Rock Disposal Experiment No. 1 was designed to provide information about the interaction between a molten, glass-based, nuclear waste simulant and rock material. Selected samples from this experiment were examined by optical microscopy and electron probe microanalysis. Analysis of the homogenized material in the convection cell that was created in the central portion of the melt region shows that an amount of rock equal to about one-half of the original amount of waste simulant was incorporated in the melt during the experiment. Stagnant melt at the sides of the cell formed a glass with large compositional gradients. A white band separated the convected and stagnant materials. The color of the band is attributed to light scattering by small crystallites formed during cooling. Four types of crystallites grew from the melt: two oxides, a Mg--Fe borate, and a silicate. Spinel (MgO, Cr 2 O 3 , FeO (Fe 2 O 3 ), and NiO) was the most common crystallite in the glass. The spinel crystallites found within the convection cell displayed skeletal morphology and oscillatory zoning which indicates growth at varying temperatures as they were carried along by convection. A single cluster of nonskeletal (Fe,Cr) 2 O 3 crystallites was found at the bottom of the melt zone where convection did not occur. Mg--Fe borate crystallites grew in clusters in the central portion of the convection cell after convection ceased. A silicate similar to Fe-rich diopside (CaMgSi 2 O 6 ) with unusual amounts of Ce 2 O 3 and other heavy metal oxides formed as larger crystallites in the stagnant melt at the side of the convection cell and as many very small crystallites in the white band

  13. Why Is There an Abrupt Transition from Solid Rock to Low Crystallinity Magma in Drilled Magma Bodies?

    Science.gov (United States)

    Eichelberger, J. C.; Carrigan, C. R.; Sun, Y.; Lavallée, Y.

    2017-12-01

    We report on a preliminary evaluation, from basic principles of heat and mass transfer, on the unexpectedly abrupt transition from cuttings of solid rock to fragments of crystal poor glass during drilling into magma bodies. Our analysis is based on conditions determined and inferred for the 2009 IDDP-1 well in Krafla Caldera, which entered apparently liquidus rhyolite magma at about 900oC at a depth of 2104 m. Simple conduction would predict some 30 m of crystallization and partial crystallization since the latest time the magma could have been intruded, approximately 30 years prior to discovery by drilling. Option 1: The expected crystallization of magma has occurred but interstitial melt remains. The pressure difference between lithostatic load of about 50 MPa on the mush and 20 MPa hydrostatic pressure in the well causes pore melt to flow from the permeable mush into the borehole, where it becomes the source of the quenched melt chips. To be viable, this mechanism must work over the time frame of a day. Option 2: The expected crystallization is occurring, but high Rayleigh number thermal convection in the magma chamber continuously displaces crystallizing roof magma by liquidus magma from the interior of the body. To be viable, this mechanism must result in overturning magma in the chamber on a time scale that is much shorter than that of crystallization. Option 3: Flow-induced crystal migration away from zones of high shear created during drilling into magma may preferentially produce low-crystal-content melt at the boundary of the borehole, which is then sampled.

  14. Supplement to the UMTRA project water sampling and analysis plan, Slick Rock, Colorado

    International Nuclear Information System (INIS)

    1995-09-01

    The water sampling and analysis plan (WSAP) provides the regulatory and technical basis for ground water and surface water sampling at the Uranium Mill Tailings Remedial Action (UMTRA) Project Union Carbide (UC) and North Continent (NC) processing sites and the Burro Canyon disposal site near Slick Rock, Colorado. The initial WSAP was finalized in August 1994 and will be completely revised in accordance with the WSAP guidance document (DOE, 1995) in late 1996. This version supplements the initial WSAP, reflects only minor changes in sampling that occurred in 1995, covers sampling scheduled for early 1996, and provides a preliminary projection of the next 5 years of sampling and monitoring activities. Once surface remedial action is completed at the former processing sites, additional and more detailed hydrogeologic characterization may be needed to develop the Ground Water Program conceptual ground water model and proposed compliance strategy. In addition, background ground water quality needs to be clearly defined to ensure that the baseline risk assessment accurately estimated risks from the contaminants of potential concern in contaminated ground water at the UC and NC sites

  15. Small population size of Pribilof Rock Sandpipers confirmed through distance-sampling surveys in Alaska

    Science.gov (United States)

    Ruthrauff, Daniel R.; Tibbitts, T. Lee; Gill, Robert E.; Dementyev, Maksim N.; Handel, Colleen M.

    2012-01-01

    The Rock Sandpiper (Calidris ptilocnemis) is endemic to the Bering Sea region and unique among shorebirds in the North Pacific for wintering at high latitudes. The nominate subspecies, the Pribilof Rock Sandpiper (C. p. ptilocnemis), breeds on four isolated islands in the Bering Sea and appears to spend the winter primarily in Cook Inlet, Alaska. We used a stratified systematic sampling design and line-transect method to survey the entire breeding range of this population during springs 2001-2003. Densities were up to four times higher on the uninhabited and more northerly St. Matthew and Hall islands than on St. Paul and St. George islands, which both have small human settlements and introduced reindeer herds. Differences in density, however, appeared to be more related to differences in vegetation than to anthropogenic factors, raising some concern for prospective effects of climate change. We estimated the total population at 19 832 birds (95% CI 17 853–21 930), ranking it among the smallest of North American shorebird populations. To determine the vulnerability of C. p. ptilocnemis to anthropogenic and stochastic environmental threats, future studies should focus on determining the amount of gene flow among island subpopulations, the full extent of the subspecies' winter range, and the current trajectory of this small population.

  16. The Effect of Fluid and Solid Properties on the Auxetic Behavior of Porous Materials Having Rock-like Microstructures

    Science.gov (United States)

    Wollner, U.; Vanorio, T.; Kiss, A. M.

    2017-12-01

    Materials with a negative Poisson's Ratio (PR), known as auxetics, exhibit the counterintuitive behavior of becoming wider when uniaxially stretched and thinner when compressed. Though negative PR is characteristic of polymer foams or cellular solids, tight as well as highly porous rocks have also been reported to exhibit a negative Poisson's ratio, both from dynamic (PRd) and static measurements. We propose a novel auxetic structure based on pore-space configuration observed in rocks. First, we performed 2D and 3D imaging of a pumice and tight basalt to analyze their rock microstructure as well as similarities to natural structures of auxetic materials - e.g., cork. Based on these analyses, we developed a theoretical auxetic 3D model consisting of rotating rigid bodies having pore configurations similar to those observed in rocks. To alleviate the mechanical assumption of rotating bodies, the theoretical model was modified to include crack-like features being represented by intersecting, elliptic cylinders. We then used a 3D printer to create a physical version of the modified model, whose PRd was tested. We also numerically explored how the compressibility of fluids located in the pore-space of the modified model as well as how the elastic properties of the material from which the model is made of affect its auxetic behavior. We conclude that for a porous medium composed of a single material saturated with a single fluid (a) the more compliant the fluid is and (b) the lower the PR of the solid material, the lower the PR value of the composite material.

  17. Alaska Geochemical Database (AGDB)-Geochemical data for rock, sediment, soil, mineral, and concentrate sample media

    Science.gov (United States)

    Granitto, Matthew; Bailey, Elizabeth A.; Schmidt, Jeanine M.; Shew, Nora B.; Gamble, Bruce M.; Labay, Keith A.

    2011-01-01

    The Alaska Geochemical Database (AGDB) was created and designed to compile and integrate geochemical data from Alaska in order to facilitate geologic mapping, petrologic studies, mineral resource assessments, definition of geochemical baseline values and statistics, environmental impact assessments, and studies in medical geology. This Microsoft Access database serves as a data archive in support of present and future Alaskan geologic and geochemical projects, and contains data tables describing historical and new quantitative and qualitative geochemical analyses. The analytical results were determined by 85 laboratory and field analytical methods on 264,095 rock, sediment, soil, mineral and heavy-mineral concentrate samples. Most samples were collected by U.S. Geological Survey (USGS) personnel and analyzed in USGS laboratories or, under contracts, in commercial analytical laboratories. These data represent analyses of samples collected as part of various USGS programs and projects from 1962 to 2009. In addition, mineralogical data from 18,138 nonmagnetic heavy mineral concentrate samples are included in this database. The AGDB includes historical geochemical data originally archived in the USGS Rock Analysis Storage System (RASS) database, used from the mid-1960s through the late 1980s and the USGS PLUTO database used from the mid-1970s through the mid-1990s. All of these data are currently maintained in the Oracle-based National Geochemical Database (NGDB). Retrievals from the NGDB were used to generate most of the AGDB data set. These data were checked for accuracy regarding sample location, sample media type, and analytical methods used. This arduous process of reviewing, verifying and, where necessary, editing all USGS geochemical data resulted in a significantly improved Alaska geochemical dataset. USGS data that were not previously in the NGDB because the data predate the earliest USGS geochemical databases, or were once excluded for programmatic reasons

  18. Radioactivity And Dose Assessment Of Rock And Soil Samples From Homa Mountain, Homa Bay County, Kenya

    International Nuclear Information System (INIS)

    Otwoma, D.; Patel, J.P.; Bartilol, S.; Mustapha, A.O.

    2013-01-01

    The in situ measured average outdoor absorbed dose rate in air was found to vary from 108.4 to 1596.4 n Gy h -1 at Homa Mountain area in southwestern Kenya. Rock and soil samples collected gave average values of the radioactivity concentrations of 40 K, 226 Ra and 232 Th of 915.6, 195.3 and 409.5 Bq kg -1 , respectively. The range of the annual effective dose for a person living in Homa Mountain area calculated varied from 28.6 to 1681.2, with a mean of 470.4 μSv. These results imply Homa Mountain have elevated levels of natural radioactivity thus the region is a high background radiation area

  19. Specific activity and hazards of Archeozoic-Cambrian rock samples collected from the Weibei area of Shaanxi (China))

    International Nuclear Information System (INIS)

    Xinwei, L.; Lingqing, W.; Xiaodan, J.; Leipeng, Y.; Gelian, D.

    2006-01-01

    The present work deals with the radioactivity of the Archeozoic-Cambrian rocks of the Weibei area, Shaanxi (China)). A total of 45 rock samples of Archeozoic-Cambrian strata were investigated. The radionuclides of the samples, in Bq kg -1 , have been measured using Na(I)Tl gamma-ray spectrometer. The concentration of 226 Ra, 232 Th and 40 K in the Archeozoic-Cambrian rock samples range from 12.3 to 55.4, from 2.4 to 98.7 and from 58.6 to 1613.3 Bq kg -1 , respectively. The measured activity concentrations for these radionuclides were compared with the typical world average values. To assess the radiological hazard of the natural radioactivity in the samples, the radium equivalent activity, the external hazard index, internal hazard index and the annual gonadal dose equivalent associated with the radionuclides were calculated and compared with the international recommended values. (authors)

  20. Laboratory testing of rock and salt samples for determination of specific gravity and total porosity of the Zeeck No. 1 well (PD-7), Palo Duro Basin, Texas: unanalyzed data

    International Nuclear Information System (INIS)

    1984-07-01

    This report contains the specific gravity and total porosity determinations for rock and salt samples from Zeeck No. 1 Well of the Permian Basin. The laboratory test samples were measured for water content, apparent specific gravity, specific gravity of solids, total porosity and effective porosity. Specimen descriptions including specimen number, formation/group, and lithologic description as well as typical data sheets are included in the appendices. These data are preliminary. They have been neither analyzed nor evaluated

  1. Transient diffusion from a waste solid into water-saturated, fractured porous rock

    International Nuclear Information System (INIS)

    Ahn, J.; Chambre, P.L.; Pigford, T.H.; Lee, W.W.-L.

    1989-09-01

    Numerical illustrations for transient mass transfer from an infinitely long cylinder intersected by a planar fracture are shown based on Chambre's exact analytical solutions. The concentration at the cylinder surface is maintained at the solubility. In the fracture contaminant diffuses in the radial direction. In the rock matrix three-dimensional diffusion is assumed in the cylindrical coordinate. No advection is assumed. Radioactive decay and sorption equilibrium are included. Radioactive decay enhances the mass transfer from the cylinder. Due to the presence of the fracture, the mass flux from the cylinder to the rock matrix becomes smaller, but the fracture effect is limited in the vicinity of the fracture in early times. Even though the fracture is assumed to be a faster diffusion path than the rock matrix, the larger waste surface exposed to the matrix and the greater assumed matrix sorption result in greater release rate to the matrix than to the fracture. 8 refs., 4 figs

  2. Biodiversity of shallow subtidal, under-rock invertebrates in Europe's first marine reserve: Effects of physical factors and scientific sampling

    Science.gov (United States)

    Trowbridge, Cynthia D.; Kachmarik, Katy; Plowman, Caitlin Q.; Little, Colin; Stirling, Penny; McAllen, Rob

    2017-03-01

    At Lough Hyne Marine Reserve in SW Ireland, shallow subtidal, under-rock biodiversity was investigated to assess (i) any deleterious effects of scientific sampling and (ii) quantitative baseline community patterns. Comparisons were made between 10 sites with annual rock-turning disturbance and 10 with multi-decadal (historical) disturbance. At each site, shallow subtidal rocks (N = 1289 total) were lifted, organisms recorded, and rocks replaced in their original position. Biodiversity indices were calculated to evaluate how diversity varied with location within the lough, frequency of sampling disturbance, degree of hypoxia/anoxia, dissolved oxygen (DO) concentration, and number of rocks turned. The richness of solitary invertebrates surveyed in situ averaged 21 taxa per site with significantly more in the South Basin (near the lough's connection to the ocean) than in the North Basin. The Shannon-Wiener Index did not differ significantly with variables investigated. However, evenness was higher at annually disturbed sites than at historical ones where anemones with algal symbionts often dominated. Several sites were hypoxic to anoxic under the shallow subtidal rocks. Cup corals were most abundant in the South Basin; DO was a crucial explanatory variable of these sensitive species. Solitary ascidians were most abundant at South-Basin annual sites with DO levels being a highly significant explanatory variable.

  3. Evaluation of leachate emissions from crushed rock and municipal solid waste incineration bottom ash used in road construction.

    Science.gov (United States)

    Lidelöw, S; Lagerkvist, A

    2007-01-01

    Three years of leachate emissions from municipal solid waste incineration bottom ash and crushed rock in a full-scale test road were evaluated. The impact of time, construction design, and climate on the emissions was studied, and the predicted release from standard leaching tests was compared with the measured release from the road. The main pollutants and their respective concentrations in leachate from the roadside slope were Al (12.8-85.3 mg l(-1)), Cr (2-125 microg l(-1)), and Cu (0.15-1.9 mg l(-1)) in ash leachate and Zn (1-780 microg l(-1)) in crushed rock leachate. From the ash, the initial Cl(-) release was high ( approximately 20 g l(-1)). After three years, the amount of Cu and Cl(-) was in the same range in both leachates, while that of Al and Cr still was more than one order of magnitude higher in ash leachate. Generally, the release was faster from material in the uncovered slopes than below the pavement. Whether the road was asphalted or not, however, had minor impacts on the leachate quality. During rain events, diluted leachates with respect to, e.g., salts were observed. The leaching tests failed to simulate field leaching from the crushed rock, whereas better agreement was observed for the ash. Comparisons of constituent release from bottom ash and conventional materials solely based on such tests should be avoided.

  4. Evaluation of stress and saturation effects on seismic velocity and electrical resistivity - laboratory testing of rock samples

    Science.gov (United States)

    Vilhelm, Jan; Jirků, Jaroslav; Slavík, Lubomír; Bárta, Jaroslav

    2016-04-01

    Repository, located in a deep geological formation, is today considered the most suitable solution for disposal of spent nuclear fuel and high-level waste. The geological formations, in combination with an engineered barrier system, should ensure isolation of the waste from the environment for thousands of years. For long-term monitoring of such underground excavations special monitoring systems are developed. In our research we developed and tested monitoring system based on repeated ultrasonic time of flight measurement and electrical resistivity tomography (ERT). As a test site Bedřichov gallery in the northern Bohemia was selected. This underground gallery in granitic rock was excavated using Tunnel Boring Machine (TBM). The seismic high-frequency measurements are performed by pulse-transmission technique directly on the rock wall using one seismic source and three receivers in the distances of 1, 2 and 3 m. The ERT measurement is performed also on the rock wall using 48 electrodes. The spacing between electrodes is 20 centimeters. An analysis of relation of seismic velocity and electrical resistivity on water saturation and stress state of the granitic rock is necessary for the interpretation of both seismic monitoring and ERT. Laboratory seismic and resistivity measurements were performed. One series of experiments was based on uniaxial loading of dry and saturated granitic samples. The relation between stress state and ultrasonic wave velocities was tested separately for dry and saturated rock samples. Other experiments were focused on the relation between electrical resistivity of the rock sample and its saturation level. Rock samples with different porosities were tested. Acknowledgments: This work was partially supported by the Technology Agency of the Czech Republic, project No. TA 0302408

  5. Radon exhalation from samples of Danish soils, subsoils and sedimentary rocks

    International Nuclear Information System (INIS)

    Korsbech, U.

    1985-01-01

    For some years it has been known that the ground below a house could be the major source of radon and radon daughters in the indoor air. Th amount of radon penetrating into buildings from the ground depends on several factors e.g. the amount of radon produced in the ground, the amount of cracks and holes in the foundation of buildings, and the pressure difference between the air in the ground (sol air) and the indoor air. As a first step in determining the influence of the ground below Danish buildings 60 samples of soils, subsoils, and sedimentary rocks have been measured for their exhalation rates of radon i.e. the amount of radon escaping the sample per mass unit and per second (Bq.kg -1 .s -1 or radon atoms per kg and per sec.). The results of the measurements of the radon exhalation are presented and commented, and a conclusion concerning the methods for finding geological deposits with a high radon halation rate is presented. (author)

  6. Determination of the thermal neutron absorption cross section for rock samples by a single measurement of the time decay constant

    International Nuclear Information System (INIS)

    Krynicka, E.

    1993-01-01

    A calibration method for the determination of the thermal neutron macroscopic mass absorption cross section for rock samples is presented. The standard deviation of the final results is discussed in detail. A big advantage of the presented method is that the calibration curves have been found using the results obtained for a variety of natural rock samples of different stratigraphies and lithologies measured by Czubek's methods. An important part of the paper is a through analysis of the standard deviation of the final result. (author). 13 refs, 11 figs, 5 tabs

  7. Estimation of spacial geo-stress components in rock samples by using the Kaiser effect of acoustic emission

    International Nuclear Information System (INIS)

    Kanagawa, Tadashi; Hayashi, Masao; Nakasa, Hiroyasu.

    1976-01-01

    The spacial remaining stress component of the rock core sample is experimentally obtained by using Kaiser effect of acoustic emission (AE), and the estimated ground pressure is compared with the natural ground pressure measured by the conventional over-coring method, in order to see the feasiblity of AE method. In this experiments of AE, 111 specimens were cut out in all directions of the rock cores (tuff) sampled from the place where the ground pressure was measured by the over-coring method, and the generation of AE caused by the load was measured. Whereby, the stress components in three directions are determined. As a result of comparison, t the AE method is proved to be effective enough to estimate the ground pressure of rock geo-dynamically. In the application of the Kaiser effect to the estimation of the geo-stress in rock samples, one of the most difficult problems is how to eliminate the obstruction of erroneous AE signals caused by the strong stress concentration at the end corners of the rock specimen. As the result of comparison, the values obtained by the AE method have a tendency of greater than the values obtained by the over-coring method. It is conceived that the AE method can easily detect the maximum stress value for geo historical long time, and that the stress concentration is apt to mix in AE method by boring. (Iwakiri, K.)

  8. A sampling study on rock properties affecting drilling rate index (DRI)

    Science.gov (United States)

    Yenice, Hayati; Özdoğan, Mehmet V.; Özfırat, M. Kemal

    2018-05-01

    Drilling rate index (DRI) developed in Norway is a very useful index in determining the drillability of rocks and even in performance prediction of hard rock TBMs and it requires special laboratory test equipment. Drillability is one of the most important subjects in rock excavation. However, determining drillability index from physical and mechanical properties of rocks is very important for practicing engineers such as underground excavation, drilling operations in open pit mining, underground mining and natural stone production. That is why many researchers have studied concerned with drillability to find the correlations between drilling rate index (DRI) and penetration rate, influence of geological properties on drillability prediction in tunneling, correlations between rock properties and drillability. In this study, the relationships between drilling rate index (DRI) and some physico-mechanical properties (Density, Shore hardness, uniaxial compressive strength (UCS, σc), Indirect tensile strength (ITS, σt)) of three different rock groups including magmatic, sedimentary and metamorphic were evaluated using both simple and multiple regression analysis. This study reveals the effects of rock properties on DRI according to different types of rocks. In simple regression, quite high correlations were found between DRI and uniaxial compressive strength (UCS) and also between DRI and indirect tensile strength (ITS) values. Multiple regression analyses revealed even higher correlations when compared to simple regression. Especially, UCS, ITS, Shore hardness (SH) and the interactions between them were found to be very effective on DRI values.

  9. Small Population Size of the Pribilof Rock Sandpiper Confirmed through Distance-Sampling Surveys in Alaska

    NARCIS (Netherlands)

    Ruthrauff, D.R.; Tibbitts, T.L.; Gill, R.E.; Dementyev, M.N.

    2012-01-01

    The Rock Sandpiper (Calidris ptilocnemis) is endemic to the Bering Sea region and unique among shorebirds in the North Pacific for wintering at high latitudes. The nominate subspecies, the Pribilof Rock Sandpiper (C. p. ptilocnemis), breeds on four isolated islands in the Bering Sea and appears to

  10. Microbial Fluid-Rock Interactions in Chalk Samples and Salinity Factor in Divalent Ca2+ ions Release for Microbial Enhanced Oil Recovery Purposes

    DEFF Research Database (Denmark)

    Jimoh, Ismaila Adetunji; Rudyk, Svetlana Nikolayevna; Søgaard, Erik Gydesen

    2011-01-01

    In this study, laboratory experiments were performed on chalk samples from Danish sector of the North Sea to study microbial fluid-rock interactions with carbonate rock and to evaluate the dissolution of rock matrix (CaCO3). Result showed that the average concentration of Ca2+ ions after microbia...

  11. Quantitative analysis of nano-pore geomaterials and representative sampling for digital rock physics

    Science.gov (United States)

    Yoon, H.; Dewers, T. A.

    2014-12-01

    Geomaterials containing nano-pores (e.g., shales and carbonate rocks) have become increasingly important for emerging problems such as unconventional gas and oil resources, enhanced oil recovery, and geologic storage of CO2. Accurate prediction of coupled geophysical and chemical processes at the pore scale requires realistic representation of pore structure and topology. This is especially true for chalk materials, where pore networks are small and complex, and require characterization at sub-micron scale. In this work, we apply laser scanning confocal microscopy to characterize pore structures and microlithofacies at micron- and greater scales and dual focused ion beam-scanning electron microscopy (FIB-SEM) for 3D imaging of nanometer-to-micron scale microcracks and pore distributions. With imaging techniques advanced for nano-pore characterization, a problem of scale with FIB-SEM images is how to take nanometer scale information and apply it to the thin-section or larger scale. In this work, several texture characterization techniques including graph-based spectral segmentation, support vector machine, and principal component analysis are applied for segmentation clusters represented by 1-2 FIB-SEM samples per each cluster. Geometric and topological properties are analyzed and lattice-Boltzmann method (LBM) is used to obtain permeability at several different scales. Upscaling of permeability to the Darcy scale (e.g., the thin-section scale) with image dataset will be discussed with emphasis on understanding microfracture-matrix interaction, representative volume for FIB-SEM sampling, and multiphase flow and reactive transport. Funding from the DOE Basic Energy Sciences Geosciences Program is gratefully acknowledged. Sandia National Laboratories is a multi-program laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under

  12. Fault rocks from the SAFOD core samples : implications for weakening at shallow depths along the San Andreas Fault, California

    NARCIS (Netherlands)

    Holdsworth, R.E.; van Diggelen, E.W.E.; Spiers, C.J.; Bresser, J.H.P. de; Walker, R.J.; Bown, L.

    2011-01-01

    The drilling of a deep borehole across the actively creeping Parkfield segment of the San Andreas Fault Zone (SAFZ), California, and collection of core materials permit direct geological study of fault zone processes at 2–3 km depth. The three drill cores sample both host and fault rocks and pass

  13. Spin imaging in solids using synchronously rotating field gradients and samples

    International Nuclear Information System (INIS)

    Wind, R.A.; Yannoni, C.S.

    1983-01-01

    A method for spin-imaging in solids using nuclear magnetic resonance (NMR) spectroscopy is described. With this method, the spin density distribution of a two- or three-dimensional object such as a solid can be constructed resulting in an image of the sample. This method lends itself to computer control to map out an image of the object. This spin-imaging method involves the steps of placing a solid sample in the rf coil field and the external magnetic field of an NMR spectrometer. A magnetic field gradient is superimposed across the sample to provide a field gradient which results in a varying DC field that has different values over different parts of the sample. As a result, nuclei in different parts of the sample have different resonant NMR frequencies. The sample is rotated about an axis which makes a particular angle of 54.7 degrees with the static external magnetic field. The magnetic field gradient which has a spatial distribution related to the sample spinning axis is then rotated synchronously with the sample. Data is then collected while performing a solid state NMR line narrowing procedure. The next step is to change the phase relation between the sample rotation and the field gradient rotation. The data is again collected as before while the sample and field gradient are synchronously rotated. The phase relation is changed a number of times and data collected each time. The spin image of the solid sample is then reconstructed from the collected data

  14. Effects of porosity on seismic velocities, elastic moduli and Poisson's ratios of solid materials and rocks

    Directory of Open Access Journals (Sweden)

    Chengbo Yu

    2016-02-01

    Full Text Available The generalized mixture rule (GMR is used to provide a unified framework for describing Young's (E, shear (G and bulk (K moduli, Lame parameter (λ, and P- and S-wave velocities (Vp and Vs as a function of porosity in various isotropic materials such as metals, ceramics and rocks. The characteristic J values of the GMR for E, G, K and λ of each material are systematically different and display consistent correlations with the Poisson's ratio of the nonporous material (ν0. For the materials dominated by corner-shaped pores, the fixed point at which the effective Poisson's ratio (ν remains constant is at ν0 = 0.2, and J(G > J(E > J(K > J(λ and J(G  0.2 and ν0  J(Vp and J(Vs  0.2 and ν0  0.2 and ν0 = 0.2, respectively. For natural rocks containing thin-disk-shaped pores parallel to mineral cleavages, grain boundaries and foliation, however, the ν fixed point decreases nonlinearly with decreasing pore aspect ratio (α: width/length. With increasing depth or pressure, cracks with smaller α values are progressively closed, making the ν fixed point rise and finally reach to the point at ν0 = 0.2.

  15. Seismic attenuation and scattering tomography of rock samples using stochastic wavefields: linking seismology, volcanology, and rock physics.

    Science.gov (United States)

    Fazio, Marco; De Siena, Luca; Benson, Phillip

    2016-04-01

    Seismic attenuation and scattering are two attributes that can be linked with porosity and permeability in laboratory experiments. When measuring these two quantities using seismic waveforms recorder at lithospheric and volcanic scales the areas of highest heterogeneity, as batches of melt and zones of high deformation, produce anomalous values of the measured quantities, the seismic quality factor and scattering coefficient. When employed as indicators of heterogeneity and absorption in volcanic areas these anomalous effects become strong indicators of magma accumulation and tectonic boundaries, shaping magmatic chambers and conduit systems. We perform attenuation and scattering measurements and imaging using seismic waveforms produced in laboratory experiments, at frequencies ranging between the kHz and MHz. As attenuation and scattering are measured from the shape of the envelopes, disregarding phases, we are able to connect the observations with the micro fracturing and petrological quantities previously measured on the sample. Connecting the imaging of dry and saturated samples via these novel attributes with the burst of low-period events with increasing saturation and deformation is a challenge. Its solution could plant the seed for better relating attenuation and scattering tomography measurements to the presence of fluids and gas, therefore creating a novel path for reliable porosity and permeability tomography. In particular for volcanoes, being able to relate attenuation/scattering measurements with low-period micro seismicity could deliver new data to settle the debate about if both source and medium can produce seismic resonance.

  16. Determination of element concentrations in biological reference materials by solid sampling and other analytical methods

    International Nuclear Information System (INIS)

    Schauenburg, H.; Weigert, P.

    1992-01-01

    Using solid sampling with graphite furnace atomic absorption spectrometry (GFAAS), values for cadmium, copper, lead and zinc in six biological reference materials were obtained from up to four laboratories participating in three collaborative studies. These results are compared with those obtained with other methods used in routine analysis from laboratories of official food control. Under certain conditions solid sampling with GFAAS seems to be suitable for routine analysis as well as conventional methods. (orig.)

  17. Solid State Characterization of Commercial Crystalline and Amorphous Atorvastatin Calcium Samples

    OpenAIRE

    Shete, Ganesh; Puri, Vibha; Kumar, Lokesh; Bansal, Arvind K.

    2010-01-01

    Atorvastatin calcium (ATC), an anti-lipid BCS class II drug, is marketed in crystalline and amorphous solid forms. The objective of this study was to perform solid state characterization of commercial crystalline and amorphous ATC drug samples available in the Indian market. Six samples each of crystalline and amorphous ATC were characterized using X-ray powder diffractometry (XRPD), differential scanning calorimetry (DSC), thermogravimetric analysis, Karl Fisher titrimetry, microscopy (hot s...

  18. Molecular diversity of bacterial communities from subseafloor rock samples in a deep-water production basin in Brazil.

    Science.gov (United States)

    von der Weid, Irene; Korenblum, Elisa; Jurelevicius, Diogo; Rosado, Alexandre Soares; Dino, Rodolfo; Sebastian, Gina Vasquez; Seldin, Lucy

    2008-01-01

    The deep subseafloor rock in oil reservoirs represents a unique environment in which a high oilcontamination and very low biomass can be observed. Sampling this environment has been a challenge owing to the techniques used for drilling and coring. In this study, the facilities developed by the Brazilian oil company PETROBRAS for accessing deep subsurface oil reservoirs were used to obtain rock samples at 2,822-2,828 m below the ocean floor surface from a virgin field located in the Atlantic Ocean, Rio de Janeiro. To address the bacterial diversity of these rock samples, PCR amplicons were obtained using the DNA from four core sections and universal primers for 16S rRNA and for APS reductase (aps) genes. Clone libraries were generated from these PCR fragments and 87 clones were sequenced. The phylogenetic analyses of the 16S rDNA clone libraries showed a wide distribution of types in the domain bacteria in the four core samples, and the majority of the clones were identified as belonging to Betaproteobacteria. The sulfate-reducing bacteria community could only be amplified by PCR in one sample, and all clones were identified as belonging to Gammaproteobacteria. For the first time, the bacterial community was assessed in such deep subsurface environment.

  19. Busted Butte Phase 2: Analysis of Post-Test Mineback and Overcore Rock Samples

    International Nuclear Information System (INIS)

    Turin, H.J.; McGraw, M.A.; Jones, C.L.; Scism, C.D.; Soll, W.E.

    2002-01-01

    A complex tracer mixture was injected continuously for over two years into a 10 x 10 x 7 m block of tuff as part of the unsaturated-zone (UZ) tracer test at Busted Butte. The test was designed to address uncertainties associated with flow and transport models within the Topopah Springs and Calico Hills tuffs. The tracer mixture included nonreactive (Br, I, and FBAs) and reactive tracers (Li, Ce, Sm, Ni, Coy and Mn) and synthetic colloids. Once injection was completed, samples from the block were collected in two ways. Overcores were taken from around and below injection holes. Then, the entire block was excavated via mineback--during which progressive vertical planes of the block were exposed. Samples from the overcores and mineback were analyzed to determine the distribution of tracers on different spatial scales than available from collection borehole data. Rock analyses confirmed collection pad results that the nonreactive tracers, Br and FBAs, moved several meters. Furthermore, Br and FBAs are observed above and lateral to the injector planes suggesting that capillarity was an important process for tracer movement. Lithium, the most mobile of the metals, was transported on a scale of meters. This is consistent with laboratory sorption measurements and observed breakthrough on the collection pads. Co and Ni show transport distances of tens of cm, while Sm and Ce moved far less, possibly due to precipitation and sorption effects. Colloid transport was assessed using 1 ft3 blocks extracted from the BB Phase 2 block. In the Calico Hills material, after 15 L of water was injected over 3.5 months, less than 1% of the colloids injected were recovered. Flow patterns in the block indicate that water injected at the center imbibed outward from the injection point. In a block taken from a boundary of the Calico Hills ashfall layer, breakthrough was observed only due to fractures formed during drying of the block. The colloid transport module for FEHM was tested against

  20. Characterization of rock samples localized in some sites of the Mexican Pacific coast

    International Nuclear Information System (INIS)

    Pena, P.; Torre, J. de la; Falcon, T.; Segovia, N.; Azorin, J.

    1999-01-01

    Geophysical studies in zones of high seismicity have showed differences in the content of radioactive material that is used in the study of the geochemical behavior of the subsoil. In an emanometric mapping of radon in soil realized in the Mexican Pacific coast were finding distinct levels in zones with different lithology. With the finality to know the mineralization types in two zones of study which are localized in the Guerrero coast and they belonging to terrains named Guerrero and Xolapa it was determined the mineralogic characteristics in two types of rocks. The identification of the rocks was realized by X-ray diffraction and was determined the elemental chemical composition using a scanning electron microscope. It was indicated in the results obtained that in the two types of rocks were found minerals such as: quartz, albite, microcline anortite, ferroactinolite and biotite. However, it was found differences between them by the presence of their mineralogic compounds because in the rock belonging to Xolapa terrain were presented whereas in the rock localized in the Guerrero terrain were presented sodic and potassic feldspars. The analysis by the Elemental Chemical Composition technique (Energy Dispersive Spectroscopy) corroborated the results obtained by the X-ray diffraction technique. (Author)

  1. Method for fractional solid-waste sampling and chemical analysis

    DEFF Research Database (Denmark)

    Riber, Christian; Rodushkin, I.; Spliid, Henrik

    2007-01-01

    four subsampling methods and five digestion methods, paying attention to the heterogeneity and the material characteristics of the waste fractions, it was possible to determine 61 substances with low detection limits, reasonable variance, and high accuracy. For most of the substances of environmental...... of variance (20-85% of the overall variation). Only by increasing the sample size significantly can this variance be reduced. The accuracy and short-term reproducibility of the chemical characterization were good, as determined by the analysis of several relevant certified reference materials. Typically, six...... to eight different certified reference materials representing a range of concentrations levels and matrix characteristics were included. Based on the documentation provided, the methods introduced were considered satisfactory for characterization of the chemical composition of waste-material fractions...

  2. A simple source preparation method for alpha-ray spectrometry of volcanic rock sample

    International Nuclear Information System (INIS)

    Takahashi, Masaomi; Kurihara, Yuichi; Sato, Jun

    2006-01-01

    A simple source preparation method was developed for the alpha-ray spectrometry to determine U and Th in volcanic rockes. Isolation of U and Th from volcanic rocks was made by use of UTEVA-Spec. resin, extraction chromatograph material. U and Th were extracted by TTA-benzene solution and organic phase was evaporated drop by drop on a hot stainless steel planchet to dryness. This method was found to be effective for the preparation of sources for alpha-ray spectrometry. (author)

  3. Investigate the capability of INAA absolute method to determine the concentrations of 238U and 232Th in rock samples

    International Nuclear Information System (INIS)

    Alnour, I.A.

    2014-01-01

    This work aimed to study the capability of INAA absolute method in determining the elemental concentration of 238 U and 232 Th in the rock samples. The INAA absolute method was implemented in PUSPATI TRIGA Mark II research reactor, Malaysian Nuclear Agency (NM). The accuracy of INAA absolute method was performed by analyzing the IAEA certified reference material (CRM) Soil-7. The analytical results showed the deviations between experimental and certified values were mostly less than 10 % with Z-score in most cases less than 1. In general, the results of analysed CRM Soil-7 show a good agreement between certified and experimental results which mean that the INAA absolute method can be used accurately for elemental analysis of uranium and thorium in various types of samples. The concentration of 238 U and 232 Th ranged from 1.77 to 24.25 and 0.88 to 95.50 ppm respectively. The highest value of 238 U and 232 Th was recorded for granite rock sample G17 of 238 U and sample G9 of 232 Th, whereas the lower value was 1.77 ppm of 238 U recorded in sandstone rock and 0.88 ppm of 232 Th for gabbro. Moreover, a comparison of the 238 U and 232 Th results obtained by the INAA absolute method shows an acceptable level of consistency with those obtained by the INAA relative method. (author)

  4. Spatio-temporal foreshock activity during stick-slip experiments of large rock samples

    Science.gov (United States)

    Tsujimura, Y.; Kawakata, H.; Fukuyama, E.; Yamashita, F.; Xu, S.; Mizoguchi, K.; Takizawa, S.; Hirano, S.

    2016-12-01

    Foreshock activity has sometimes been reported for large earthquakes, and has been roughly classified into the following two classes. For shallow intraplate earthquakes, foreshocks occurred in the vicinity of the mainshock hypocenter (e.g., Doi and Kawakata, 2012; 2013). And for intraplate subduction earthquakes, foreshock hypocenters migrated toward the mainshock hypocenter (Kato, et al., 2012; Yagi et al., 2014). To understand how foreshocks occur, it is useful to investigate the spatio-temporal activities of foreshocks in the laboratory experiments under controlled conditions. We have conducted stick-slip experiments by using a large-scale biaxial friction apparatus at NIED in Japan (e.g., Fukuyama et al., 2014). Our previous results showed that stick-slip events repeatedly occurred in a run, but only those later events were preceded by foreshocks. Kawakata et al. (2014) inferred that the gouge generated during the run was an important key for foreshock occurrence. In this study, we proceeded to carry out stick-slip experiments of large rock samples whose interface (fault plane) is 1.5 meter long and 0.5 meter wide. After some runs to generate fault gouge between the interface. In the current experiments, we investigated spatio-temporal activities of foreshocks. We detected foreshocks from waveform records of 3D array of piezo-electric sensors. Our new results showed that more than three foreshocks (typically about twenty) had occurred during each stick-slip event, in contrast to the few foreshocks observed during previous experiments without pre-existing gouge. Next, we estimated the hypocenter locations of the stick-slip events, and found that they were located near the opposite end to the loading point. In addition, we observed a migration of foreshock hypocenters toward the hypocenter of each stick-slip event. This suggests that the foreshock activity observed in our current experiments was similar to that for the interplate earthquakes in terms of the

  5. Procedures for sampling and sample reduction within quality assurance systems for solid biofuels

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2005-07-01

    The objective of this experimental study on sampling was to determine the size and number of samples of biofuels required (taken at two sampling points in each case) and to compare two methods of sampling. The first objective of the sample-reduction exercise was to compare the reliability of various sampling methods, and the second objective was to measure the variations introduced as a result of reducing the sample size to form suitable test portions. The materials studied were sawdust, wood chips, wood pellets and bales of straw, and these were analysed for moisture, ash, particle size and chloride. The sampling procedures are described. The study was conducted in Scandinavia. The results of the study were presented in Leipzig in October 2004. The work was carried out as part of the UK's DTI Technology Programme: New and Renewable Energy.

  6. Correlation Analysis of the Ultrasonic Emission from Loaded Rock Samples – the Study of Interaction of Microcracking Nucleation Centres

    Czech Academy of Sciences Publication Activity Database

    Vilhelm, J.; Rudajev, Vladimír; Lokajíček, Tomáš; Veverka, Ján

    2008-01-01

    Roč. 41, č. 5 (2008), s. 695-714 ISSN 0723-2632 R&D Projects: GA ČR GA205/04/0088; GA ČR GA205/06/0906 Institutional research plan: CEZ:AV0Z30130516; CEZ:AV0Z30460519 Keywords : rock sample * ultrasonic emission * cracks nucleation * autocorrelation analysis * laboratory loading Subject RIV: DB - Geology ; Mineralogy Impact factor: 0.589, year: 2008

  7. Study on the application of crown ether for neutron activation analysis of rubidium and rhenium in rock samples

    International Nuclear Information System (INIS)

    Wang Xiaolin; Fu Yibei; Liu Yinong; Xiong Zonghua; Hao Fanhua

    1996-01-01

    The extraction behaviour of rubidium and rhenium with 18-crown-6 (18C6) and benzo-15-crown-5 (B15C5) in nitrobenzene from picric acid or potassium hydroxide solution are studied and methods for separation and determination are developed. The molar ratio of 18C6 to Rb and B15C5 to Re in the extracted species is probably 2:1. Rubidium and rhenium in rock samples are satisfactorily determined by neutron activation method

  8. Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip

    Science.gov (United States)

    Mora, Maria F.; Stockton, Amanda M.; Willis, Peter A.

    2013-01-01

    There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given

  9. Two-dimensional T2 distribution mapping in rock core plugs with optimal k-space sampling.

    Science.gov (United States)

    Xiao, Dan; Balcom, Bruce J

    2012-07-01

    Spin-echo single point imaging has been employed for 1D T(2) distribution mapping, but a simple extension to 2D is challenging since the time increase is n fold, where n is the number of pixels in the second dimension. Nevertheless 2D T(2) mapping in fluid saturated rock core plugs is highly desirable because the bedding plane structure in rocks often results in different pore properties within the sample. The acquisition time can be improved by undersampling k-space. The cylindrical shape of rock core plugs yields well defined intensity distributions in k-space that may be efficiently determined by new k-space sampling patterns that are developed in this work. These patterns acquire 22.2% and 11.7% of the k-space data points. Companion density images may be employed, in a keyhole imaging sense, to improve image quality. T(2) weighted images are fit to extract T(2) distributions, pixel by pixel, employing an inverse Laplace transform. Images reconstructed with compressed sensing, with similar acceleration factors, are also presented. The results show that restricted k-space sampling, in this application, provides high quality results. Copyright © 2012 Elsevier Inc. All rights reserved.

  10. Solid state characterization of commercial crystalline and amorphous atorvastatin calcium samples.

    Science.gov (United States)

    Shete, Ganesh; Puri, Vibha; Kumar, Lokesh; Bansal, Arvind K

    2010-06-01

    Atorvastatin calcium (ATC), an anti-lipid BCS class II drug, is marketed in crystalline and amorphous solid forms. The objective of this study was to perform solid state characterization of commercial crystalline and amorphous ATC drug samples available in the Indian market. Six samples each of crystalline and amorphous ATC were characterized using X-ray powder diffractometry (XRPD), differential scanning calorimetry (DSC), thermogravimetric analysis, Karl Fisher titrimetry, microscopy (hot stage microscopy, scanning electron microscopy), contact angle, and intrinsic dissolution rate (IDR). All crystalline ATC samples were found to be stable form I, however one sample possessed polymorphic impurity, evidenced in XRPD and DSC analysis. Amongst the amorphous ATC samples, XRPD demonstrated five samples to be amorphous 'form 27', while, one matched amorphous 'form 23'. Thermal behavior of amorphous ATC samples was compared to amorphous ATC generated by melt quenching in DSC. ATC was found to be an excellent glass former with T(g)/T(m) of 0.95. Residual crystallinity was detected in two of the amorphous samples by complementary use of conventional and modulated DSC techniques. The wettability and IDR of all amorphous samples was found to be higher than the crystalline samples. In conclusion, commercial ATC samples exhibited diverse solid state behavior that can impact the performance and stability of the dosage forms.

  11. Study of uranium mineralization in rock samples from marwat range bannu basin by fission track analysis technique

    International Nuclear Information System (INIS)

    Qureshi, A.Z.; Ullah, K.; Ullah, N.; Akram, M.

    2004-07-01

    The Geophysics Division, Atomic Energy Minerals Centre (AEMC), Lahore has planned a uranium exploration program in Marwat Range, Bannu Basin. In this connection 30 thin sections of rock samples, collected from four areas; namely, Darra Tang, Simukili, Karkanwal and Sheikhillah from Marwat Range, and one from Salt Range were provided to Nuclear Geology Group of Physics Research Division, PINSTECH for the study of nature and mechanism of uranium mineralization These studies are aimed to help in designing uranium exploration strategy by providing the loci of uranium sources in the Marwat and Salt Ranges. The samples have been studied using fission track analysis technique. (author)

  12. Effluents from a waste rock deposit of a former uranium mine in Saxony/Germany - Mass flow balance of water and dissolved solids

    International Nuclear Information System (INIS)

    Biehler, D.

    2002-01-01

    Soon after uranium mining had ceased in eastern Germany in 1990, work for remediation of several mining sites began. The Wismut GmbH, owner of the Mine of Dresden-Gittersee's waste rock dump, introduced the concept of reducing the impact to the environment via water and air paths by implementing a multi-layer soil cover. The deposit consists mainly of waste rock (clastic sediments of Doehlener Becken, deep metamorphic rocks) but also of low-grade ore (U-rich coal) and tailing materials. At the time when remediation started, the effluents completely infiltrated the underground. Because of previous surface exfiltration activities, they were already known to be very rich in dissolved solids, especially in sulphate and uranium. As demanded by the state authorities, the owner funded a vast hydrogeological study of the site. In testing the efficiency of surface sealing, the study indicated a mass flow balance of water and dissolved solids for the current situation, and predicted emissions into the water path which would occur after realisation of the proposed soil cover. The field investigation program consisted of: measurements of flow, of concentrations of dissolved solids (esp. U and Ra-226) and of contents of environmental isotopes in precipitation, surface runoff, seepage water and groundwater in the current condition of the dump; the study of waste rock material (geochemistry, mineralogy); waste rock material elution tests; underground investigation by drilling boreholes up to 270 m in depth. The resulting data allowed for: a hydrogeological conceptual model of the site; a consistent mass flow balance for the current condition of the dump; a prediction of concentrations in groundwater resulting after the realisation of a soil cover. The predictions show that the concentrations of dissolved solids in the contaminated groundwater would be significantly decreased. Furthermore it would be possible to reach the standards for drinking water with respect to uranium

  13. Hydrothermal frictional strengths of rock and mineral samples relevant to the creeping section of the San Andreas Fault

    Science.gov (United States)

    Moore, Diane E.; Lockner, David A.; Hickman, Stephen H.

    2016-01-01

    We compare frictional strengths in the temperature range 25–250 °C of fault gouge from SAFOD (CDZ and SDZ) with quartzofeldspathic wall rocks typical of the central creeping section of the San Andreas Fault (Great Valley sequence and Franciscan Complex). The Great Valley and Franciscan samples have coefficients of friction, μ > 0.35 at all experimental conditions. Strength is unchanged between 25° and 150 °C, but μ increases at higher temperatures, exceeding 0.50 at 250 °C. Both samples are velocity strengthening at room temperature but show velocity-weakening behavior beginning at 150 °C and stick-slip motion at 250 °C. These rocks, therefore, have the potential for unstable seismic slip at depth. The CDZ gouge, with a high saponite content, is weak (μ = 0.09–0.17) and velocity strengthening in all experiments, and μ decreases at temperatures above 150 °C. Behavior of the SDZ is intermediate between the CDZ and wall rocks: μ < 0.2 and does not vary with temperature. Although saponite is probably not stable at depths greater than ∼3 km, substitution of the frictionally similar minerals talc and Mg-rich chlorite for saponite at higher temperatures could potentially extend the range of low strength and stable slip down to the base of the seismogenic zone.

  14. Trace and major elements in rock samples from Itingussu River Basin, Coroa-Grande, Rio de Janeiro

    International Nuclear Information System (INIS)

    Araripe, D.R.; Patchineelam, S.R.; Bellido, A.V.B.; Vasconcellos, M.B.A.

    2006-01-01

    The goal of the present work was to determine the concentration of 23 elements by instrumental neutron activation analysis in rock samples from the vicinity of Itingussu River, in order to investigate the contribution of trace and major elements from the local lithology to the river basin. The Itingussu River Basin ends in a mangrove area not yet largely impacted by antropogenic activities. So far, there are no data for the concentration of trace elements in that region, even though these data are important to the understanding of the influence of the rocks on the composition of the mangrove sediments. The results showed some enrichment of Th and some light rare earths, probably because of the presence of the mineral allanite and other accessory minerals, as identified by petrographic analysis. (author)

  15. Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

    Science.gov (United States)

    Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

    2004-01-01

    A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

  16. Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

    International Nuclear Information System (INIS)

    Pourreza, N.

    2004-01-01

    Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

  17. Radon exhalations of rock samples from the Muellenbach uranium test mine

    International Nuclear Information System (INIS)

    Keller, G.; Dudler, R.

    1985-01-01

    Radiation exposure of workers in underground mines with high U/Ra concentration is mostly due to inhalation of the short-lived radioactive decay products of the noble gas radon. Knowledge of the Rn-222 exhalation rates of walls and rocks as well as the contributing influencing parameters is therefore of interest for radiation protection purposes. Measurements showed that in the hours following shortfiring operations, the fresh dirt and the new walls had several times the exhalation rates of older dirt and walls. Measurements of exhalation rates on drill cores can help to assess exhalation for an adequate layout of the mine ventilation system. (orig./PW) [de

  18. Modified emission-transmission method for determining trace elements in solid samples using the XRF techniques

    International Nuclear Information System (INIS)

    Poblete, V.; Alvarez, M.; Hermosilla, M.

    2000-01-01

    This is a study of an analysis of trace elements in medium thick solid samples, by the modified transmission emission method, using the energy dispersion X-ray fluorescence technique (EDXRF). The effects of absorption and reinforcement are the main disadvantages of the EDXRF technique for the quantitative analysis of bigger elements and trace elements in solid samples. The implementation of this method and its application to a variety of samples was carried out using an infinitely thick multi-element white sample that calculates the correction factors by absorbing all the analytes in the sample. The discontinuities in the masic absorption coefficients versus energies association for each element, with medium thick and homogenous samples, are analyzed and corrected. A thorough analysis of the different theoretical and test variables are proven by using real samples, including certified material with known concentration. The simplicity of the calculation method and the results obtained show the method's major precision, with possibilities for the non-destructive routine analysis of different solid samples, using the EDXRF technique (author)

  19. Fast acquisition of multidimensional NMR spectra of solids and mesophases using alternative sampling methods.

    Science.gov (United States)

    Lesot, Philippe; Kazimierczuk, Krzysztof; Trébosc, Julien; Amoureux, Jean-Paul; Lafon, Olivier

    2015-11-01

    Unique information about the atom-level structure and dynamics of solids and mesophases can be obtained by the use of multidimensional nuclear magnetic resonance (NMR) experiments. Nevertheless, the acquisition of these experiments often requires long acquisition times. We review here alternative sampling methods, which have been proposed to circumvent this issue in the case of solids and mesophases. Compared to the spectra of solutions, those of solids and mesophases present some specificities because they usually display lower signal-to-noise ratios, non-Lorentzian line shapes, lower spectral resolutions and wider spectral widths. We highlight herein the advantages and limitations of these alternative sampling methods. A first route to accelerate the acquisition time of multidimensional NMR spectra consists in the use of sparse sampling schemes, such as truncated, radial or random sampling ones. These sparsely sampled datasets are generally processed by reconstruction methods differing from the Discrete Fourier Transform (DFT). A host of non-DFT methods have been applied for solids and mesophases, including the G-matrix Fourier transform, the linear least-square procedures, the covariance transform, the maximum entropy and the compressed sensing. A second class of alternative sampling consists in departing from the Jeener paradigm for multidimensional NMR experiments. These non-Jeener methods include Hadamard spectroscopy as well as spatial or orientational encoding of the evolution frequencies. The increasing number of high field NMR magnets and the development of techniques to enhance NMR sensitivity will contribute to widen the use of these alternative sampling methods for the study of solids and mesophases in the coming years. Copyright © 2015 John Wiley & Sons, Ltd.

  20. Impact of solid second phases on deformation mechanisms of naturally deformed salt rocks (Kuh-e-Namak, Dashti, Iran) and rheological stratification of the Hormuz Salt Formation

    Science.gov (United States)

    Závada, P.; Desbois, G.; Urai, J. L.; Schulmann, K.; Rahmati, M.; Lexa, O.; Wollenberg, U.

    2015-05-01

    Viscosity contrasts displayed in flow structures of a mountain namakier (Kuh-e-Namak - Dashti), between 'weak' second phase bearing rock salt and 'strong' pure rock salt types are studied for deformation mechanisms using detailed quantitative microstructural study. While the solid inclusions rich ("dirty") rock salts contain disaggregated siltstone and dolomite interlayers, "clean" salts reveal microscopic hematite and remnants of abundant fluid inclusions in non-recrystallized cores of porphyroclasts. Although the flow in both, the recrystallized "dirty" and "clean" salt types is accommodated by combined mechanisms of pressure-solution creep (PS), grain boundary sliding (GBS), transgranular microcracking and dislocation creep accommodated grain boundary migration (GBM), their viscosity contrasts observed in the field outcrops are explained by: 1) enhanced ductility of "dirty" salts due to increased diffusion rates along the solid inclusion-halite contacts than along halite-halite contacts, and 2) slow rates of intergranular diffusion due to dissolved iron and inhibited dislocation creep due to hematite inclusions for "clean" salt types Rheological contrasts inferred by microstructural analysis between both salt rock classes apply in general for the "dirty" salt forming Lower Hormuz and the "clean" salt forming the Upper Hormuz of the Hormuz Formation and imply strain rate gradients or decoupling along horizons of mobilized salt types of different composition and microstructure.

  1. Solid phase microextraction headspace sampling of chemical warfare agent contaminated samples : method development for GC-MS analysis

    Energy Technology Data Exchange (ETDEWEB)

    Jackson Lepage, C.R.; Hancock, J.R. [Defence Research and Development Canada, Medicine Hat, AB (Canada); Wyatt, H.D.M. [Regina Univ., SK (Canada)

    2004-07-01

    Defence R and D Canada-Suffield (DRDC-Suffield) is responsible for analyzing samples that are suspected to contain chemical warfare agents, either collected by the Canadian Forces or by first-responders in the event of a terrorist attack in Canada. The analytical techniques used to identify the composition of the samples include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Fourier-transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy. GC-MS and LC-MS generally require solvent extraction and reconcentration, thereby increasing sample handling. The authors examined analytical techniques which reduce or eliminate sample manipulation. In particular, this paper presented a screening method based on solid phase microextraction (SPME) headspace sampling and GC-MS analysis for chemical warfare agents such as mustard, sarin, soman, and cyclohexyl methylphosphonofluoridate in contaminated soil samples. SPME is a method which uses small adsorbent polymer coated silica fibers that trap vaporous or liquid analytes for GC or LC analysis. Collection efficiency can be increased by adjusting sampling time and temperature. This method was tested on two real-world samples, one from excavated chemical munitions and the second from a caustic decontamination mixture. 7 refs., 2 tabs., 3 figs.

  2. Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

    Czech Academy of Sciences Publication Activity Database

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

    Roč. 99, S (2005), s489-s491 ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] Institutional research plan: CEZ:AV0Z40310501 Keywords : solid sampling * electrothermal atomic absorption spectrometry * trace analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

  3. The Validation of AAN Method Used by Rock Sample SRM 2780

    International Nuclear Information System (INIS)

    Rina Mulyaningsih, Th.

    2004-01-01

    AAN methods is a non standard testing method. The testing laboratory must be validate its using method to ensure and confirm that it is suitable with application. The analysis of SRM 2780 Hard rock mine waste with 9 replicates has been done to test the accuracy of AAN methods. The result showed that the elements As, Ba, Mn, V, Zn and Na have good accuration were evaluated against the acceptance criteria for accuracy with confidence level 95 %. The elements As, Co, Sc, Cr, Ba, Sb, Cs, Mn, V, Au, Zn and Na have low relative bias between the analyst's value and the target value. The continued testing must be done to test the accuracy of another certificated elements. (author)

  4. A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples

    Science.gov (United States)

    Carr, R. H.; Bustin, R.; Gibson, E. K.

    1987-01-01

    A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen.

  5. Hydrothermal interaction of solid wafers of Topopah Spring Tuff with J-13 water and distilled water at 90, 150, and 250{sup 0}C, using Dickson-type, gold-bag rocking autoclaves

    Energy Technology Data Exchange (ETDEWEB)

    Knauss, K.G.; Beiriger, W.J.; Peifer, D.W.; Piwinskii, A.J.

    1985-09-01

    The Nevada Nuclear Waste Storage Investigations Project has conducted experiments to study the hydrothermal interaction of rock and water representative of a potential high-level waste repository at Yucca Mountain, Nevada. The results of these experiments help define the near-field repository environment during and shortly after the thermal period that results from the emplacement of nuclear waste. When considered in conjunction with results contained in companion reports, these results can be used to assess our ability to accelerate tests using the surface area/volume parameter and/or temperature. These rock-water interaction experiments were conducted with solid polished wafers cut from both drillcore and outcrop samples of Topopah tuff, using both a natural ground water and distilled water as the reacting fluid. Pre- and post-test characterization of the reacting materials was extensive. Post-test identification and chemical analysis of secondary phases resulting from the hydrothermal interactions were aided by using monoliths of tuff rather than crushed material. All experiments were run in Dickson-type, gold-bag rocking autoclaves that were periodically sampled at in situ conditions. A total of nine short-term (up to 66-day) experiments were run in this series; these experiments covered the range from 90 to 250{sup 0}C and from 50 to 100 bar. The results obtained from the experiments have been used to evaluate the modeled results produced by calculations using the geochemical reaction process code EQ3/6. 31 refs., 37 figs., 7 tabs.

  6. Hydrothermal interaction of solid wafers of Topopah Spring Tuff with J-13 water and distilled water at 90, 150, and 2500C, using Dickson-type, gold-bag rocking autoclaves

    International Nuclear Information System (INIS)

    Knauss, K.G.; Beiriger, W.J.; Peifer, D.W.; Piwinskii, A.J.

    1985-09-01

    The Nevada Nuclear Waste Storage Investigations Project has conducted experiments to study the hydrothermal interaction of rock and water representative of a potential high-level waste repository at Yucca Mountain, Nevada. The results of these experiments help define the near-field repository environment during and shortly after the thermal period that results from the emplacement of nuclear waste. When considered in conjunction with results contained in companion reports, these results can be used to assess our ability to accelerate tests using the surface area/volume parameter and/or temperature. These rock-water interaction experiments were conducted with solid polished wafers cut from both drillcore and outcrop samples of Topopah tuff, using both a natural ground water and distilled water as the reacting fluid. Pre- and post-test characterization of the reacting materials was extensive. Post-test identification and chemical analysis of secondary phases resulting from the hydrothermal interactions were aided by using monoliths of tuff rather than crushed material. All experiments were run in Dickson-type, gold-bag rocking autoclaves that were periodically sampled at in situ conditions. A total of nine short-term (up to 66-day) experiments were run in this series; these experiments covered the range from 90 to 250 0 C and from 50 to 100 bar. The results obtained from the experiments have been used to evaluate the modeled results produced by calculations using the geochemical reaction process code EQ3/6. 31 refs., 37 figs., 7 tabs

  7. Reimiep 87. An interlaboratory U-235 enrichment determination by gamma measurement on solid UF6 sample

    International Nuclear Information System (INIS)

    Aparo, M.; Cresti, P.

    1988-01-01

    Gamma spectroscopy technique, based on the measurement of U 235 186 KeV flux, is now currently used for the determination of Uranium enrichment in different material of nuclear fuel cycle, namely: Uranium metallic, UO 2 pellets, UF 6 liquid or solid. The present paper describes the use of such a technique and the obtained results in determining the U 235 /U atomic isotopic abundance on a certified UF 6 solid sample. The measurements have been carried out in the frame work of the partecipation to the ''UF 6 Interlaboratory Measurements Evaluation Programme'' organized by CBNM/Geel with the support of the ESARDA (European Safeguards Research and Development Association)

  8. Non-destructive sampling of rock-dwelling microbial communities using sterile adhesive tape.

    Science.gov (United States)

    Cutler, Nick A; Oliver, Anna E; Viles, Heather A; Whiteley, Andrew S

    2012-12-01

    Building stone provides a habitat for an array of microorganisms, many of which have been demonstrated to have a deleterious effect on the appearance and/or structural integrity of stone masonry. It is essential to understand the composition and structure of stone-dwelling (lithobiontic) microbial communities if successful stone conservation strategies are to be applied, particularly in the face of global environmental change. Ideally, the techniques used to sample such assemblages should be non-destructive due to the sensitive conservation status of many stone buildings. This paper quantitatively assesses the performance of sterile adhesive tape as a non-destructive sampling technique and compares the results of tape sampling with an alternative, destructive, sampling method. We used DNA fingerprinting (TRFLP) to characterise the algal, fungal and bacterial communities living on a stone slab. Our results demonstrate that tape sampling may be used to collect viable quantities of microbial DNA from environmental samples. This technique is ideally suited to the sampling of microbial biofilms, particularly when these communities are dominated by green algae. It provides a good approximation of total community diversity (i.e. the aggregate diversity of epilithic and endolithic communities). Tape sampling is straightforward, rapid and cost effective. When combined with molecular analytical techniques, this sampling method has the potential to make a major contribution to efforts to understand the structure of lithobiontic microbial communities and our ability to predict the response of such communities to future environmental change. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. Determination of radiocaesium in agriculture-related water samples containing suspended solids using gelling method

    International Nuclear Information System (INIS)

    Matsunami, Hisaya; Shin, Moono; Takahashi, Yoshihiko; Shinano, Takuro; Kitajima, Shiori; Tsuchiya, Takashi

    2015-01-01

    After the TEPCO Fukushima Dai-ichi Nuclear Power Plant accident in 2011, the radiocaesium, which flowed into the paddy fields via irrigation water, have been widely investigated. When the concentration of radiocaesium in the water samples containing suspended solids were directly measured using a high purity germanium detector with a 2 L marinelli beaker, the radiocaesium concentration might be overestimated due to the sedimentation of the suspended solids during the measurement time. In fact, the values obtained by the direct method were higher than those obtained by the filtering method and/or the gelling method in most of the agriculture-related water samples. We concluded that the gelling method using sodium polyacrylate can be widely adapted for the analysis of the total radiocaesium in the agriculture-related water samples because of its many advantage such as simple preparation procedure, accurate analysis values, excellent long-term stability of geometry and low operating cost. (author)

  10. Water - rock interaction in different rock environments

    International Nuclear Information System (INIS)

    Lamminen, S.

    1995-01-01

    The study assesses the groundwater geochemistry and geological environment of 44 study sites for radioactive waste disposal. Initially, the study sites were divided by rock type into 5 groups: (1) acid - intermediate rocks, (2) mafic - ultramafic rocks, (3) gabbros, amphibolites and gneisses that contain calc-silicate (skarn) rocks, (4) carbonates and (5) sandstones. Separate assessments are made of acid - intermediate plutonic rocks and of a subgroup that comprises migmatites, granite and mica gneiss. These all belong to the group of acid - intermediate rocks. Within the mafic -ultramafic rock group, a subgroup that comprises mafic - ultramafic plutonic rocks, serpentinites, mafic - ultramafic volcanic rocks and volcanic - sedimentary schists is also evaluated separately. Bedrock groundwaters are classified by their concentration of total dissolved solids as fresh, brackish, saline, strongly saline and brine-class groundwaters. (75 refs., 24 figs., 3 tabs.)

  11. Fatty Acid Detection in Mars-Analogous Rock Samples with the TMAH Wet Chemistry Experiment on the Sample Analysis at Mars (SAM) Instrument

    Science.gov (United States)

    Williams, A. J.; Eigenbrode, J. L.; Wilhelm, M. B.; Johnson, S. S.; Craft, K.; O'Reilly, S.; Lewis, J. M. T.; Williams, R.; Summons, R. E.; Benison, K. C.; Mahaffy, P. R.

    2017-12-01

    The Curiosity rover is exploring sedimentary rock sequences in Gale Crater for evidence of habitability and searching for organic compounds using the Sample Analysis at Mars (SAM) instrument suite. SAM includes a gas chromatograph mass spectrometer (GC-MS) and pyrolysis ovens. SAM has the ability to perform wet chemistry experiments, one of which uses tetramethylammonium hydroxide (TMAH) thermochemolysis to liberate bound lipids, making them sufficiently volatile for detection by GC-MS. To determine the effectiveness of the SAM-like TMAH experiment on fatty acid methyl ester (FAME) biomarker identification, rock and sediment samples were collected from a variety of Mars analog environments including iron oxides from a modern mineral precipitate and older surface gossan at Iron Mountain, CA, as well as modern acid salt and neutral lake sediments with mixed iron oxides and clays from Western Australia; siliceous sinter from recently inactive and modern near-vent Icelandic hot springs deposits; modern carbonate ooids from The Bahamas, and organic-rich shale from Germany. Samples underwent pyrolysis with TMAH. Fatty acids were analyzed by pyro-GC-MS using a SAM-like heating ramp (35°C/min) as well as a 500°C flash on a Frontier pyrolyzer and Agilent GC-MS instrument. Results reveal that FAMEs were detectable with the TMAH experiment in nearly all samples. Low molecular weight (MW) C6:0-C10:0 FAMEs were present in all samples, medium MW C11:0-C18:2 FAMEs were present in select samples, and high MW (HMW) C20:0-C30:0 FAMEs were present in the shale sample. Many of these samples exhibited an even-over-odd carbon number preference, indicating biological production. These experiments demonstrate that TMAH thermochemolysis with SAM-like pyro-GC-MS is effective in fatty acid analysis from natural Mars-analog samples that vary in mineralogy, age, and microbial community input. HMW FAMEs are not detected in iron-dominated samples, and may not be detectable at low

  12. EPA Method 3135.2I: Cyanide, Total and Amenable in Aqueous and Solid Samples Automated Colorimetric With Manual Digestion

    Science.gov (United States)

    This method describes procedures for preparation and analysis of solid, water and wipe samples for detection and measurement of cyanide amendable to chlorination using acid digestion and spectrophotometry.

  13. Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104

    International Nuclear Information System (INIS)

    Ross, G.A.

    1998-01-01

    A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method

  14. The Influence of Mark-Recapture Sampling Effort on Estimates of Rock Lobster Survival.

    Directory of Open Access Journals (Sweden)

    Ziya Kordjazi

    Full Text Available Five annual capture-mark-recapture surveys on Jasus edwardsii were used to evaluate the effect of sample size and fishing effort on the precision of estimated survival probability. Datasets of different numbers of individual lobsters (ranging from 200 to 1,000 lobsters were created by random subsampling from each annual survey. This process of random subsampling was also used to create 12 datasets of different levels of effort based on three levels of the number of traps (15, 30 and 50 traps per day and four levels of the number of sampling-days (2, 4, 6 and 7 days. The most parsimonious Cormack-Jolly-Seber (CJS model for estimating survival probability shifted from a constant model towards sex-dependent models with increasing sample size and effort. A sample of 500 lobsters or 50 traps used on four consecutive sampling-days was required for obtaining precise survival estimations for males and females, separately. Reduced sampling effort of 30 traps over four sampling days was sufficient if a survival estimate for both sexes combined was sufficient for management of the fishery.

  15. The Influence of Mark-Recapture Sampling Effort on Estimates of Rock Lobster Survival

    Science.gov (United States)

    Kordjazi, Ziya; Frusher, Stewart; Buxton, Colin; Gardner, Caleb; Bird, Tomas

    2016-01-01

    Five annual capture-mark-recapture surveys on Jasus edwardsii were used to evaluate the effect of sample size and fishing effort on the precision of estimated survival probability. Datasets of different numbers of individual lobsters (ranging from 200 to 1,000 lobsters) were created by random subsampling from each annual survey. This process of random subsampling was also used to create 12 datasets of different levels of effort based on three levels of the number of traps (15, 30 and 50 traps per day) and four levels of the number of sampling-days (2, 4, 6 and 7 days). The most parsimonious Cormack-Jolly-Seber (CJS) model for estimating survival probability shifted from a constant model towards sex-dependent models with increasing sample size and effort. A sample of 500 lobsters or 50 traps used on four consecutive sampling-days was required for obtaining precise survival estimations for males and females, separately. Reduced sampling effort of 30 traps over four sampling days was sufficient if a survival estimate for both sexes combined was sufficient for management of the fishery. PMID:26990561

  16. On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yebra, M.C.; Moreno-Cid, A.

    2003-01-01

    Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g -1 manganese (dry mass). The detection limit is 0.4 μg g -1 (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples

  17. Sample-size effects in fast-neutron gamma-ray production measurements: solid-cylinder samples

    International Nuclear Information System (INIS)

    Smith, D.L.

    1975-09-01

    The effects of geometry, absorption and multiple scattering in (n,Xγ) reaction measurements with solid-cylinder samples are investigated. Both analytical and Monte-Carlo methods are employed in the analysis. Geometric effects are shown to be relatively insignificant except in definition of the scattering angles. However, absorption and multiple-scattering effects are quite important; accurate microscopic differential cross sections can be extracted from experimental data only after a careful determination of corrections for these processes. The results of measurements performed using several natural iron samples (covering a wide range of sizes) confirm validity of the correction procedures described herein. It is concluded that these procedures are reliable whenever sufficiently accurate neutron and photon cross section and angular distribution information is available for the analysis. (13 figures, 5 tables) (auth)

  18. Improved Rock Core Sample Break-off, Retention and Ejection System, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The proposed effort advances the design of an innovative core sampling and acquisition system with improved core break-off, retention and ejection features. The...

  19. Improved Rock Core Sample Break-off, Retention and Ejection System, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The proposed effort advances the design of an innovative core sampling and acquisition system with improved core break-off, retention and ejection features. Phase 1...

  20. Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

    Science.gov (United States)

    Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

    2018-04-01

    This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Discrete element method (DEM) simulations of stratified sampling during solid dosage form manufacturing.

    Science.gov (United States)

    Hancock, Bruno C; Ketterhagen, William R

    2011-10-14

    Discrete element model (DEM) simulations of the discharge of powders from hoppers under gravity were analyzed to provide estimates of dosage form content uniformity during the manufacture of solid dosage forms (tablets and capsules). For a system that exhibits moderate segregation the effects of sample size, number, and location within the batch were determined. The various sampling approaches were compared to current best-practices for sampling described in the Product Quality Research Institute (PQRI) Blend Uniformity Working Group (BUWG) guidelines. Sampling uniformly across the discharge process gave the most accurate results with respect to identifying segregation trends. Sigmoidal sampling (as recommended in the PQRI BUWG guidelines) tended to overestimate potential segregation issues, whereas truncated sampling (common in industrial practice) tended to underestimate them. The size of the sample had a major effect on the absolute potency RSD. The number of sampling locations (10 vs. 20) had very little effect on the trends in the data, and the number of samples analyzed at each location (1 vs. 3 vs. 7) had only a small effect for the sampling conditions examined. The results of this work provide greater understanding of the effect of different sampling approaches on the measured content uniformity of real dosage forms, and can help to guide the choice of appropriate sampling protocols. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Chemical Data for Rock, Sediment, Biological, Precipitate, and Water Samples from Abandoned Copper Mines in Prince William Sound, Alaska

    Science.gov (United States)

    Koski, Randolph A.; Munk, LeeAnn

    2007-01-01

    In the early 20th century, approximately 6 million metric tons of copper ore were mined from numerous deposits located along the shorelines of fjords and islands in Prince William Sound, Alaska. At the Beatson, Ellamar, and Threeman mine sites (fig. 1), rocks containing Fe, Cu, Zn, and Pb sulfide minerals are exposed to chemical weathering in abandoned mine workings and remnant waste piles that extend into the littoral zone. Field investigations in 2003 and 2005 as well as analytical data for rock, sediment, precipitate, water, and biological samples reveal that the oxidation of sulfides at these sites is resulting in the generation of acid mine drainage and the transport of metals into the marine environment (Koski and others, 2008; Stillings and others, 2008). At the Ellamar and Threeman sites, plumes of acidic and metal-enriched water are flowing through beach gravels into the shallow offshore environment. Interstitial water samples collected from beach sediment at Ellamar have low pH levels (to ~3) and high concentrations of metals including iron, copper, zinc, cobalt, lead, and mercury. The abundant precipitation of the iron sulfate mineral jarosite in the Ellamar gravels also signifies a low-pH environment. At the Beatson mine site (the largest copper mine in the region) seeps containing iron-rich microbial precipitates drain into the intertidal zone below mine dumps (Foster and others, 2008). A stream flowing down to the shoreline from underground mine workings at Beatson has near-neutral pH, but elevated levels of zinc, copper, and lead (Stillings and others, 2008). Offshore sediment samples at Beatson are enriched in these metals. Preliminary chemical data for tissue from marine mussels collected near the Ellamar, Threeman, and Beatson sites reveal elevated levels of copper, zinc, and lead compared to tissue in mussels from other locations in Prince William Sound (Koski and others, 2008). Three papers presenting results of this ongoing investigation of

  3. Eosinophilia in routine blood samples as a biomarker for solid tumor development

    DEFF Research Database (Denmark)

    Andersen, Christen Bertel L; Siersma, V.D.; Hasselbalch, H.C.

    2014-01-01

    eosinophilia in routine blood samples as a potential biomarker of solid tumor development in a prospective design. MATERIAL AND METHODS: From the Copenhagen Primary Care Differential Count (CopDiff) Database, we identified 356 196 individuals with at least one differential cell count (DIFF) encompassing...... was increased with mild eosinophilia [OR 1.93 (CI 1.29-2.89), p = 0.0013]. No associations with eosinophilia were observed for the remaining solid cancers. CONCLUSION: We demonstrate that eosinophilia in routine blood samples associates with an increased risk of bladder cancer. Our data emphasize...... that additional preclinical studies are needed in order to shed further light on the role of eosinophils in carcinogenesis, where it is still unknown whether the cells contribute to tumor immune surveillance or neoplastic evolution....

  4. Precise simultaneous determination of zirconium and hafnium in silicate rocks, meteorites and lunar samples. [Neutron reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, P A; Garg, A N; Ehmann, W D [Kentucky Univ., Lexington (USA). Dept. of Chemistry

    1977-01-01

    A precise, sensitive and rapid analytical technique has been developed for the simultaneous determination of Zr and Hf in natural silicate matrices. The technique is based on radiochemical neutron activation analysis and employs a rapid fusion dissolution of the sample and simultaneous precipitation of the Zr-Hf pair with p-hydroxybenzene arsenic acid in an acidic medium. The indicator radionuclides, /sup 95/Zr and /sup 181/Hf, are counted and the /sup 95/Zr activity is corrected for the contribution from U fission. The chemical yields of the radiochemical separation are based on Hf carrier. The yield is determined by reactivation of the processed samples and standards with a /sup 252/Cf isotopic neutron source and by counting the 18.6 sec half-life sup(179m)Hf. The RNAA procedure for Zr and Hf has been shown to be precise and accurate for natural silicate samples, based on replicate analyses of samples containing Zr in the range of 1 ..mu..g/g to over 600 ..mu..g/g. The procedure is relatively rapid with a total chemical processing time of approximately 3 hours. At least 4 samples are processed simultaneously. Ten additional elements (Fe, Cr, Co, Sc, Eu, La, Lu, Ce, Th and Tb) can be determined by direct Ge(Li) spectrometry (INAA) on the samples prior to dissolution for the RNAA determination of Zr and Hf. Corrections for the U fission contribution can be made on the basis of the known U content or from the INAA Th content, based on the relatively constant natural Th/U ratio.

  5. Assessment of Metaborate Fusion for the Rapid Dissolution of Solid Samples: Suitability with the Northstar ARSIIe

    Science.gov (United States)

    2016-07-01

    5 Table 3. Residual Silicates avec Flocculation in Glass Beaker or Polyethylene Cone ................ 8 Table 4...is formed. Since the concentration of silicates in soil or sediment is high (up to 70-75% in silicon dioxide ( SiO2 ) in some cases), the condensation...flux, for the fusion of acidic samples such as solids containing a significant portion of SiO2 . Conversely, lithium tetraborate, an acidic flux, will

  6. Organic petrology and Rock-Eval characteristics in selected surficial samples of the Tertiary Formation, South Sumatra Basin

    Directory of Open Access Journals (Sweden)

    M. H. Hermiyanto

    2014-06-01

    Full Text Available http://dx.doi.org/10.17014/ijog.vol4no3.20096Organic petrologic data of the DOM of Talangakar and Muaraenim Formations show that the organic matter consisting mainly of vitrinite group is essentially composed of telocollinite (1.0 – 70.8 % and desmocollinite (0.8 – 66.6 % with minor telinite (0.6 – 9.4 %, detrovitrinite (0.6 – 6.0 %, and cor- pocollinite (0.6 – 2.0 %. Minor exinite (0.4 – 7.8 % and inertinite (0.4 – 8.0 % are also determined. However, mineral matter varies from 0.6 – 99.44 %. Downwards, the increase in vitrinite reflectance (0.33 – 0.48 % is concomitant with the depth of each formation. Furthermore, based on Rock-eval pyrolysis, TOC value of the Talangakar Formation ranges from 0.09 – 15.38 %, Gumai 0.34 – 0.39 %, Airbenakat 0.32 – 4.82 %, and Muaraenim between 0.08 – 15.22 %. Moreover the PY (Potential Yield value variation of the Talangakar, Gumai, Airbenakat, and Muaraenim Formations are between 0.04 – 36.61 mg HC/g rock, 0.53 – 0.81 mg HC/g rock, 0.1 – 4.37 mg HC/g rock, and 0.07 – 129.8 mg HC/g rock respectively. Therefore, on the basis of those two parameters, the four formations are included into a gas - oil prone source rock potential. However, the Talangakar and Muaraenim Formations are poor to excellent category, whereas the Air Benakat tends to indicate a poor – fair category and Gumai Formation are only within a poor category. Tmax value of the Talangakar ranges from 237 – 4380 C, Gumai 316 – 3590 C, Airbenakat 398 – 4340 C with exceptions of 4970 C and 5180 C, and Muaraenim Forma- tions 264 – 4250 C. The Talangakar Formation contains kerogen Type II dan III, with the HI (Hydrogen Index value varies from 45.16 – 365.43. However two samples show value of 0. The organic content of the Gumai and Air Benakat Formations are included into kerogen type III, with HI value ranges from11.87 – 40.82, and 19 – 114 respectively. Moreover the Muaraenim Formation has two category of

  7. A contact method of determination of thermophysical properties of rocks from core samples

    International Nuclear Information System (INIS)

    Gavril'ev, R.I.

    1995-01-01

    The zone of the action of thermal disturbances around a circular heat source on the surface of a semi-infinite body is estimated with the aim of using contact methods of determination of thermophysical properties of materials from core samples

  8. Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

    Science.gov (United States)

    Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

    2015-05-11

    In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

  9. The correlations between natural elements (K, U, Th) concentrations and thermal neutron absorption cross-section value (Σa) for rock samples of Carpatia area

    International Nuclear Information System (INIS)

    Swakon, J.; Cywicka-Jakiel, T.; Drozdowicz, E.; Gabanska, B.; Loskiewicz, J.; Woznicka, U.

    1991-01-01

    The paper presents a study of correlations between concentrations of potassium, uranium and thorium and thermal neutron absorption cross section in rock samples. This knowledge of correlation should help in recognizing the expansion ways and accumulation places of the elements responsible of high thermal neutron absorption cross section in some geological environments. The correlations show the existence of connections between the thermal neutron absorption cross section value and natural radioactivity elements concentration in rocks. The results confirm the existence of correlations between natural radioactive elements concentrations (particularly thorium) and thermal neutron absorption cross - section value in some rocks. (author). 12 refs, 23 figs, 6 tabs

  10. Evaluation of the readsorption of plutonium and americium in dynamic fractionations of environmental solid samples

    DEFF Research Database (Denmark)

    Petersen, Roongrat; Hou, Xiaolin; Hansen, Elo Harald

    2008-01-01

    A dynamic extraction system exploiting sequential injection (SI) for sequential extractions incorporating a specially designed extraction column is developed to fractionate radionuclides in environmental solid samples such as soils and sediments. The extraction column can contain a large amount...... of soil sample (up to 5 g), and under optimal operational conditions it does not give rise to creation of back pressure. Attention has been placed on studies of the readsorption problems during sequential extraction using a modified Standards, Measurements and Testing (SM&T) scheme with 4-step sequential...

  11. Solid Phase Characterization Of Heel Samples From Tank 241-C-110

    International Nuclear Information System (INIS)

    Page, J.S.; Cooke, G.A.; Pestovich, J.A.; Huber, H.J.

    2011-01-01

    During sluicing operations of tank 241-C-110, a significant amount of solids were unable to be retrieved. These solids (often referred to as the tank 'heel') were sampled in 2010 and chemically and mineralogically analyzed in the 222-S Laboratory. Additionally, dissolution tests were performed to identify the amount of undissolvable material after using multiple water contacts. This report covers the solid phase characterization of six samples from these tests using scanning electron microscopy, polarized light microscopy, and X-ray diffraction. The chemical analyses, particle size distribution analysis, and dissolution test results are reported separately. Two of the samples were from composites created from as-received material - Composite A and Composite B. The main phase in these samples was sodium-fluoride-phosphate hydrate (natrophosphate) - in the X-ray diffraction spectra, this phase was the only phase identifiable. Polarized light microscopy showed the presence of minor amounts of gibbsite and other phases. These phases were identified by scanning electron microscopy - energy dispersive X-ray spectroscopy as sodium aluminosilicates, sodium diuranate, and sodium strontium phosphate hydrate (nastrophite) crystals. The natrophosphate crystals in the scanning electron microscopy analysis showed a variety of erosive and dissolution features from perfectly shaped octahedral to well-rounded appearance. Two samples were from water-washed Composites A and B, with no change in mineralogy compared to the as-received samples. This is not surprising, since the water wash had only a short period of water contact with the material as opposed to the water dissolution tests. The last two samples were residual solids from the water dissolution tests. These tests included multiple additions of water at 15 C and 45 C. The samples were sieved to separate a coarser fraction of > 710 μm and a finer fraction of < 710 μm. These two fractions were analyzed separately. The coarser

  12. Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 101

    International Nuclear Information System (INIS)

    Diaz, L.A.

    1998-01-01

    One waste sample that was obtained with solids from tank 101 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprene tubing (Phthalate free) was obtained in a glass jar with teflon lid was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Results are presented

  13. Mercury speciation in environmental solid samples using thermal release technique with atomic absorption detection

    Energy Technology Data Exchange (ETDEWEB)

    Shuvaeva, Olga V. [Institute of Inorganic Chemistry, Academician Lavrent' ev Prospect 3, 630090 Novosbirsk (Russian Federation)], E-mail: olga@che.nsk.su; Gustaytis, Maria A.; Anoshin, Gennadii N. [Institute of Geology and Mineralogy, Siberian Branch of Russian Academy of Sciences, Koptyug Prospect 3, 630090 Novosibirsk (Russian Federation)

    2008-07-28

    A sensitive and very simple method for determination of mercury species in solid samples has been developed involving thermal release analysis in combination with atomic absorption (AAS) detection. The method allows determination of mercury(II) chloride, methylmercury and mercury sulfide at the level of 0.70, 0.35 and 0.20 ng with a reproducibility of the results of 14, 25 and 18%, respectively. The accuracy of the developed assay has been estimated using certified reference materials and by comparison of the results with those of an independent method. The method has been applied for Hg species determination in original samples of lake sediments and plankton.

  14. Digitally Available Interval-Specific Rock-Sample Data Compiled from Historical Records, Nevada Test Site and Vicinity, Nye County, Nevada.

    Energy Technology Data Exchange (ETDEWEB)

    David B. Wood

    2007-10-24

    Between 1951 and 1992, 828 underground tests were conducted on the Nevada Test Site, Nye County, Nevada. Prior to and following these nuclear tests, holes were drilled and mined to collect rock samples. These samples are organized and stored by depth of borehole or drift at the U.S. Geological Survey Core Library and Data Center at Mercury, Nevada, on the Nevada Test Site. From these rock samples, rock properties were analyzed and interpreted and compiled into project files and in published reports that are maintained at the Core Library and at the U.S. Geological Survey office in Henderson, Nevada. These rock-sample data include lithologic descriptions, physical and mechanical properties, and fracture characteristics. Hydraulic properties also were compiled from holes completed in the water table. Rock samples are irreplaceable because pre-test, in-place conditions cannot be recreated and samples cannot be recollected from the many holes destroyed by testing. Documenting these data in a published report will ensure availability for future investigators.

  15. Digitally Available Interval-Specific Rock-Sample Data Compiled from Historical Records, Nevada Test Site and Vicinity, Nye County, Nevada

    Energy Technology Data Exchange (ETDEWEB)

    David B. Wood

    2009-10-08

    Between 1951 and 1992, underground nuclear weapons testing was conducted at 828 sites on the Nevada Test Site, Nye County, Nevada. Prior to and following these nuclear tests, holes were drilled and mined to collect rock samples. These samples are organized and stored by depth of borehole or drift at the U.S. Geological Survey Core Library and Data Center at Mercury, Nevada, on the Nevada Test Site. From these rock samples, rock properties were analyzed and interpreted and compiled into project files and in published reports that are maintained at the Core Library and at the U.S. Geological Survey office in Henderson, Nevada. These rock-sample data include lithologic descriptions, physical and mechanical properties, and fracture characteristics. Hydraulic properties also were compiled from holes completed in the water table. Rock samples are irreplaceable because pre-test, in-place conditions cannot be recreated and samples cannot be recollected from the many holes destroyed by testing. Documenting these data in a published report will ensure availability for future investigators.

  16. Effect of mineral constituents in the bioleaching of uranium from uraniferous sedimentary rock samples, Southwestern Sinai, Egypt

    International Nuclear Information System (INIS)

    Amin, Maisa M.; Elaassy, Ibrahim E.; El-Feky, Mohamed G.; Sallam, Abdel Sattar M.; Talaat, Mona S.; Kawady, Nilly A.

    2014-01-01

    Bioleaching, like Biotechnology uses microorganisms to extract metals from their ore materials, whereas microbial activity has an appreciable effect on the dissolution of toxic metals and radionuclides. Bioleaching of uranium was carried out with isolated fungi from uraniferous sedimentary rocks from Southwestern Sinai, Egypt. Eight fungal species were isolated from different grades of uraniferous samples. The bio-dissolution experiments showed that Aspergillus niger and Aspergillus terreus exhibited the highest leaching efficiencies of uranium from the studied samples. Through monitoring the bio-dissolution process, the uranium grade and mineralogic constituents of the ore material proved to play an important role in the bioleaching process. The tested samples asserted that the optimum conditions of uranium leaching are: 7 days incubation time, 3% pulp density, 30 °C incubation temperature and pH 3. Both fungi produced the organic acids, namely; oxalic, acetic, citric, formic, malonic, galic and ascorbic in the culture filtrate, indicating an important role in the bioleaching processes. - Highlights: • Aspergillus niger and Aspergillus terreus are the only isolates achieved highest leaching efficiency of uranium from the studied samples. • Bioleaching process directly related to variations in mineral constituents and uranium grades. • The optimum conditions of uranium bioleaching from its ores, were found to be 7 days, 3% pulp density, pH 3 and 30 °C. • A. niger and A. terreus organic acids play an important and effective role for uranium leaching process

  17. An integrated rock magnetic and EPR study in soil samples from a hydrocarbon prospective area

    Science.gov (United States)

    González, F.; Aldana, M.; Costanzo-Álvarez, V.; Díaz, M.; Romero, I.

    Magnetic susceptibility (MS) and organic matter free radical concentration (OMFRC) determined by electron paramagnetic resonance, have been measured in soil samples (≈1.5 m depth) from an oil prospective area located at the southern flank of the Venezuelan Andean Range. S-ratios close to 1, as well as high temperature susceptibility analyses, reveal magnetite as the chief magnetic phase in most of these samples. Ethane concentrations, MS and OMFRC normalized data have been plotted against the relative position of 22 sampling sites sequentially arranged from north to south. Although there is not a linear correlation between MS and OMFRC data, these two profiles seem to vary in like fashion. A MS and OMFRC southern anomaly coincides with the zone of highest ethane concentration that overlies a “Cretaceous kitchen”. OMFRC highs could be linked to the degradation or alteration of organic matter, the possible result of hydrocarbon gas leakage, whose surface expression is the stressed fern observed by remote sensing studies previously performed in the area. Ethane anomalies are associated to this seepage that also produces changes in the magnetic mineralogies detected as MS positive anomalies.

  18. Numerical modelling of fracture initiation and propagation in biaxial tests on rock samples

    CSIR Research Space (South Africa)

    Van de Steen, B

    2001-03-01

    Full Text Available and Peirce, 1995). Additional edges can be obtained in the Voronoi tessellation, by connecting the geometric centre of the Voronoi polygons with the vertices of the polygons. These last elements are further referred to as the internal fracture paths, while... samples without flaws therefore display a very brittle behaviour (Napier and Peirce, 1995). To obtain a more plastic behaviour, it may be necessary to adjust the flaw density as well (D0 to D0b, Table 2). The brittleness of the simulated biaxial tests...

  19. Uranium favorability of tertiary sedimentary rocks of the Pend Oreille River valley, Washington. [Measurement and sampling of surface sections, collection of samples from isolated outcrops, chemical and mineralogical analyses of samples, and examination of available water logs

    Energy Technology Data Exchange (ETDEWEB)

    Marjaniemi, D.K.; Robins, J.W.

    1975-08-01

    Tertiary sedimentary rocks in the Pend Oreille River valley were investigated in a regional study to determine the favorability for potential uranium resources of northeastern Washington. This project involved measurement and sampling of surface sections, collection of samples from isolated outcrops, chemical and mineralogical analyses of samples, and examination of available water well logs. The Box Canyon Dam area north of Ione is judged to have very high favorability. Thick-bedded conglomerates interbedded with sandstones and silty sandstones compose the Tiger Formation in this area, and high radioactivity levels are found near the base of the formation. Uranophane is found along fracture surfaces or in veins. Carbonaceous material is present throughout the Tiger Formation in the area. Part of the broad Pend Oreille valley surrounding Cusick, Washington, is an area of high favorability. Potential host rocks in the Tiger Formation, consisting of arkosic sandstones interbedded with radioactive shales, probably extend throughout the subsurface part of this area. Carbonaceous material is present and some samples contain high concentrations of uranium. In addition, several other possible chemical indicators were found. The Tiger-Lost Creek area is rated as having medium favorability. The Tiger Formation contains very hard, poorly sorted granite conglomerate with some beds of arkosic sandstone and silty sandstone. The granite conglomerate was apparently derived from source rocks having relatively high uranium content. The lower part of the formation is more favorable than the upper part because of the presence of carbonaceous material, anomalously high concentrations of uranium, and other possible chemical indicators. The area west of Ione is judged to have low favorability, because of the very low permeability of the rocks and the very low uranium content. (auth)

  20. Rock Physics

    DEFF Research Database (Denmark)

    Fabricius, Ida Lykke

    2017-01-01

    Rock physics is the discipline linking petrophysical properties as derived from borehole data to surface based geophysical exploration data. It can involve interpretation of both elastic wave propagation and electrical conductivity, but in this chapter focus is on elasticity. Rock physics is based...... on continuum mechanics, and the theory of elasticity developed for statics becomes the key to petrophysical interpretation of velocity of elastic waves. In practice, rock physics involves interpretation of well logs including vertical seismic profiling (VSP) and analysis of core samples. The results...

  1. Experimental study on deformation field evolution in rock sample with en echelon faults using digital speckle correlation method

    Science.gov (United States)

    Ma, S.; Ma, J.; Liu, L.; Liu, P.

    2007-12-01

    Digital speckle correlation method (DSCM) is one kind of photomechanical deformation measurement method. DSCM could obtain continuous deformation field contactlessly by just capturing speckle images from specimen surface. Therefore, it is suitable to observe high spatial resolution deformation field in tectonophysical experiment. However, in the general DSCM experiment, the inspected surface of specimen needs to be painted to bear speckle grains in order to obtain the high quality speckle image. This also affects the realization of other measurement techniques. In this study, an improved DSCM system is developed and utilized to measure deformation field of rock specimen without surface painting. The granodiorite with high contrast nature grains is chosen to manufacture the specimen, and a specially designed DSCM algorithm is developed to analyze this kind of nature speckle images. Verification and calibration experiments show that the system could inspect a continuous (about 15Hz) high resolution displacement field (with resolution of 5μm) and strain field (with resolution of 50μɛ), dispensing with any preparation on rock specimen. Therefore, it could be conveniently utilized to study the failure of rock structure. Samples with compressive en echelon faults and extensional en echelon faults are studied on a two-direction servo-control test machine. The failure process of the samples is discussed based on the DSCM results. Experiment results show that: 1) The contours of displacement field could clearly indicate the activities of faults and new cracks. The displacement gradient adjacent to active faults and cracks is much greater than other areas. 2) Before failure of the samples, the mean strain of the jog area is largest for the compressive en echelon fault, while that is smallest for the extensional en echelon fault. This consists with the understanding that the jog area of compressive fault subjects to compression and that of extensional fault subjects to

  2. Effect of mineral constituents in the bioleaching of uranium from uraniferous sedimentary rock samples, Southwestern Sinai, Egypt.

    Science.gov (United States)

    Amin, Maisa M; Elaassy, Ibrahim E; El-Feky, Mohamed G; Sallam, Abdel Sattar M; Talaat, Mona S; Kawady, Nilly A

    2014-08-01

    Bioleaching, like Biotechnology uses microorganisms to extract metals from their ore materials, whereas microbial activity has an appreciable effect on the dissolution of toxic metals and radionuclides. Bioleaching of uranium was carried out with isolated fungi from uraniferous sedimentary rocks from Southwestern Sinai, Egypt. Eight fungal species were isolated from different grades of uraniferous samples. The bio-dissolution experiments showed that Aspergillus niger and Aspergillus terreus exhibited the highest leaching efficiencies of uranium from the studied samples. Through monitoring the bio-dissolution process, the uranium grade and mineralogic constituents of the ore material proved to play an important role in the bioleaching process. The tested samples asserted that the optimum conditions of uranium leaching are: 7 days incubation time, 3% pulp density, 30 °C incubation temperature and pH 3. Both fungi produced the organic acids, namely; oxalic, acetic, citric, formic, malonic, galic and ascorbic in the culture filtrate, indicating an important role in the bioleaching processes. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Receiver calibration and the nonlinearity parameter measurement of thick solid samples with diffraction and attenuation corrections.

    Science.gov (United States)

    Jeong, Hyunjo; Barnard, Daniel; Cho, Sungjong; Zhang, Shuzeng; Li, Xiongbing

    2017-11-01

    This paper presents analytical and experimental techniques for accurate determination of the nonlinearity parameter (β) in thick solid samples. When piezoelectric transducers are used for β measurements, the receiver calibration is required to determine the transfer function from which the absolute displacement can be calculated. The measured fundamental and second harmonic displacement amplitudes should be modified to account for beam diffraction and material absorption. All these issues are addressed in this study and the proposed technique is validated through the β measurements of thick solid samples. A simplified self-reciprocity calibration procedure for a broadband receiver is described. The diffraction and attenuation corrections for the fundamental and second harmonics are explicitly derived. Aluminum alloy samples in five different thicknesses (4, 6, 8, 10, 12cm) are prepared and β measurements are made using the finite amplitude, through-transmission method. The effects of diffraction and attenuation corrections on β measurements are systematically investigated. When diffraction and attenuation corrections are all properly made, the variation of β between different thickness samples is found to be less than 3.2%. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

    DEFF Research Database (Denmark)

    Edjabou, Vincent Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona

    2015-01-01

    Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both...... comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub......-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10-50 waste fractions, organised according to a three-level (tiered approach) facilitating,comparison of the waste data between individual sub-areas with different fractionation (waste...

  5. Rapid determination of trace level copper in tea infusion samples by solid contact ion selective electrode

    Directory of Open Access Journals (Sweden)

    Aysenur Birinci

    2016-07-01

    Full Text Available A new solid contact copper selective electrode with a poly (vinyl chloride (PVC membrane consisting of o-xylylenebis(N,N-diisobutyldithiocarbamate as ionophore has been prepared. The main novelties of constructed ion selective electrode concept are the enhanced robustness, cheapness, and fastness due to the use of solid contacts. The electrode exhibits a rapid (< 10 seconds and near-Nernstian response to Cu2+ activity from 10−1 to 10−6 mol/L at the pH range of 4.0–6.0. No serious interference from common ions was found. The electrode characterizes by high potential stability, reproducibility, and full repeatability. The electrode was used as an indicator electrode in potentiometric titration of Cu(II ions with EDTA and for the direct assay of tea infusion samples by means of the calibration graph technique. The results compared favorably with those obtained by the atomic absorption spectroscopy (AAS.

  6. Rollerjaw Rock Crusher

    Science.gov (United States)

    Peters, Gregory; Brown, Kyle; Fuerstenau, Stephen

    2009-01-01

    The rollerjaw rock crusher melds the concepts of jaw crushing and roll crushing long employed in the mining and rock-crushing industries. Rollerjaw rock crushers have been proposed for inclusion in geological exploration missions on Mars, where they would be used to pulverize rock samples into powders in the tens of micrometer particle size range required for analysis by scientific instruments.

  7. New color-photographic observation of thermoluminescence from sliced rock samples

    International Nuclear Information System (INIS)

    Hashimoto, Tetsuo; Kimura, Kenichi; Koyanagi, Akira; Takahashi, Kuniaki; Sotobayashi, Takeshi

    1983-01-01

    New observation technique has been established for the thermoluminescence photography using extremely high-sensitive color films. Considering future application to the geological fields, a granite was selected as a testing material. The sliced specimens (0.5--0.7 mm in thickness), which were irradiated with a 60 Co source, were mounted on the heater attached with a thermocouple, which was connected to a microcomputer for measuring the temperature. The samples were heated in the temperature range of 80--400 0 C by operating the camera-shutter controlled with the microcomputer. Four commercially available films (Kodak-1000(ASA), -400, Sakura-400, Fuji-400) could give apparently detectable color-images of artificial thermoluminescence above a total absorbed dose of 880 Gy(88 krad). The specimens, irradiated upto 8.4 kGy(840krad), allowed easily to distinguish the distinct appearance of the thermoluminescence images depending on kinds of white mineral constituents. Moreover, such color images were changeable with the heating temperature. Sakura-400 film has proved the most colorful images from aspects of color tone although Kodak-1000 film showed the highest sensitivity. By applying this Kodak-1000, it was found that the characteristic color image due to natural thermoluminescence was significantly observed on the Precambrian granite which was exposed with natural radiation alone since its formation. This simple and interesting technique, obtainable surface information reflecting impurities and local crystal defects in addition to small mineral constituents, was named as the thermoluminescence color imaging (abbreviated to TLCI) technique by the authors and its versatile applications were discussed. (author)

  8. Detection of fission fragments using thick samples in contact with solid state nuclear track detectors

    International Nuclear Information System (INIS)

    Lima, D.A. de; Martins, J.B.; Tavares, O.A.P.

    1987-01-01

    Whenever use is made of thick samples in contact with solid state nuclear track detectors for determining fission yields, one of the fundamental problems is the evaluation of the effective number of target nuclei which contributes to the fraction of the number of fission events that will be recorded. The evaluation of the effective number of target nuclei which contributes to recorded events is based on the effective thickness of the sample. A method for evaluating effective thickness of thick samples for binary fission modes, is presented. A cross section equation which takes into account all the necessary corrections due to fragment attenuation effects by a thick target for calculation induced fission yields, was obtained. (Author) [pt

  9. Sampling, characterisation and processing of solid recovered fuel production from municipal solid waste: An Italian plant case study.

    Science.gov (United States)

    Ranieri, Ezio; Ionescu, Gabriela; Fedele, Arcangela; Palmieri, Eleonora; Ranieri, Ada Cristina; Campanaro, Vincenzo

    2017-08-01

    This article presents the classification of solid recovered fuel from the Massafra municipal solid waste treatment plant in Southern Italy in compliancy with the EN 15359 standard. In order to ensure the reproducibility of this study, the characterisation methods of waste input and output flow, the mechanical biological treatment line scheme and its main parameters for each stage of the processing chain are presented in details, together with the research results in terms of mass balance and derived fuel properties. Under this study, only 31% of refused municipal solid waste input stream from mechanical biological line was recovered as solid recovered fuel with a net heating value (NC=HV) average of 15.77 MJ kg -1 ; chlorine content average of 0.06% on a dry basis; median of mercury solid recovered fuel produced meets the European Union standard requirements and can be classified with the class code: Net heating value (3); chlorine (1); mercury (1).

  10. Determination of Pu isotopic composition and 241Am by high resolution gamma spectrometry on solid samples

    International Nuclear Information System (INIS)

    Sarkar, Arnab; Paul, Sumana; Aggarwal, Suresh K.; Tomar, Bhupendra S.

    2011-08-01

    The present report gives a detailed account of the development of non-destructive assay technique using high resolution gamma-ray spectrometry (HRGS) for determination of plutonium (Pu) isotopic composition and the 241 Am content in solid Pu samples. Energy range 120-420 keV was used in this study. The methodology involves in situ relative efficiency calibration during the measurement process itself, to reduce the errors and increase the reliability of the method. Twenty solid Pu samples of power reactor and research reactor grade were analyzed by this method and the results were compared with those obtained by thermal ionization mass spectrometry. The accuracy of the final results depends strongly upon the accuracy of the available nuclear data (decay constant, gamma abundance etc.). MATLAB based programme was written to perform the analysis. A counting time of 4 hour was chosen for achieving good statistics on the results for samples having 100-200 mg of Pu. The attainable accuracy is found to be 0.5-1% for the fissile isotopes ( 239 Pu + 241 Pu) and 5-10% for 241 Am content. (author)

  11. Solid Sampling with a Diode Laser for Portable Ambient Mass Spectrometry.

    Science.gov (United States)

    Yung, Yeni P; Wickramasinghe, Raveendra; Vaikkinen, Anu; Kauppila, Tiina J; Veryovkin, Igor V; Hanley, Luke

    2017-07-18

    A hand-held diode laser is implemented for solid sampling in portable ambient mass spectrometry (MS). Specifically, a pseudocontinuous wave battery-powered surgical laser diode is employed for portable laser diode thermal desorption (LDTD) at 940 nm and compared with nanosecond pulsed laser ablation at 2940 nm. Postionization is achieved in both cases using atmospheric pressure photoionization (APPI). The laser ablation atmospheric pressure photoionization (LAAPPI) and LDTD-APPI mass spectra of sage leaves (Salvia officinalis) using a field-deployable quadrupole ion trap MS display many similar ion peaks, as do the mass spectra of membrane grown biofilms of Pseudomonas aeruginosa. These results indicate that LDTD-APPI method should be useful for in-field sampling of plant and microbial communities, for example, by portable ambient MS. The feasibility of many portable MS applications is facilitated by the availability of relatively low cost, portable, battery-powered diode lasers. LDTD could also be coupled with plasma- or electrospray-based ionization for the analysis of a variety of solid samples.

  12. Comparison of hot hydroxylamine hydrochloride and oxalic acid leaching of stream sediment and coated rock samples as anomaly enhancement techniques

    Science.gov (United States)

    Filipek, L.H.; Chao, T.T.; Theobald, P.K.

    1982-01-01

    A hot hydroxylamine hydrochloride (H-Hxl) extraction in 25% acetic acid is compared with the commonly used oxalic acid extraction as a method of anomaly enhancement for Cu and Zn in samples from two very different metal deposits and climatic environments. Results obtained on minus-80-mesh stream sediments from an area near the Magruder massive sulfide deposit in Lincoln County, Georgia, where the climate is humid subtropical, indicate that H-Hxl enhances the anomaly for Cu by a factor of 2 and for Zn by a factor of 1.5, compared to the oxalic method. Analyses of Fe oxide-coated rock samples from outcrops overlying the North Silver Bell porphyry copper deposit near Tucson, Arizona, where the climate is semi-arid to arid, indicate that both techniques effectively outline the zones of hydrothermal alteration. The H-Hxl extraction can also perform well in high-carbonate or high-clay environments, where other workers have suggested that oxalic acid is not very effective. Therefore, the H-Hxl method is recommended for general exploration use. ?? 1982.

  13. Solubility and sorption characteristics of uranium(VI) associated with rock samples and brines/groundwaters from WIPP and NTS

    International Nuclear Information System (INIS)

    Dosch, R.G.

    1981-01-01

    Solubility measurements for U(VI) in WIPP-related brines/groundwaters were made using initial U(VI) concentrations in the range of 1 to 50 μg/ml. Distribution coefficients (Kd) for U(VI) were determined for Culebra and Magenta dolomites using four different brine/groundwater compositions and for argillaceous shale and hornfels samples from the Eleana and Calico Hills Formation on NTS using a groundwater simulant typical of that area. The Kd's were evaluated as functions of: (1) U(VI) concentration (1.4 x 10 -4 to 1.4 μg/ml); (2) solution volume-to-rock mass ratios used in the measurements (5 to 100 ml/g), and for WIPP material only; (3) water composition (0 to 100% brine in groundwater); and (4) sample location in the Culebra and Magenta dolomite members of the Rustler Formation. The results indicate that if groundwater intrudes into a repository and leaches a waste form, significant concentrations of dissolved or colloidal U(VI) could be maintained in the liquid phase. Should these solutions enter an aquifer system, there are reasonable sets of conditions which could lead to subsequent migration of U(VI) away from the repository site

  14. Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes

    Energy Technology Data Exchange (ETDEWEB)

    Jakeman, David L.; Mitchell, Dan J.; Shuttleworth, Wendy A.; Evans, Jeremy N.S. [Washington State University, Department of Biochemistry and Biophysics (United States)

    1998-10-15

    Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of {sup 13}P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 {+-} 12 Hz and 125 {+-} 7 Hz respectively, by a variety of methods involving additives and freezing techniques.

  15. A method of estimating hydrogen in solid and liquid samples by means of neutron thermalisation

    International Nuclear Information System (INIS)

    Carter, D.H.; Sanders, J.E.

    1967-06-01

    The count-rate of a cadmium-covered Pu239 fission chamber placed in a reactor neutron flux increases when a hydrogen-containing material is inserted due to the thermalisation of epicadmium neutrons. This effect forms the basis of a non-destructive method of estimating hydrogen in solid or liquid samples, and trial experiments to demonstrate the principles have been made. The sensitivity is such that hydrogen down to 10 p.p.m. in a typical metal should be detected. A useful feature of the method is its very low response to elements other than hydrogen. (author)

  16. Developments of solid materials for UF6 sampling

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Nicholas [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Hebden, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Savina, Joseph [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

    2017-11-15

    This project demonstrated that a device using majority Commercial Off the Shelf (COTS) components could be used to collect uranium hexafluoride samples safely from gaseous or solid sources. The device was based on the successful Cristallini method developed by ABACC over the past 10 years. The system was designed to capture and store the UF6 as an inert fluoride salt to ease transportation regulations. In addition, the method was considerably faster than traditional cryogenic methods, collected enough material to perform analyses without undue waste, and could be used either inside a facility or in the storage yard.

  17. A long-term validation of the modernised DC-ARC-OES solid-sample method.

    Science.gov (United States)

    Flórián, K; Hassler, J; Förster, O

    2001-12-01

    The validation procedure based on ISO 17025 standard has been used to study and illustrate both the longterm stability of the calibration process of the DC-ARC solid sample spectrometric method and the main validation criteria of the method. In the calculation of the validation characteristics depending on the linearity(calibration), also the fulfilment of predetermining criteria such as normality and homoscedasticity was checked. In order to decide whether there are any trends in the time-variation of the analytical signal or not, also the Neumann test of trend was applied and evaluated. Finally, a comparison with similar validation data of the ETV-ICP-OES method was carried out.

  18. Disk Rock Cutting Tool for the Implementation of Resource-Saving Technologies of Mining of Solid Minerals

    Science.gov (United States)

    Manietyev, Leonid; Khoreshok, Aleksey; Tsekhin, Alexander; Borisov, Andrey

    2017-11-01

    The directions of a resource and energy saving when creating a boom-type effectors of roadheaders of selective action with disc rock cutting tools on a multi-faceted prisms for the destruction of formation of minerals and rocks pricemax are presented. Justified reversing the modes of the crowns and booms to improve the efficiency of mining works. Parameters of destruction of coal and rock faces by the disk tool of a biconical design with the unified fastening knots to many-sided prisms on effectors of extraction mining machines are determined. Parameters of tension of the interfaced elements of knots of fastening of the disk tool at static interaction with the destroyed face of rocks are set. The technical solutions containing the constructive and kinematic communications realizing counter and reverse mode of rotation of two radial crowns with the disk tool on trihedral prisms and cases of booms with the disk tool on tetrahedral prisms in internal space between two axial crowns with the cutter are proposed. Reserves of expansion of the front of loading outside a table of a feeder of the roadheader of selective action, including side zones in which loading corridors by blades of trihedral prisms in internal space between two radial crowns are created are revealed.

  19. Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

    Science.gov (United States)

    Herrero Latorre, C; Barciela García, J; García Martín, S; Peña Crecente, R M

    2013-12-04

    Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Hydrogeologic applications for historical records and images from rock samples collected at the Nevada National Security Site and vicinity, Nye County, Nevada - A supplement to Data Series 297

    Science.gov (United States)

    Wood, David B.

    2018-03-14

    Rock samples have been collected, analyzed, and interpreted from drilling and mining operations at the Nevada National Security Site for over one-half of a century. Records containing geologic and hydrologic analyses and interpretations have been compiled into a series of databases. Rock samples have been photographed and thin sections scanned. Records and images are preserved and available for public viewing and downloading at the U.S. Geological Survey ScienceBase, Mercury Core Library and Data Center Web site at https://www.sciencebase.gov/mercury/ and documented in U.S. Geological Survey Data Series 297. Example applications of these data and images are provided in this report.

  1. STRAIN LOCALIZATION PECULIARITIES AND DISTRIBUTION OF ACOUSTIC EMISSION SOURCES IN ROCK SAMPLES TESTED BY UNIAXIAL COMPRESSION AND EXPOSED TO ELECTRIC PULSES

    Directory of Open Access Journals (Sweden)

    V. A. Mubassarova

    2014-01-01

    accumulation of defects. The location system can be effectively applied when events with high amplitudes are accumulated in sufficient number. In this regard, clustering of AE sources (defects in the area of a future fault was recorded only during the measuring test when the AE activity was quite high at the constant load.As shown by data from the optical diagnostics set of equipment, LаVision Strain Master System, deformation of a specimen takes place in a non-uniform pattern over its surface, which is manifested as consecutively propagating waves of localized strain. This conclusion contributes to the research results obtained earlier for rock samples under tension and compression [Panteleev et al., 2013b, 2013c, 2013d]. Localized axial strain waves and localized radial strain waves (when material particles move in the direction perpendicular to the compression direction are concurrently observed. Such localized strain waves are ‘slow’ – they propagate at velocities that are by six or seven orders lower than the intrinsic velocity of sound propagation in the material. This observation correlates with the research results obtained earlier in studies of strain localization forms in the course of rock deformation [Zuev, 2011; Zuev et al., 2012].When the loaded specimen is impacted by the electromagnetic field, maximum strain values are slightly decreased in comparison with those in the ordinary case (when only compressive load is applied. This trend seems to be a specific feature of changes in localization of deformation in the loaded rock samples impacted by electric pulses. Besides, the experiments demonstrate that a source of macro-destruction can be induced by the influence of an external electromagnetic field, and the growth of a nucleus of such source can be stabilized during the impact. The above conclusions correlate with the statistical model of a solid body with defects which is developed in ICMM [Panteleev et al., 2011, 2012, 2013a].

  2. A comparison of iron oxide-rich joint coatings and rock chips as geochemical sampling media in exploration for disseminated gold deposits

    Science.gov (United States)

    Crone, W.; Larson, L.T.; Carpenter, R.H.; Chao, T.T.; Sanzolone, R.F.

    1984-01-01

    We evaluated the effectiveness of iron oxide-rich fracture coatings as a geochemical sampling medium for disseminated gold deposits, as compared with conventional lithogeochemical methods, for samples from the Pinson mine and Preble prospect in southeastern Humboldt County, Nevada. That disseminated gold mineralization is associated with Hg, As, and Sb is clearly demonstrated in these deposits for both fracture coatings and rock chip samples. However, the relationship is more pronounced for fracture coatings. Fracture coatings at Pinson contain an average of 3.61, 5.13, 14.37, and 3.42 times more Au, As, Sb and Hg, respectively, than adjacent rock samples. At Preble, fracture coatings contain 3.13, 9.72, 9.18, and 1.85 times more Au, As, Sb and Hg, respectively, than do adjacent rock samples. Geochemical anomalies determined from fracture coatings are thus typically more intense than those determined from rock samples for these elements. The sizes of anomalies indicated by fracture coatings are also somewhat larger, but this is less obvious. In both areas, Sb anomalies are more extensive in fracture coatings. At Preble, some Hg and Au anomalies are also more extensive in fracture coatings. In addition to halos formed by the Hg, As and Sb, high values for Au/Ag and Zn/(Fe + Mn) are closely associated with gold mineralization at the Pinson mine. The large enhancement in geochemical response afforded by fracture coatings indicates a definite potential in the search for buried disseminated gold deposits. ?? 1984.

  3. Automated sample preparation station for studying self-diffusion in porous solids with NMR spectroscopy

    Science.gov (United States)

    Hedin, Niklas; DeMartin, Gregory J.; Reyes, Sebastián C.

    2006-03-01

    In studies of gas diffusion in porous solids with nuclear magnetic resonance (NMR) spectroscopy the sample preparation procedure becomes very important. An apparatus is presented here that pretreats the sample ex situ and accurately sets the desired pressure and temperature within the NMR tube prior to its introduction in the spectrometer. The gas manifold that supplies the NMR tube is also connected to a microbalance containing another portion of the same sample, which is kept at the same temperature as the sample in the NMR tube. This arrangement permits the simultaneous measurement of the adsorption loading on the sample, which is required for the interpretation of the NMR diffusion experiments. Furthermore, to ensure a good seal of the NMR tube, a hybrid valve design composed of titanium, a Teflon® seat, and Kalrez® O-rings is utilized. A computer controlled algorithm ensures the accuracy and reproducibility of all the procedures, enabling the NMR diffusion experiments to be performed at well controlled conditions of pressure, temperature, and amount of gas adsorbed on the porous sample.

  4. Sampling of tar from sewage sludge gasification using solid phase adsorption.

    Science.gov (United States)

    Ortiz González, Isabel; Pérez Pastor, Rosa Ma; Sánchez Hervás, José Ma

    2012-06-01

    Sewage sludge is a residue from wastewater treatment plants which is considered to be harmful to the environment and all living organisms. Gasification technology is a potential source of renewable energy that converts the sewage sludge into gases that can be used to generate energy or as raw material in chemical synthesis processes. But tar produced during gasification is one of the problems for the implementation of the gasification technology. Tar can condense on pipes and filters and may cause blockage and corrosion in the engines and turbines. Consequently, to minimize tar content in syngas, the ability to quantify tar levels in process streams is essential. The aim of this work was to develop an accurate tar sampling and analysis methodology using solid phase adsorption (SPA) in order to apply it to tar sampling from sewage sludge gasification gases. Four types of commercial SPA cartridges have been tested to determine the most suitable one for the sampling of individual tar compounds in such streams. Afterwards, the capacity, breakthrough volume and sample stability of the Supelclean™ ENVI-Carb/NH(2), which is identified as the most suitable, have been determined. Basically, no significant influences from water, H(2)S or NH(3) were detected. The cartridge was used in sampling real samples, and comparable results were obtained with the present and traditional methods.

  5. Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

    Science.gov (United States)

    Hill, April A; Lipert, Robert J; Porter, Marc D

    2010-03-15

    The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  6. Long Term Sorption Diffusion Experiment (LTDE-SD). Supporting laboratory program - Sorption diffusion experiments and rock material characterisation. With supplement of adsorption studies on intact rock samples from the Forsmark and Laxemar site investigations

    Energy Technology Data Exchange (ETDEWEB)

    Widestrand, Henrik; Byegaard, Johan; Selnert, Eva; Skaalberg, Mats; Hoeglund, Susanne; Gustafsson, Erik (Geosigma AB, Uppsala (Sweden))

    2010-12-15

    The LTDE-SD experiment, (Long Term Sorption Diffusion Experiment) aims at increasing the scientific knowledge of sorption and diffusion under in situ conditions and to provide data for performance and safety assessment calculations. In this report, performance and results of laboratory sorption and diffusion experiments and porosity investigations using site-specific crushed and intact rock materials are presented, including a geological and mineralogical characterization of the samples. A synthetic groundwater and a part of the radionuclide tracer cocktail that was used for the in situ experiment were used also in the laboratory experiments. 13 radionuclide tracers were analysed in the laboratory experiments. The method descriptions from SKB Site Investigations were applied in order to enable comparisons with Site Investigations data. The water saturation porosity of 10 unaltered matrix rock samples from KA3065A02 and A03 is 0.26 +- 0.08% and two fracture material samples show porosities of 2.4% and 5.2% respectively. 14C-methylmethacrylate impregnation (the PMMA-method) show that the unaltered rock matrix porosity is relatively homogeneous with grain boundary porosity, while the porosity of fracture samples is heterogeneous and have increased porosity up to more than 10% in some parts. Through-diffusion experiments using tritiated water (H3HO) give a matrix diffusivity in the range from 2.7centre dot10-14 to 6.5centre dot10-14 m2/s in four samples from KA3065A02 and A03. The results of the porosity and diffusion measurements are coherent in ranges with earlier LTDE-SD measurements and are also in line with the SKB Site Investigations results. In the batch sorption experiments using crushed rock material, two matrix rock samples of Aevroe granodiorite, one red-stained altered Aevroe granodiorite sample and two chlorite-calcite dominated fracture samples were analysed for three different size fractions as a function of time up to 186 days contact time. The

  7. Solid Phase Microextraction (SPME in Determination of Pesticide Residues in Soil Samples

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2011-01-01

    Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

  8. Preliminary evaluation of new polymer matrix for solid-phase extraction of nonylphenol from water samples.

    Science.gov (United States)

    Guerreiro, António; Soares, Ana; Piletska, Elena; Mattiasson, Bo; Piletsky, Sergey

    2008-03-31

    Molecularly imprinted (MIP) and blank polymers with affinity for nonylphenol were designed using computational modelling. Chromatographic tests demonstrated higher affinity of imprinted polymers towards the template nonylphenol as compared with blank polymers. The performance of both polymers in solid-phase extraction was however very similar. Both blank and imprinted polymers appeared to be suitable for the removal and pre-concentration of nonylphenol from contaminated water samples with 99% efficiency of the recovery. The commercial resins PH(EC) (Biotage) and C18 (Varian) tested in the same conditions used for comparative purposes had recovery rate <84%. The polymer capacity for nonylphenol was 231 mg g(-1) for blank and 228 mg g(-1) for MIP. The synthesised materials can have significance for sample pre-concentration and environmental analysis of this class of compounds.

  9. Determination of Sr-90 in environmental samples using solid phase extraction disk

    International Nuclear Information System (INIS)

    Zal U'yun Wan Mahmood

    2002-01-01

    A method is described for determination of Sr-90 in environmental samples using solid phase extraction disk (Empore TM Strontium Rad Disk) and GM counter. To determine the optimum condition for capacity of Empore TM Strontium Rad Disk, its characterization studies such as the effects Sr content, acidity (molarity) of acids, presence of Ca 2+ and other major ions (Na + , Mg 2+ etc), influence of interference (Pb and Bi) and others were carried out. An optimized the using of Empore TM Strontium Rad Disk for determination of Sr-90 was validated by application to environmental samples. Quantitative recoveries above 95%for Sr (stable) were recorded in 6M HCl condition. Typical environmental samples may contain an assortment of anionic and cationic species, but in general, Empore TM Strontium Rad Disk has enough capacity to effectively separate Sr for wide variety of aqueous solutions. Sr recovery in a matrix-free or the content of matrix less than 300 mg/sample is typically greater than 99% is reported in this research work. In particular, sample, which may contain interference such as Pb and Bi would require an addition separation step before processing to ensure an accurate measurement of Sr. In this research work, radiotracer 85 Sr was used to monitor the behavior of Sr and calculation its recovery. For analytical methods that can count Y-90, the Sr-90 activity/concentration in environmental sample was calculated. The concentration of Sr-90 in ash sample (Quality Controled Sample) of 276 ± 18 Bq/kg ash was determined from Y-90 activity. The relative percent difference of 1.1% was achievable for Empore TM Sr-Rad Disk methods when compared to the conventional method (fumed-HNO 3 method) - 279 ± 11 Bq/kg ash. (Author)

  10. Current status of crushed rock and whole rock column studies

    International Nuclear Information System (INIS)

    Vine, E.N.; Daniels, W.R.; Rundberg, R.S.; Thompson, J.L.

    1980-01-01

    Measurements on a large number of crushed rock columns of tuff, granite, and argillite are discussed. The isotopes 85 Sr, 137 Cs, 133 Ba, 141 Ce, 152 Eu, /sup 95m/Tc, and 233 U were used. Flow rates were varied from approx. 30 to approx. 30000 m/y. Other parameters studied include isotope concentration and atmosphere. The sorption ratios calculated were compared with batch sorption ratios on the same samples. Methods of studying the movement of radionuclides through whole rock cores are described. The problems associated with sealing the cores to prevent leaking along the exterior surface and one possible solution are discussed. The strontium sorption ratio obtained by elution of one solid tuff core is compared with the batch and crushed rock column sorption ratios

  11. Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

    International Nuclear Information System (INIS)

    Edjabou, Maklawe Essonanawe; Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn; Petersen, Claus; Scheutz, Charlotte; Astrup, Thomas Fruergaard

    2015-01-01

    Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

  12. Municipal solid waste composition: Sampling methodology, statistical analyses, and case study evaluation

    Energy Technology Data Exchange (ETDEWEB)

    Edjabou, Maklawe Essonanawe, E-mail: vine@env.dtu.dk [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Jensen, Morten Bang; Götze, Ramona; Pivnenko, Kostyantyn [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark); Petersen, Claus [Econet AS, Omøgade 8, 2.sal, 2100 Copenhagen (Denmark); Scheutz, Charlotte; Astrup, Thomas Fruergaard [Department of Environmental Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark)

    2015-02-15

    Highlights: • Tiered approach to waste sorting ensures flexibility and facilitates comparison of solid waste composition data. • Food and miscellaneous wastes are the main fractions contributing to the residual household waste. • Separation of food packaging from food leftovers during sorting is not critical for determination of the solid waste composition. - Abstract: Sound waste management and optimisation of resource recovery require reliable data on solid waste generation and composition. In the absence of standardised and commonly accepted waste characterisation methodologies, various approaches have been reported in literature. This limits both comparability and applicability of the results. In this study, a waste sampling and sorting methodology for efficient and statistically robust characterisation of solid waste was introduced. The methodology was applied to residual waste collected from 1442 households distributed among 10 individual sub-areas in three Danish municipalities (both single and multi-family house areas). In total 17 tonnes of waste were sorted into 10–50 waste fractions, organised according to a three-level (tiered approach) facilitating comparison of the waste data between individual sub-areas with different fractionation (waste from one municipality was sorted at “Level III”, e.g. detailed, while the two others were sorted only at “Level I”). The results showed that residual household waste mainly contained food waste (42 ± 5%, mass per wet basis) and miscellaneous combustibles (18 ± 3%, mass per wet basis). The residual household waste generation rate in the study areas was 3–4 kg per person per week. Statistical analyses revealed that the waste composition was independent of variations in the waste generation rate. Both, waste composition and waste generation rates were statistically similar for each of the three municipalities. While the waste generation rates were similar for each of the two housing types (single

  13. If an antelope is a document, then a rock is data: preserving earth science samples for the future

    Science.gov (United States)

    Ramdeen, S.

    2015-12-01

    As discussed in seminal works by Briet (1951) and Buckland (1998), physical objects can be considered documents when given specific context. In the case of an antelope, in the wild it's an animal, in a zoo it's a document. It is the primary source of information, specifically when it is made an object of study. When discussing earth science data, we may think about numbers in a spreadsheet or verbal descriptions of a rock. But what about physical materials such as cores, cuttings, fossils, and other tangible objects? The most recent version of the American Geophysical Union's data position statement states data preservation and management policies should apply to both "digital data and physical objects"[1]. If an antelope is a document, than isn't a rock a form of data? Like books in a library or items in a museum, these objects require surrogates (digital or analog) that allow researchers to access and retrieve them. Once these scientific objects are acquired, researchers can process the information they contain. Unlike books, and some museum materials, most earth science objects cannot yet be completely replaced by digital surrogates. A fossil may be scanned, but the original is needed for chemical testing and ultimately for 'not yet developed' processes of scientific analysis. These objects along with their metadata or other documentation become scientific data when they are used in research. Without documentation of key information (i.e. the location where it was collected) these objects may lose their scientific value. This creates a complex situation where we must preserve the object, its metadata, and the connection between them. These factors are important as we consider the future of earth science data, our definitions of what constitutes scientific data, as well as our data preservation and management practices. This talk will discuss current initiatives within the earth science communities (EarthCube's EC3 and iSamples; USGS's data preservation program

  14. Headspace Solid Phase Microextraction in Pesticide Residues Analysis: 2. Apple Samples

    Directory of Open Access Journals (Sweden)

    Jelena Milinović

    2007-01-01

    Full Text Available Headspace solid phase microextraction method (HS/SPME, optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS. A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.

  15. Determination of lead in rice grains by solid sampling HR-CS GFAAS.

    Science.gov (United States)

    Gunduz, Sema; Akman, Suleyman

    2013-12-01

    A study was performed for the determination of lead in rice grains directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) without digesting sample. The effects of sample amount, pyrolysis/atomization temperatures on the determination of lead in rice were investigated and optimized using a certificated rice flour. The lead concentrations were determined applying 800 °C of pyrolysis and 1800 °C of atomization temperatures without modifier. LOD (N=10, 3σ) and characteristic mass were 2.3 μg kg(-1) and 8.1 pg, respectively. The certified lead value of a rice flour CRM was found in its uncertainity limits. The lead contents of various rice samples obtained from markets in Turkey were between 0.009 and 0.162 mg kg(-1) which are in acceptable range. The average lead concentrations in various rice grains taken from the same package were significantly different from each other. Copyright © 2013 Elsevier Ltd. All rights reserved.

  16. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  17. Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

    Science.gov (United States)

    Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2017-05-05

    Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Membrane solid-phase extraction: Field application for isolation of polycyclic aromatic hydrocarbons from water samples

    International Nuclear Information System (INIS)

    Furlong, E.T.; Koleis, J.C.; Gates, P.M.

    1995-01-01

    Solid-phase extraction (SPE) membranes (M-SPE) were used to isolate microgram-per-liter to nanogram-per-liter quantities of polycyclic aromatic hydrocarbons (PAH) in 4- to 8-liter ground-water samples from a crude-oil-contaminated ground-water site near Bemidji, Minnesota. The M-SPE method was evaluated (1) under laboratory conditions using reagent water fortified with individual PAH at 1.23 micrograms per liter, and (2) at the Bemidji site. At the site, ground-water samples were processed and PAH isolated using a M-SPE system connected directly to the well pump. Following sample isolation, all M-SPE samples were extracted using dichloromethane and analyzed by gas chromatography-mass spectrometry with selected-ion monitoring. Operationally, the M-SPE method provided a simple means to isolate PAH on site at the wellhead, particularly for anoxic water samples. Acceptable recoveries, ranging from 56 to over 100 percent, were observed for lower molecular weight PAH (naphthalene to pyrene) using the M-SPE method. Recoveries using M-SPE were somewhat lower, but reproducible, for higher molecular weight PAH (chrysene to benzo[ghi]perylene), ranging from 18 to 56 percent. M-SPE provides the capability to collect and field isolate PAH from a sufficiently large number of samples to identify environmental chemical processes occurring at individual compound concentrations of 50 to 1,200 nanograms per liter. Using M-SPE, the potential for facilitated transport of PAH by in situ-derived dissolved organic carbon (DOC) was evaluated at the site. Plots comparing DOC and PAH concentrations indicate that PAH concentrations increase exponentially with linear increases in DOC concentrations

  19. A direct solid sampling analysis method for the detection of silver nanoparticles in biological matrices.

    Science.gov (United States)

    Feichtmeier, Nadine S; Ruchter, Nadine; Zimmermann, Sonja; Sures, Bernd; Leopold, Kerstin

    2016-01-01

    Engineered silver nanoparticles (AgNPs) are implemented in food contact materials due to their powerful antimicrobial properties and so may enter the human food chain. Hence, it is desirable to develop easy, sensitive and fast analytical screening methods for the determination of AgNPs in complex biological matrices. This study describes such a method using solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (GFAAS). A recently reported novel evaluation strategy uses the atomization delay of the respective GFAAS signal as significant indicator for AgNPs and thereby allows discrimination of AgNPs from ionic silver (Ag(+)) in the samples without elaborate sample pre-treatment. This approach was further developed and applied to a variety of biological samples. Its suitability was approved by investigation of eight different food samples (parsley, apple, pepper, cheese, onion, pasta, maize meal and wheat flour) spiked with ionic silver or AgNPs. Furthermore, the migration of AgNPs from silver-impregnated polypropylene food storage boxes to fresh pepper was observed and a mussel sample obtained from a laboratory exposure study with silver was investigated. The differences in the atomization delays (Δt(ad)) between silver ions and 20-nm AgNPs vary in a range from -2.01 ± 1.38 s for maize meal to +2.06 ± 1.08 s for mussel tissue. However, the differences were significant in all investigated matrices and so indicative of the presence/absence of AgNPs. Moreover, investigation of model matrices (cellulose, gelatine and water) gives the first indication of matrix-dependent trends. Reproducibility and homogeneity tests confirm the applicability of the method.

  20. WIPP Sampling and Analysis Plan for Solid Waste Management Units and Areas of Concern

    International Nuclear Information System (INIS)

    2000-01-01

    This Sampling and Analysis Plan (SAP) has been prepared to fulfill requirements of Module VII, Section VII.M.2 and Table VII.1, requirement 4 of the Waste Isolation Pilot Plant (WIPP) Hazardous Waste Permit, NM4890139088-TSDF (the Permit); (NMED [New Mexico Environment Department], 1999a). This SAP describes the approach for investigation of the Solid Waste Management Units (SWMU) and Areas of Concern (AOC) specified in the Permit. This SAP addresses the current Permit requirements for a RCRA Facility Investigation(RFI) investigation of SWMUs and AOCs. It uses the results of previous investigations performed at WIPP and expands the investigations as required by the Permit. As an alternative to the RFI specified in Module VII of the Permit, current NMED guidance identifies an Accelerated Corrective Action Approach (ACAA) that may be used for any SWMU or AOC (NMED, 1998). This accelerated approach is used to replace the standard RFI work plan and report sequence with a more flexible decision-making approach. The ACAA process allows a facility to exit the schedule of compliance contained in the facility's Hazardous and Solid Waste Amendments (HSWA) permit module and proceed on an accelerated time frame. Thus, the ACAA process can beentered either before or after a RFI work plan. According to NMED's guidance, a facility can prepare a RFI work plan or SAP for any SWMU or AOC (NMED, 1998).

  1. Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

    International Nuclear Information System (INIS)

    Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

    2004-01-01

    A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

  2. WIPP Sampling and Analysis Plan for Solid Waste Management Units and Areas of Concern

    Energy Technology Data Exchange (ETDEWEB)

    None, None

    2000-05-23

    This Sampling and Analysis Plan (SAP) has been prepared to fulfill requirements of Module VII, Section VII.M.2 and Table VII.1, requirement 4 of the Waste Isolation Pilot Plant (WIPP) Hazardous Waste Permit, NM4890139088-TSDF (the Permit); (NMED [New Mexico Environment Department], 1999a). This SAP describes the approach for investigation of the Solid Waste Management Units (SWMU) and Areas of Concern (AOC) specified in the Permit. This SAP addresses the current Permit requirements for a RCRA Facility Investigation(RFI) investigation of SWMUs and AOCs. It uses the results of previous investigations performed at WIPP and expands the investigations as required by the Permit. As an alternative to the RFI specified in Module VII of the Permit, current NMED guidance identifies an Accelerated Corrective Action Approach (ACAA) that may be used for any SWMU or AOC (NMED, 1998). This accelerated approach is used to replace the standard RFI work plan and report sequence with a more flexible decision-making approach. The ACAA process allows a facility to exit the schedule of compliance contained in the facility's Hazardous and Solid Waste Amendments (HSWA) permit module and proceed on an accelerated time frame. Thus, the ACAA process can beentered either before or after a RFI work plan. According to NMED's guidance, a facility can prepare a RFI work plan or SAP for any SWMU or AOC (NMED, 1998).

  3. Leaching of boron, arsenic and selenium from sedimentary rocks: I. Effects of contact time, mixing speed and liquid-to-solid ratio

    Energy Technology Data Exchange (ETDEWEB)

    Tabelin, Carlito Baltazar, E-mail: carlito@trans-er.eng.hokudai.ac.jp [Laboratory of Soil Environment Engineering, Faculty of Engineering, Hokkaido University, Sapporo (Japan); Hashimoto, Ayaka, E-mail: a.hashimoto@diaconsult.co.jp [DIA Consultants Co. Ltd., Sapporo (Japan); Igarashi, Toshifumi, E-mail: tosifumi@eng.hokudai.ac.jp [Laboratory of Groundwater and Mass Transport, Faculty of Engineering, Hokkaido University, Sapporo (Japan); Yoneda, Tetsuro, E-mail: yonet@eng.hokudai.ac.jp [Laboratory of Soil Environment Engineering, Faculty of Engineering, Hokkaido University, Sapporo (Japan)

    2014-02-01

    Sedimentary rocks of marine origin excavated in tunnel projects were recently identified as potentially hazardous because they could release significant amounts of toxic trace elements when exposed to the environment. This study investigated the leaching characteristics of B, As, Se and the major coexisting ions under various conditions to identify the factors and processes controlling their evolution in the leachate. In addition, we evaluated whether the parameters of the currently used leachability test for excavated rocks were adequate. Although the leachabilities of B, As and Se similarly increased at longer contact times, only those of B and As were influenced by the mixing speed and/or liquid-to-solid ratio (L/S). The majority of trace elements dissolved in the leachate originated from the dissolution of soluble salts formed from seawater of the Cretaceous trapped during the formation of the sedimentary rocks. Moreover, the alkaline pH of the leachates could be attributed to the simultaneous dissolutions at varying degrees of the mineral components of the rocks as well as the precipitation of clay minerals. In the leaching test of excavated rocks for regulatory purposes, the best values of contact time and mixing speed should represent conditions of the highest trace element extractabilities, which in this study were found at longer contact times ( > 48 h) and the fastest mixing speed (200 rpm). The most appropriate L/S for the leaching test is 10 because it was around this L/S that the extractabilities and leaching concentrations of the trace elements were simultaneously observed at their highest values. - Highlights: • B, As and Se leaching increased with time reaching equilibrium after ca. 48 h. • Effect of L/S on B and As leaching was strong but not that much on Se. • All leachates were alkaline regardless of the contact time, mixing speed and L/S. • Na{sup +}–SO{sub 4}{sup 2−} and Na{sup +}–HCO{sub 3}{sup −} type leachates were produced

  4. Relationships between data from Rock-Eval pyrolysis and proximate, ultimate, petrographic, and physical analyses of 142 diverse U.S. coal samples

    Science.gov (United States)

    Bostick, N.H.; Daws, T.A.

    1994-01-01

    Basic research on coal and oil shale led to automated pyrolysis analysis of petroleum source rocks; most widely used is the Rock-Eval equipment. In order to interpret Rock-Eval analyses in relation to traditional coal data, we analyzed 142 commercial coals with diverse rank, age, maceral and sulfur contents, for most regions of the United States. We compared the Rock-Eval data with traditional industrial coal data, including volatile matter, calorific value, hydrogen and oxygen content, free swelling index, and vitrinite reflectance. We found: (1) there is a close relationship between Tmax and vitrinite reflectance in the ranges 420-590??C Tmax and 0.4-3%Romax of most coals. (2) A close relationship between Tmax and volatile matter (%VM) extends through the entire sample range, including low-rank samples with 35-70% VM, a range where %VM is not considered to be a useful rank parameter. (3) TOC of medium- and high-rank coals is seriously under-measured by Rock-Eval; TOC of low-rank coals (less than 0.8%Romax) is close to "dry basis" carbon from ultimate analysis. (4) The direct relationships between oxygen index (OI) and %O and between hydrogen index (HI) and %H are clear, though only broadly defined. However, there is virtually no band of concentrated data points on the HI versus OI pseudo-Van Krevelen diagram comparable to the "development line" on the H/C versus O/C diagram. (5) There are systematic relationships between Rock-Eval and industrial coal parameters such as calorific value and FSI, but much standardization would be needed before Rock-Eval could find a place in the coal industry. Tests with blends of coal and quartz sand and with various loads of coal alone showed that the amount of organic matter in the Rock-Eval load greatly influences results. Total load in the crucible, if largely inert, plays a small role, however. Increasing absolute or relative coal content causes under-evaluation of Rock-Eval TOC and over-rating of hydrogen. Blends of several

  5. Are Flow Injection-based Approaches Suitable for Automated Handling of Solid Samples?

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Cerdà, Victor

    Flow-based approaches were originally conceived for liquid-phase analysis, implying that constituents in solid samples generally had to be transferred into the liquid state, via appropriate batch pretreatment procedures, prior to analysis. Yet, in recent years, much effort has been focused...... electrolytic or aqueous leaching, on-line dialysis/microdialysis, in-line filtration, and pervaporation-based procedures have been successfully implemented in continuous flow/flow injection systems. In this communication, the new generation of flow analysis, including sequential injection, multicommutated flow.......g., soils, sediments, sludges), and thus, ascertaining the potential mobility, bioavailability and eventual impact of anthropogenic elements on biota [2]. In this context, the principles of sequential injection-microcolumn extraction (SI-MCE) for dynamic fractionation are explained in detail along...

  6. Dynamic Flow-through Methods for Metal Fractionation in Environmental Solid Samples

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Petersen, Roongrat

    occurring processes always take place under dynamic conditions, recent trends have been focused on the development of alternative flow-through dynamic methods aimed at mimicking environmental events more correctly than their classical extraction counterparts. In this lecture particular emphasis is paid......Accummulation of metal ions in different compartments of the biosphere and their possible mobilization under changing environmental conditions induce a pertubation of the ecosystem and may cause adverse health effects. Nowadays, it is widely recognized that the information on total content...... the ecotoxicological significance of metal ions in solid environmental samples. The background of end-over-end fractionation for releasing metal species bound to particular soil phases is initially discussed, its relevant features and limitations being thoroughly described. However, taking into account that naturally...

  7. Recovery of solid rock in open-cast mines vs. combination of open-cast mining and deep mines. A cost balance sheet; Festgesteinsgewinnung im Tagebau vs. Kombination von Tagebau und Tiefbau. Eine Kostenbilanz

    Energy Technology Data Exchange (ETDEWEB)

    Hennig, Alexander; Niemann-Delius, Christian; Skrypzak, Thorsten [RWTH Aachen (DE). Inst. fuer Rohstoffgewinnung ueber Tage und Bohrtechnik (BBK III)

    2011-10-15

    Rising fuel prices have led to greater interest in working methods, which offer an economical alternative for extraction of solid rock by means of shovel and truck in recent years. In this connection starting points exist in the reduction of the specific energy consumption and wider use of cheaper electrical energy. However, energy demand and costs are only partial aspects, their effect on the overall profitability sometimes being difficult to estimate. Taking the example of a solid rock deposit two working methods, which differ fundamentally with regard to equipment and energy input, are subjected to a cost/benefit analysis below. (orig.)

  8. Perspectives of an acoustic–electrostatic/electrodynamic hybrid levitator for small fluid and solid samples

    International Nuclear Information System (INIS)

    Lierke, E G; Holitzner, L

    2008-01-01

    The feasibility of an acoustic–electrostatic hybrid levitator for small fluid and solid samples is evaluated. A proposed design and its theoretical assessment are based on the optional implementation of simple hardware components (ring electrodes) and standard laboratory equipment into typical commercial ultrasonic standing wave levitators. These levitators allow precise electrical charging of drops during syringe- or ink-jet-type deployment. The homogeneous electric 'Millikan field' between the grounded ultrasonic transducer and the electrically charged reflector provide an axial compensation of the sample weight in an indifferent equilibrium, which can be balanced by using commercial optical position sensors in combination with standard electronic PID position control. Radial electrostatic repulsion forces between the charged sample and concentric ring electrodes of the same polarity provide stable positioning at the centre of the levitator. The levitator can be used in a pure acoustic or electrostatic mode or in a hybrid combination of both subsystems. Analytical evaluations of the radial–axial force profiles are verified with detailed numerical finite element calculations under consideration of alternative boundary conditions. The simple hardware modification with implemented double-ring electrodes in ac/dc operation is also feasible for an electrodynamic/acoustic hybrid levitator

  9. Calibration of track detectors and measurement of radon exhalation rate from solid samples

    International Nuclear Information System (INIS)

    Singh, Ajay Kumar; Jojo, P.J.; Prasad, Rajendra; Khan, A.J.; Ramachandran, T.V.

    1997-01-01

    CR-39 and LR-115 type II track detectors to be used for radon exhalation measurements have been calibrated. The configurations fitted with detectors in Can technique in the open cup mode are cylindrical plastic cup (PC) and conical plastic cup (CPC). The experiment was performed in radon exposure chamber having monodisperse aerosols of 0.2 μm size, to find the relationship between track density and the radon concentration. The calibration factors for PC and CPC type dosimeters with LR-115 type II detector were found to be 0.056 and 0.083 tracks cm -2 d -1 (Bqm -3 ) -1 respectively, while with CR-39 detector the values were 0.149 and 0.150 tracks cm -2 d -1 (Bq m -3 ) -1 . Employing the Can technique, measurements of exhalation rates from solid samples used as construction materials, are undertaken. Radon exhalation rate is found to be minimum in cement samples while in fly ash it is not enhanced as compared to coal samples. (author)

  10. Microporous Carbon Spheres Solid Phase Membrane Tip Extraction for the Analysis of Nitrosamines in Water Samples

    International Nuclear Information System (INIS)

    Mohammed Salisu Musa; Wan Aini Wan Ibrahim

    2015-01-01

    A simple solid phase membrane tip extraction (SPMTE) utilizing microporous carbon spheres (MCS) was developed for the analysis of nitrosamines in aqueous samples. The method termed MCS-SPMTE was optimized for various important extraction parameters namely conditioning organic solvent, extraction time, effects of salt addition and pH change, desorption time, desorption solvent and sample volume. Under the optimized conditions, the method indicated good linearity in the range of 10-100 μg/ L with coefficients of determination, r 2 ≥0.9984. The method also demonstrated good reproducibility with % RSDs values ranging from 2.2 - 8.9 (n = 3). Limit of detection (LOD) and limit of quantification (LOQ) for the method ranged from 3.2 - 4.8 μg/ L and 10.9 - 15.9 μg/L respectively. Recoveries for both tap-water and lake water samples spiked at 10 μg/L were in the range of 83.2 - 107.5 %. (author)

  11. [Optimization of solid-phase extraction for enrichment of toxic organic compounds in water samples].

    Science.gov (United States)

    Zhang, Ming-quan; Li, Feng-min; Wu, Qian-yuan; Hu, Hong-ying

    2013-05-01

    A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.

  12. Solid phase extraction for sample preparation in trace analysis of ionogenic compounds by capillary isotachophoresis

    International Nuclear Information System (INIS)

    Hutta, M.; Kaniansky, D.; Simunicova, E.; Zelenska, V.; Madajova, V.; Siskova, A.

    1992-01-01

    Various sorbents recommended for solid phase extraction (SPE) in sample preparation procedures were studied for use in combination with capillary isotachophoresis (ITP). They were very efficient in achieving trace concentration levels (low ppb, i.e., low parts per 10 9 ) for different types of ITP analytes present in environmental and biological matrices. A macroporous carbon sorbent was convenient for sample preparation in ITP analysis of short chain fatty acids (C 4 -C 9 ) in drinking water. Chelating sorbents based on hydroxyalkyl methacrylate matrix with salicylate, thioglycolate and 8-hydroxyquinolinate functionalities were found to be very suitable for preconcentration of heavy metals with an inherent sample clean-up. An octadecyl-bonded silica sorbent enabled in ITP a photometric detection of γ-aminobutyrate (labeled with a 2,4,6-trinitrophenyl group) at concentrations considerably lower than required for the determination of this amino acid in cerebrospinal fluid (∼5*10 -8 mol/l). (author) 34 refs.; 3 figs.; 1 tab

  13. Molecularly imprinted solid-phase extraction of glutathione from urine samples

    International Nuclear Information System (INIS)

    Song, Renyuan; Hu, Xiaoling; Guan, Ping; Li, Ji; Zhao, Na; Wang, Qiaoli

    2014-01-01

    Molecularly imprinted polymer (MIP) particles for glutathione were synthesized through iniferter-controlled living radical precipitation polymerization (IRPP) under ultraviolet radiation at ambient temperature. Static adsorption, solid-phase extraction, and high-performance liquid chromatography were carried out to evaluate the adsorption properties and selective recognition characteristics of the polymers for glutathione and its structural analogs. The obtained IRPP-MIP particles exhibited a regularly spherical shape, rapid binding kinetics, high imprinting factor, and high selectivity compared with the MIP particles prepared using traditional free-radical precipitation polymerization. The selective separation and enrichment of glutathione from the mixture of glycyl-glycine and glutathione disulfide could be achieved on the IRPP-MIP cartridge. The recoveries of glutathione, glycyl-glycine, and glutathione disulfide were 95.6% ± 3.65%, 29.5% ± 1.26%, and 49.9% ± 1.71%, respectively. The detection limit (S/N = 3) of glutathione was 0.5 mg·L −1 . The relative standard deviations (RSDs) for 10 replicate detections of 50 mg·L −1 of glutathione were 5.76%, and the linear range of the calibration curve was 0.5 mg·L −1 to 200 mg·L −1 under optimized conditions. The proposed approach was successfully applied to determine glutathione in spiked human urine samples with recoveries of 90.24% to 96.20% and RSDs of 0.48% to 5.67%. - Highlights: • Imprinted polymer particles were prepared by IRPP at ambient temperature. • High imprinting factor, high selectivity, and rapid binding kinetics were achieved. • Selective solid-phase extraction of glutathione from human urine samples

  14. Distribution and evolution of Zn, Cd, and Pb in Apollo 16 regolith samples and the average U-Pb ages of the parent rocks

    Science.gov (United States)

    Cirlin, E. H.; Housley, R. M.

    1982-01-01

    The concentration of surface (low temperature site) and interior (high temperature site) Cd, Zn, and Pb in 13 Apollo 16 highland fines samples, pristine rock 65325, and mare fines sample 75081 were analyzed directly from the thermal release profiles obtained by flameless atomic absorption technique (FLAA). Cd and Zn in pristine ferroan anothosite 65325, anorthositic grains of the most mature fines 65701, and basaltic rock fragments of mare fines 75081 were almost all surface Cd and Zn indicating that most volatiles were deposited on the surfaces of vugs, vesicles and microcracks during the initial cooling process. A considerable amount of interior Cd and Zn was observed in agglutinates. This result suggests that high temperature site interior volatiles originate from entrapment during the lunar maturation processes. Interior Cd found in the most mature fines sample 65701 was only about 15% of the total Cd in the sample. Interior Pb present in Apollo 16 fines samples went up to 60%. From our Cd studies we can assume that this interior Pb in highland fines samples is largely due to the radiogenic decay which occurred after the redistribution of the volatiles took place. We obtained an average age of 4.0 b.y. for the parent rocks of Apollo 16 highland regolith from our interior Pb analyses.

  15. Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction.

    Science.gov (United States)

    Jochmann, Maik A; Yuan, Xue; Schmidt, Torsten C

    2007-03-01

    In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-microm film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons.

  16. Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction

    Energy Technology Data Exchange (ETDEWEB)

    Jochmann, Maik A.; Schmidt, Torsten C. [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany); Chair of Instrumental Analysis, University Duisburg-Essen, Duisburg (Germany); Yuan, Xue [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany)

    2007-03-15

    In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-{mu}m film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons. (orig.)

  17. Chromium speciation in environmental samples using a solid phase spectrophotometric method

    Science.gov (United States)

    Amin, Alaa S.; Kassem, Mohammed A.

    2012-10-01

    A solid phase extraction technique is proposed for preconcentration and speciation of chromium in natural waters using spectrophotometric analysis. The procedure is based on sorption of chromium(III) as 4-(2-benzothiazolylazo)2,2'-biphenyldiol complex on dextran-type anion-exchange gel (Sephadex DEAE A-25). After reduction of Cr(VI) by 0.5 ml of 96% concentrated H2SO4 and ethanol, the system was applied to the total chromium. The concentration of Cr(VI) was calculated as the difference between the total Cr and the Cr(III) content. The influences of some analytical parameters such as: pH of the aqueous solution, amounts of 4-(2-benzothiazolylazo)2,2'-biphenyldiol (BTABD), and sample volumes were investigated. The absorbance of the gel, at 628 and 750 nm, packed in a 1.0 mm cell, is measured directly. The molar absorptivities were found to be 2.11 × 107 and 3.90 × 107 L mol-1 cm-1 for 500 and 1000 ml, respectively. Calibration is linear over the range 0.05-1.45 μg L-1 with RSD of <1.85% (n = 8.0). Using 35 mg exchanger, the detection and quantification limits were 13 and 44 ng L-1 for 500 ml sample, whereas for 1000 ml sample were 8.0 and 27 ng L-1, respectively. Increasing the sample volume can enhance the sensitivity. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The proposed method was applied to the speciation of chromium in natural waters and total chromium preconcentration in microwave digested tobacco, coffee, tea, and soil samples. The results were simultaneously compared with those obtained using an ET AAS method, whereby the validity of the method has been tested.

  18. In Situ Analysis of Mars Soil and Rocks Sample with the Sam Gcms Instrumentation Onboard Curiosity : Interpretation and Comparison of Measurements Done during the First Martian Year of Curiosity on Mars

    Science.gov (United States)

    Szopa, C.; Coll, P. J.; Cabane, M.; Buch, A.; Coscia, D.; Millan, M.; Francois, P.; Belmahadi, I.; Teinturier, S.; Navarro-Gonzalez, R.; Glavin, D. P.; Freissinet, C.; Steele, A.; Eigenbrode, J. L.; Mahaffy, P. R.

    2014-12-01

    The characterisation of the chemical and mineralogical composition of solid surface samples collected with the Curiosity rover is a primary objective of the SAM experiment. These data should provide essential clues on the past habitability of Gale crater. Amongst the SAM suite of instruments [1], SAM-GC (Gas Chromatograph) is devoted to identify and quantify volatiles evolved from the thermal (heating up to about 900°C)/chemical (derivatization procedure) treatment of any soil sample collected by the Curiosity rover. With the aim to search for potential organic molecules outgassed from the samples, SAM-GC analytical channels composed of thermal-desorption injector, and a MXT-CLP or a MXT-Q chromatographic column was chosen to achieve all the measurements done up today, with the aim to separate of a wide range of volatile inorganic and organic molecules. Four solid samples have been analyzed with GCMS, one sand sample collected at the Rocknest site, two rock samples (John Klein and Cumberland respectively) collected at the Yellowknife Bay site using the Curiosity driller, and one rock sample collected at the Kimberly site. All the measurements were successful and they produced complex chromatograms with both detectors used for SAM GC, i.e. a thermal conductivity detector and the SAM quandrupole mass spectrometer. Their interpretation already revealed the presence of an oxychlorine phase present in the sample which is at the origin of chlorohydrocarbons clearly identified [2] but this represents only a fraction of the GCMS signal recorded [3,4]. This work presents a systematic comparison of the GCMS measurements done for the different samples collected, supported by reference data obtained in laboratory with different spare models of the gas chromatograph, with the aim to bring new elements of interpretation of the SAM measurements. References: [1] Mahaffy, P. et al. (2012) Space Sci Rev, 170, 401-478. [2] Glavin, D. et al. (2013), JGR. [3] Leshin L. et al. (2013

  19. High-resolution delineation of chlorinated volatile organic compounds in a dipping, fractured mudstone: depth- and strata-dependent spatial variability from rock-core sampling

    Science.gov (United States)

    Goode, Daniel J.; Imbrigiotta, Thomas E.; Lacombe, Pierre J.

    2014-01-01

    Synthesis of rock-core sampling and chlorinated volatile organic compound (CVOC) analysis at five coreholes, with hydraulic and water-quality monitoring and a detailed hydrogeologic framework, was used to characterize the fine-scale distribution of CVOCs in dipping, fractured mudstones of the Lockatong Formation of Triassic age, of the Newark Basin in West Trenton, New Jersey. From these results, a refined conceptual model for more than 55 years of migration of CVOCs and depth- and strata-dependent rock-matrix contamination was developed. Industrial use of trichloroethene (TCE) at the former Naval Air Warfare Center (NAWC) from 1953 to 1995 resulted in dense non-aqueous phase liquid (DNAPL) TCE and dissolved TCE and related breakdown products, including other CVOCs, in underlying mudstones. Shallow highly weathered and fractured strata overlie unweathered, gently dipping, fractured strata that become progressively less fractured with depth. The unweathered lithology includes black highly fractured (fissile) carbon-rich strata, gray mildly fractured thinly layered (laminated) strata, and light-gray weakly fractured massive strata. CVOC concentrations in water samples pumped from the shallow weathered and highly fractured strata remain elevated near residual DNAPL TCE, but dilution by uncontaminated recharge, and other natural and engineered attenuation processes, have substantially reduced concentrations along flow paths removed from sources and residual DNAPL. CVOCs also were detected in most rock-core samples in source areas in shallow wells. In many locations, lower aqueous concentrations, compared to rock core concentrations, suggest that CVOCs are presently back-diffusing from the rock matrix. Below the weathered and highly fractured strata, and to depths of at least 50 meters (m), groundwater flow and contaminant transport is primarily in bedding-plane-oriented fractures in thin fissile high-carbon strata, and in fractured, laminated strata of the gently

  20. High Precision 142Nd/144Nd and 143Nd/144Nd Isotope Ratio Measurements in Rock Samples

    Science.gov (United States)

    Ali, A.; Srinivasan, G.

    2009-05-01

    The long-lived 147Sm-143Nd system with a half-life (T1/2) of 106 Gyr is generally used for geochronology. The short-lived 146Sm-142Nd system (T1/2= 103 Myr) is used as a geological tracer to track early (˜500 Ma) silicate differentiation [1] events in different planetary bodies. The isotope composition measurements by thermal ionization mass spectrometry (TIMS) require purification of Nd using chemical separation methods. This is important as an impure sample will give both a very poor ion yield and cause beam instability in the mass spectrometer, potentially resulting in a poor analysis [2]. The separation of Nd for 143Nd isotope measurement is, fairly straightforward because there is no isobaric interference of any other REE. While 142Nd isotope analysis needs chemically separated Nd fraction to be ˜100% Ce-free as latter is composed of a substantial amount of 142Ce isotope. A 4-steps technique, modified from Caro et al., [3], for the separation of Nd is established at the Cosmochemistry Laboratory of University of Toronto, Canada and applied to the measurement of Nd isotope ratios in geological reference sample BCR-2 (USGS, Columbia River basalt) using TIMS. Results of the isotopic ratios obtained for BCR-2 are in good agreement with published values [e.g., 4]. Analytical work on the samples discovered as the oldest rocks on Earth [5] from Nuvvuagittuq greenstone belt in Québec, Canada and various meteorites is in progress. An account of the procedures involved is briefly described here. All working solutions and acids were prepared using >18.2 MΩ.cm-1 H2O from a Milli-Q water system. Experiments were performed under Class 100 clean work bench with acid-cleaned apparatus and plastic-ware. The whole rock powders were weighed (20-30 mg) and dissolved in a mixture of HF and HNO3 using PFA vials and heated at 110°C. Further decomposition was done in Teflon bomb in the oven at 205°C. Later on contents of the Teflon bomb were transferred to vials and fluorides

  1. Investigation of the suspected presence of solid hydrocarbon in bedded salt samples from the Palo Duro Basin, Texas

    International Nuclear Information System (INIS)

    1985-10-01

    This report contains laboratory test results for two bedded salt samples from the Grabbe No. 1 (PD-2) Well of the Palo Duro Basin, Texas. This study was commissioned to determine whether or not solid hydrocarbons exist in bedded salt samples in the Palo Duro Basin. Laboratory investigations include electron microprobe examinations on polished thin sections and optical examinations and chemical tests on insoluble residues of the salt samples. No direct evidence was found that identifiable solid hydrocarbons are present in either sample of the bedded salt core. The total carbon content of the two salt samples was measured yielding 0.016 and 0.022 weight percent carbon. Detailed microscopic analyses showed that the carbon in the samples was associated with calcite, clays, and the epoxy resin used in sample preparation

  2. Microbial analyses of clay and water from different samples from the Mont Terri Rock Laboratory (RL), Switzerland

    International Nuclear Information System (INIS)

    Sergeant, C.; Vesvres, M.H.; Barsotti, V.; Stroes-Gascoyne, S.; Hamon, C.J.; Neble, S.; Shippers, A.; Le Marrec, C.; Vinsot, A.; Schwyn, B.

    2010-01-01

    processes that may develop locally in Opalinus Clay upon disturbance by drilling and excavation (i.e., introduction of space, water, microbes and nutrients). In a second part of this work, results are presented here from detection and identification of microorganisms in water which accumulated in an open borehole drilled in the Opalinus Clay (BEZ-G5). Besides introduced (exogenous) microorganisms, such water may contain autochthonous species. The latter may be easier to detect in water samples than by direct analysis of the clay rock. Both culturing (aerobic and anaerobic media) and direct (DNA extraction and PCR-DGGE) methods were used. Pure cultures of bacteria isolated in several enrichment media and identified by DNA extraction, PCR and sequencing indicated that most isolated bacteria are heterotrophic aerobes or facultative anaerobes commonly isolated from soil and water (such as Dietzia sp., Pseudomonas sp.) and therefore probably contaminants. In parallel, direct DNA extraction from water and PCR-DGGE revealed other contaminant bacteria (such as Staphylococcus sp., Rhizobium sp.). Nevertheless, some species may be indigenous in the Opalinus Clay such as Desulfosporosinus sp. isolated on sulfate-reducing media or Speleomyces sp., identified by PCRDGGE and previously isolated from a medieval mine. Complementary characterizations of these bacteria are required to confirm these first results. The diversity of microorganisms detected shows that both culturing and molecular approaches are essential to study this type of environment. (authors)

  3. Passive sampling of ambient ozone by solid phase microextraction with on-fiber derivatization

    International Nuclear Information System (INIS)

    Lee, I-S.; Tsai, S.-W.

    2008-01-01

    The solid phase microextraction (SPME) device with the polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was used as a passive sampler for ambient ozone. Both O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) and 1,2-di-(4-pyridyl)ethylene (DPE) were loaded onto the fiber before sampling. The SPME fiber assembly was then inserted into a PTFE tubing as a passive sampler. Known concentrations of ozone around the ambient ground level were generated by a calibrated ozone generator. Laboratory validations of the SPME passive sampler with the direct-reading ozone monitor were performed side-by-side in an exposure chamber at 25 deg. C. After exposures, pyriden-4-aldehyde was formed due to the reaction between DPE and ozone. Further on-fiber derivatizations between pyriden-4-aldehyde and PFBHA were followed and the derivatives, oximes, were then determined by portable gas chromatography with electron capture detector. The experimental sampling rate of the SPME ozone passive sampler was found to be 1.10 x 10 -4 cm 3 s -1 with detection limit of 58.8 μg m -3 h -1 . Field validations with both SPME device and the direct-reading ozone monitor were also performed. The correlations between the results from both methods were found to be consistent with r = 0.9837. Compared with other methods, the current designed sampler provides a convenient and sensitive tool for the exposure assessments of ozone

  4. Mass spectrometry of solid samples in open air using combined laser ionization and ambient metastable ionization

    International Nuclear Information System (INIS)

    He, X.N.; Xie, Z.Q.; Gao, Y.; Hu, W.; Guo, L.B.; Jiang, L.; Lu, Y.F.

    2012-01-01

    Mass spectrometry of solid samples in open air was carried out using combined laser ionization and metastable ionization time-of-flight mass spectrometry (LI-MI-TOFMS) in ambient environment for qualitative and semiquantitative (relative analyte information, not absolute information) analysis. Ambient metastable ionization using a direct analysis in realtime (DART) ion source was combined with laser ionization time-of-flight mass spectrometry (LI-TOFMS) to study the effects of combining metastable and laser ionization. A series of metallic samples from the National Institute of Standards and Technology (NIST 494, 495, 498, 499, and 500) and a pure carbon target were characterized using LI-TOFMS in open air. LI-MI-TOFMS was found to be superior to laser-induced breakdown spectroscopy (LIBS). Laser pulse energies between 10 and 200 mJ at the second harmonic (532 nm) of an Nd:YAG laser were applied in the experiment to obtain a high degree of ionization in plasmas. Higher laser pulse energy improves signal intensities of trace elements (such as Fe, Cr, Mn, Ni, Ca, Al, and Ag). Data were analyzed by numerically calculating relative sensitivity coefficients (RSCs) and limit of detections (LODs) from mass spectrometry (MS) and LIBS spectra. Different parameters, such as boiling point, ionization potential, RSC, LOD, and atomic weight, were shown to analyze the ionization and MS detection processes in open air.

  5. Igneous rocks formed by hypervelocity impact

    Science.gov (United States)

    Osinski, Gordon R.; Grieve, Richard A. F.; Bleacher, Jacob E.; Neish, Catherine D.; Pilles, Eric A.; Tornabene, Livio L.

    2018-03-01

    Igneous rocks are the primary building blocks of planetary crusts. Most igneous rocks originate via decompression melting and/or wet melting of protolith lithologies within planetary interiors and their classification and compositional, petrographic, and textural characteristics, are well-studied. As our exploration of the Solar System continues, so too does the inventory of intrusive and extrusive igneous rocks, settings, and processes. The results of planetary exploration have also clearly demonstrated that impact cratering is a ubiquitous geological process that has affected, and will continue to affect, all planetary objects with a solid surface, whether that be rock or ice. It is now recognized that the production of igneous rocks is a fundamental outcome of hypervelocity impact. The goal of this review is to provide an up-to-date synthesis of our knowledge and understanding of igneous rocks formed by hypervelocity impact. Following a brief overview of the basics of the impact process, we describe how and why melts are generated during impact events and how impact melting differs from endogenic igneous processes. While the process may differ, we show that the products of hypervelocity impact can share close similarities with volcanic and shallow intrusive igneous rocks of endogenic origin. Such impact melt rocks, as they are termed, can display lobate margins and cooling cracks, columnar joints and at the hand specimen and microscopic scale, such rocks can display mineral textures that are typical of volcanic rocks, such as quench crystallites, ophitic, porphyritic, as well as features such as vesicles, flow textures, and so on. Historically, these similarities led to the misidentification of some igneous rocks now known to be impact melt rocks as being of endogenic origin. This raises the question as to how to distinguish between an impact versus an endogenic origin for igneous-like rocks on other planetary bodies where fieldwork and sample analysis may not

  6. Application of nuclear techniques to the measurement of rock density and transport of solid particles suspended in rivers

    International Nuclear Information System (INIS)

    Seddiki, A.

    1984-10-01

    In order to better understand hydron phenomens in semi-arid regions characterized by torrential rains, we measured solid particles suspended to dums and in rivers. We also determined the density profile of a drilling and density of saline solutions. We designed an automatic nuclear gauge used for measuring the concentration of particles suspended to rivers. The installation, calibration and operations of a LABEN gauge were done in BENI SLIMANE on the 27th and 28th of February, 1984. The first results we obtained were received on the 24th of April, 1984

  7. Precise and accurate δ13C analysis of rock samples using Flash Combustion–Cavity Ring Down Laser Spectroscopy

    DEFF Research Database (Denmark)

    Balslev-Clausen, David Morten; Dahl, Tais W.; Saad, Nabil

    2013-01-01

    The ratio of 13C to 12C in marine sedimentary rocks holds important clues to the evolution of the carbon cycle through Earth history. Isotopic analyses are traditionally carried out using isotope ratio mass spectrometry (IRMS), but this technique is both labor-intensive, expensive and requires...

  8. Elastic wave velocities, chemistry and modal mineralogy of crustal rocks sampled by the Outokumpu scientific drill hole: Evidence from lab measurements and modeling

    Science.gov (United States)

    Kern, H.; Mengel, K.; Strauss, K. W.; Ivankina, T. I.; Nikitin, A. N.; Kukkonen, I. T.

    2009-07-01

    The Outokumpu scientific deep drill hole intersects a 2500 m deep Precambrian crustal section comprising a 1300 m thick biotite-gneiss series (mica schists) at top, followed by a 200 m thick meta-ophiolite sequence, underlain again by biotite gneisses (mica schists) (500 m thick) with intercalations of amphibolite and meta-pegmatoids (pegmatitic granite). From 2000 m downward the dominating rock types are meta-pegmatoids (pegmatitic granite). Average isotropic intrinsic P- and S-wave velocities and densities of rocks were calculated on the basis of the volume fraction of the constituent minerals and their single crystal properties for 29 core samples covering the depth range 198-2491 m. The modal composition of the rocks is obtained from bulk rock (XRF) and mineral chemistry (microprobe), using least squares fitting. Laboratory seismic measurements on 13 selected samples representing the main lithologies revealed strong anisotropy of P- and S-wave velocities and shear wave splitting. Seismic anisotropy is strongly related to foliation and is, in particular, an important property of the biotite gneisses, which dominate the upper and lower gneiss series. At in situ conditions, velocity anisotropy is largely caused by oriented microcracks, which are not completely closed at the pressures corresponding to the relatively shallow depth drilled by the borehole, in addition to crystallographic preferred orientation (CPO) of the phyllosilicates. The contribution of CPO to bulk anisotropy is confirmed by 3D velocity calculations based on neutron diffraction texture measurements. For vertical incidence of the wave train, the in situ velocities derived from the lab measurements are significantly lower than the measured and calculated intrinsic velocities. The experimental results give evidence that the strong reflective nature of the ophiolite-derived rock assemblages is largely affected by oriented microcracks and preferred crystallographic orientation of major minerals, in

  9. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Science.gov (United States)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

  10. Sampling gaseous compounds from essential oils evaporation by solid phase microextraction devices

    Science.gov (United States)

    Cheng, Wen-Hsi; Lai, Chin-Hsing

    2014-12-01

    Needle trap samplers (NTS) are packed with 80-100 mesh divinylbenzene (DVB) particles to extract indoor volatile organic compounds (VOCs). This study compared extraction efficiency between an NTS and a commercially available 100 μm polydimethylsiloxane-solid phase microextration (PDMS-SPME) fiber sampler used to sample gaseous products in heated tea tree essential oil in different evaporation modes, which were evaporated respectively by free convection inside a glass evaporation dish at 27 °C, by evaporation diffuser at 60 °C, and by thermal ceramic wicks at 100 °C. The experimental results indicated that the NTS performed better than the SPME fiber samplers and that the NTS primarily adsorbed 5.7 ng ethylbenzene, 5.8 ng m/p-xylenes, 11.1 ng 1,2,3-trimethylbenzene, 12.4 ng 1,2,4-trimethylbenzene and 9.99 ng 1,4-diethylbenzene when thermal ceramic wicks were used to evaporate the tea tree essential oil during a 1-hr evaporation period. The experiment also indicated that the temperature used to heat the essential oils should be as low as possible to minimize irritant VOC by-products. If the evaporation temperature does not exceed 100 °C, the concentrations of main by-products trimethylbenzene and diethylbenzene are much lower than the threshold limit values recommended by the National Institute for Occupational Safety and Health (NIOSH).

  11. Polychromatic solid-state lamps versus tungsten radiator: hue changes of Munsell samples

    International Nuclear Information System (INIS)

    Stanikunas, R; Vaitkevicius, H; Svegzda, A; Viliunas, V; Bliznikas, Z; Breive, K; Vaicekauskas, R; Novickovas, A; Kurilcik, G; Zukauskas, A; Gaska, R; Shur, M S

    2005-01-01

    Colour-perception differences under illumination by two quadrichromatic solid-state sources of light have been studied with respect to a tungsten radiator with the same correlated colour temperature (2600 K). A virtual RYgCB source (illuminant), which contains red, yellow-green, cyan and blue components with the line width typical of AlGaInP and AlInGaN light-emitting diodes (LEDs), was fully optimized for the highest value of the general colour-rendering index (CRI) (R a = 98.3). An implemented RAGB source (lamp) contained commercially available red, amber, green and blue LEDs (R a 79.4). Colorimetric calculations in the Commission Internationale de l'Eclairage 1976 (u',v') colour plane for 40 Munsell colour samples (value 6, chroma/6, hue increment 2.5) revealed the differences in hue discrimination and distortion for both sources in the yellow-green and blue-cyan ranges. These differences were not revealed by the standard analysis of the special CRIs and were lower for the RYgCB illuminant, which contained primary LEDs in the sensitive ranges. A psychophysical experiment on seven subjects was performed using the RAGB lamp stabilized against thermal and ageing drifts. Despite different colour-perception abilities of the subjects under investigation, the experiment confirmed the calculation results. Methods of obtaining composite white light with high subjective ratings are discussed, based on the obtained data

  12. Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

    Science.gov (United States)

    Barker, S A; Long, A R

    1994-01-01

    The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

  13. Two new solid solutions in calcite-magnesite system identified in a sample from coral reefs in the northern Perth basin

    International Nuclear Information System (INIS)

    Li, D.Y.; O'Connor, B.H.; Zhu, Z.R.; Collins, L.B.; Hunter, B.

    1998-01-01

    Full text: Dolomite, CaMg(CO 3 ) 2 , is an economically important mineral, being of particular significance in petroleum geology. Carbonate rocks have long been a focus of investigation because these rocks contain an estimated 60 percent of the world's recoverable petroleum, and include most of the world's largest reservoirs. Correct phase identification in carbonates has concerned sedimentologists and petroleum geologists for decades. A new type of solid solution in the calcite (CaCO 3 ) - magnesite (MgCO 3 ) system has been identified at Curtin University by Rietveld XRD and neutron diffraction data analysis in a sample from late Pleistocene reefs in the northern Perth Basin. It is known that the structure of calcite (space group R3C) will be transformed to dolomite (R3), which has an ordered distribution of Ca and Mg in the structure, if 50% of its Ca atoms are substituted by Mg in terms of the Ca-Mg atomic ratio. However, the upper limit of Mg substitution for Ca in calcite under sedimentary-geological conditions without there being a change in structure to dolomite is still unknown. Two carbonates examined at Curtin showed Mg substitution for Ca in calcite under coral reef sedimentary conditions of 18.1% and 37.7%, whereas Bragg peak shifts for a 'dolomite, line for these samples were interpreted by geologists as indicative of dolomite with a certain extent of order-disorder distribution between Ca and Mg atoms. The observations have provided an opportunity to re-examine the origins of dolomite and aspects of dolomitization in a coral reef environment in the Quaternary

  14. Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-10-01

    In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Study on solid-liquid interfacial phenomena and advancement of migration model in diffusion and migration processes of radionuclides in buffer materials and rock matrixes for disposal of radioactive wastes

    International Nuclear Information System (INIS)

    Sato, Haruo

    2004-06-01

    properties of porewater in sandstone, and it is discussed on the region of porewater receiving effect from solid surface. In chapter 7, it is reported on distribution coefficients (Kd) for Cs + and I - ions onto sandstone obtained by a batch method, and it is discussed on the consistency between Kd-values from the batch method and the diffusion method performed in chapter 5. In chapter 8, it is discussed on the physical and chemical properties of Horonobe mudstone, which was sampled from Horonobe area, where the construction of underground research laboratory is presently in progress. Finally, chapter 9 is the conclusion, in which information for nuclide diffusion process obtained in a series of studies is summarized. The conclusion for nuclide diffusion process in engineered barrier and natural barrier composing the multi-barrier system of the geological disposal obtained from above studies is summarized as follows. For engineered barrier, the effect of the orientation of clay particles on diffusion and the degree of resistance receive in the diffusion process of ions in compacted bentonite was studied, and the following findings were found out. (1) Clay particles orientate in a constant direction depending on compacted direction and anisotropy is found in diffusivity for a bentonite with high smectite content, (2) there is a possibility that water near solid-liquid interface is structurized by electrostatic effect from solid surface, and (3) diffusive pathway (interlayer, external pores) depends on the charge of diffusing species by electrostatic effect from solid surface, consequently necessary activation energy to diffuse depends on diffusive pathway. For natural barrier, inconsistent factor between retardation in diffusion process and Kd by the batch method on sandstone which is one of the sedimentary rocks was studied, and it was indicated that both Kd-values are approximately consistent by making agree porewater, tracer concentration and specific surface area

  16. Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Feichtmeier, Nadine S; Leopold, Kerstin

    2014-06-01

    In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples.

  17. Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

    Science.gov (United States)

    Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

    2018-04-01

    In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization

    Science.gov (United States)

    Loge, G.

    1994-09-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U3O8. Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF4 were found to be a kinetic bottleneck to the formation of UF6. This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid.

  19. Analytical determination of Chemical Oxygen Demand in samples considered to be difficult to analyse: solid substrates and liquid samples with high suspended solid concentrations

    DEFF Research Database (Denmark)

    Raposo, Francisco; Fernández-Cegrí, V.; De la Rubia, M.A.

    of a general standard method and high quality certified reference materials (CRMs), currently the traceability of the COD determination in such samples is not easy to check. Proficiency testing (PT) is a powerful tool that can be used to test the performance that the participant’s laboratories can achieve. Two...

  20. Laser Tweezer Controlled Solid Immersion Lens for High Resolution Imaging in Microfluidic and Biological Samples

    National Research Council Canada - National Science Library

    Birkbeck, Aaron L; Zlatanovic, Sanja; Ozkan, Mihrimah; Esener, Sadik C

    2005-01-01

    ...). Up to now, solid immersion lens imaging systems have relied upon cantilever-mounted SILs that are difficult to integrate into microfluidic systems and require an extra alignment step with external optics...

  1. Lunar and Meteorite Sample Education Disk Program — Space Rocks for Classrooms, Museums, Science Centers, and Libraries

    Science.gov (United States)

    Allen, J.; Luckey, M.; McInturff, B.; Huynh, P.; Tobola, K.; Loftin, L.

    2010-03-01

    NASA’s Lunar and Meteorite Sample Education Disk Program has Lucite disks containing Apollo lunar samples and meteorite samples that are available for trained educators to borrow for use in classrooms, museums, science center, and libraries.

  2. Open focused microwave-assisted sample preparation for rapid total and mercury species determination in environmental solid samples

    OpenAIRE

    Tseng, C. M.; Garraud, H.; Amouroux, D.; Donard, O. F. X.; de Diego, A.

    1998-01-01

    This paper describes rapid, simple microwave-assisted leaching/ digestion procedures for total and mercury species determination in sediment samples and biomaterials. An open focused microwave system allowed the sample preparation time to be dramatically reduced to only 24 min when a power of 40-80 W was applied. Quantitative leaching of methylmercury from sediments by HNO3 solution and complete dissolution of biomaterials by an alkaline solution, such as 25% TMAH solution, were obtained. Met...

  3. Investigation of uranium 238 level in phosphate rock samples from kurun mountain Eastern Nuba Mountains in the State of Kordfan (western Sudan)

    International Nuclear Information System (INIS)

    Yagoub, N. H. M.

    2014-06-01

    The natural radionuclide content of 20 samples collected from Kurun Mountain, western Sudan, has been determined using gamma spectrometry. The data showed that ''2''3 8 U and its decay products were the principal contributors of radioactivity in phosphate deposits. The range of the activity concentration was measured in apatite phosphate rock samples was 378.03-1332.58 Bq/Kg with a mean value of 815.46 Bq/Kg and the data showed that most of samples concentrated in medial comparable with top and bottom of mountain. The distribution of samples indicated that the weathering effect and the rainfall may be the main reasons to enhance the mobility and solubility of uranium from top to bottom of mountain.(Author)

  4. Moessbauer and XRD Comparative Study of Host Rock and Iron Rich Mineral Samples from Paz del Rio Iron Ore Mineral Mine in Colombia

    International Nuclear Information System (INIS)

    Fajardo, M.; Perez Alcazar, G. A.; Moreira, A. M.; Speziali, N. L.

    2004-01-01

    A comparative study between the host rock and the iron rich mineral samples from the Paz del Rio iron ore mineral mine in Colombia was performed using X-ray diffraction and Moessbauer spectroscopy. Diffraction results of the iron rich mineral sample show that goethite, hematite, quartz, kaolinite and siderite are the main phases, and that a small amount of illite is also present. By Moessbauer spectroscopy at room temperature (RT) the presence of all the above mentioned phases was detected except quartz as well as an additional presence of small amount of biotite. The goethite, which appears as four sextets with hyperfine fields of 33.5, 30.5, 27.5 and 18.5 T, respectively, is the majority phase. This result shows the different grades of formation of this oxyhydroxide. The Moessbauer spectrum of this sample at 80 K presents the same phases obtained at RT without any superparamagnetic effect. In this case the goethite appears as two sextets. Diffraction results of the host rock sample show a large amount of quartz and kaolinite and small amounts of illite and biotite, whereas by Moessbauer spectroscopy illite, kaolinite and biotite were detected.

  5. Study on characteristics of EMR signals induced from fracture of rock samples and their application in rockburst prediction in copper mine

    Science.gov (United States)

    Liu, Xiaofei; Wang, Enyuan

    2018-06-01

    A rockburst is a dynamic disaster that occurs during underground excavation or mining which has been a serious threat to safety. Rockburst prediction and control are as important as any other underground engineering in deep mines. For this paper, we tested electromagnetic radiation (EMR) signals generated during the deformation and fracture of rock samples from a copper mine under uniaxial compression, tension, and cycle-loading experiments, analyzed the changes in the EMR intensity, pulse number, and frequency corresponding to the loading, and a high correlation between these EMR parameters and the applied loading was observed. EMR apparently reflects the deformation and fracture status to the loaded rock. Based on this experimental work, we invented the KBD5-type EMR monitor and used it to test EMR signals generated in the rock surrounding the Hongtoushan copper mine. From the test results, it is determined the responding characteristics of EMR signals generated by changes in mine-generated stresses and stress concentrations and it is proposed that this EMR monitoring method can be used to provide early warning for rockbursts.

  6. Development of a fully automated open-column chemical-separation system—COLUMNSPIDER—and its application to Sr-Nd-Pb isotope analyses of igneous rock samples

    Science.gov (United States)

    Miyazaki, Takashi; Vaglarov, Bogdan Stefanov; Takei, Masakazu; Suzuki, Masahiro; Suzuki, Hiroaki; Ohsawa, Kouzou; Chang, Qing; Takahashi, Toshiro; Hirahara, Yuka; Hanyu, Takeshi; Kimura, Jun-Ichi; Tatsumi, Yoshiyuki

    A fully automated open-column resin-bed chemical-separation system, named COLUMNSPIDER, has been developed. The system consists of a programmable micropipetting robot that dispenses chemical reagents and sample solutions into an open-column resin bed for elemental separation. After the initial set up of resin columns, chemical reagents, and beakers for the separated chemical components, all separation procedures are automated. As many as ten samples can be eluted in parallel in a single automated run. Many separation procedures, such as radiogenic isotope ratio analyses for Sr and Nd, involve the use of multiple column separations with different resin columns, chemical reagents, and beakers of various volumes. COLUMNSPIDER completes these separations using multiple runs. Programmable functions, including the positioning of the micropipetter, reagent volume, and elution time, enable flexible operation. Optimized movements for solution take-up and high-efficiency column flushing allow the system to perform as precisely as when carried out manually by a skilled operator. Procedural blanks, examined for COLUMNSPIDER separations of Sr, Nd, and Pb, are low and negligible. The measured Sr, Nd, and Pb isotope ratios for JB-2 and Nd isotope ratios for JB-3 and BCR-2 rock standards all fall within the ranges reported previously in high-accuracy analyses. COLUMNSPIDER is a versatile tool for the efficient elemental separation of igneous rock samples, a process that is both labor intensive and time consuming.

  7. Application of the collapsing method to acoustic emissions in a rock salt sample during a triaxial compression experiment

    International Nuclear Information System (INIS)

    Manthei, G.; Eisenblaetter, J.; Moriya, H.; Niitsuma, H.; Jones, R.H.

    2003-01-01

    Collapsing is a relatively new method. It is used for detecting patterns and structures in blurred and cloudy pictures of multiple soundings. In the case described here, the measurements were made in a very small region with a length of only a few decimeters. The events were registered during a triaxial compression experiment on a compact block of rock salt. The collapsing method showed a cellular structure of the salt block across the whole length of the test piece. The cells had a length of several cm, enclosing several grains of salt with an average grain size of less than one cm. In view of the fact that not all cell walls corresponded to acoustic emission events, it was assumed that only those grain boundaries are activated that are oriented at a favourable angle to the field of tension of the test piece [de

  8. A feasibility study of U-Pb and Pb-Pb dating of kimberlites using groundmass mineral fractions and whole-rock samples

    International Nuclear Information System (INIS)

    Kramers, J.D.; Smith, C.B.

    1983-01-01

    This paper describes partly successful attempts to determine emplacement ages of kimberlites by U-Pb and Pb-Pb methods involving groundmass minerals with high U content (notably perovskite) and whole-rock kimberlite samples. U/Pb ratios in perovskite in the matrix of kimberlites can be two orders of magnitude larger than in the rest of the kimberlite material, and with simple mineral separation techniques moderate success was achieved in U-Pb dating of fresh samples of younger kimberlites (around 100 Ma). The differences in U/Pb ratios between kimberlite samples from different parts of the same pipe have also been found to be large enough, in some cases, to allow reasonably accurate U-Pb age determination. In older kimberlites the U-Pb ages obtained were mostly imcompatible with geological constraints and results obtained by other methods. However, for such pipes use of Pb-Pb systematics yields realistic age limits in some cases

  9. Measuring Sulfur Isotope Ratios from Solid Samples with the Sample Analysis at Mars Instrument and the Effects of Dead Time Corrections

    Science.gov (United States)

    Franz, H. B.; Mahaffy, P. R.; Kasprzak, W.; Lyness, E.; Raaen, E.

    2011-01-01

    The Sample Analysis at Mars (SAM) instrument suite comprises the largest science payload on the Mars Science Laboratory (MSL) "Curiosity" rover. SAM will perform chemical and isotopic analysis of volatile compounds from atmospheric and solid samples to address questions pertaining to habitability and geochemical processes on Mars. Sulfur is a key element of interest in this regard, as sulfur compounds have been detected on the Martian surface by both in situ and remote sensing techniques. Their chemical and isotopic composition can belp constrain environmental conditions and mechanisms at the time of formation. A previous study examined the capability of the SAM quadrupole mass spectrometer (QMS) to determine sulfur isotope ratios of SO2 gas from a statistical perspective. Here we discuss the development of a method for determining sulfur isotope ratios with the QMS by sampling SO2 generated from heating of solid sulfate samples in SAM's pyrolysis oven. This analysis, which was performed with the SAM breadboard system, also required development of a novel treatment of the QMS dead time to accommodate the characteristics of an aging detector.

  10. Solid-state potentiometric biosensors for pH quantification in biological samples

    NARCIS (Netherlands)

    Ivan, M.G.; Wiegersma, S.; Sweelssen, J.; Saalmink, M.; Boersma, A.

    2011-01-01

    This paper reports on manufacturing and characterization of an all-solid-state potentiometric sensor aimed at monitoring pH in dialysate or blood plasma for patients who undergo dialysis. The sensing polymer-based membrane, coated on top of the Au working electrodes, contains a polymer matrix -

  11. Determination of structure of oriented samples using two-dimensional solid state NMR techniques

    International Nuclear Information System (INIS)

    Jin Hong; Harbison, G.S.

    1990-01-01

    One dimensional and two-dimensional MAS techniques can give detailed information about the structure and dynamics of oriented systems. We describe the application of such techniques to the liquid-crystalline polymer poly(p-phenyleneterphtalimide) (PPTA), and thence deduce the solid-state structure of the material. (author). 9 refs.; 6 figs

  12. Solvent-assisted dispersive solid-phase extraction: A sample preparation method for trace detection of diazinon in urine and environmental water samples.

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-09-02

    In this research, a sample preparation method termed solvent-assisted dispersive solid-phase extraction (SA-DSPE) was applied. The used sample preparation method was based on the dispersion of the sorbent into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was received by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the diazinon, the cloudy solution was centrifuged and diazinon in the sediment phase dissolved in ethanol and determined by gas chromatography-flame ionization detector. Under the optimized conditions (pH of solution=7.0, Sorbent: benzophenone, 2%, Disperser solvent: ethanol, 500μL, Centrifuge: centrifuged at 4000rpm for 3min), the method detection limit for diazinon was 0.2, 0.3, 0.3 and 0.3μgL(-1) for distilled water, lake water, waste water and urine sample, respectively. Furthermore, the pre-concentration factor was 363.8, 356.1, 360.7 and 353.38 in distilled water, waste water, lake water and urine sample, respectively. SA-DSPE was successfully used for trace monitoring of diazinon in urine, lake and waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of boron in plant tissues

    International Nuclear Information System (INIS)

    Resano, M.; Briceno, J.; Aramendia, M.; Belarra, M.A.

    2007-01-01

    In this work, the potential of graphite furnace atomic absorption spectrometry for the direct determination of B in plant tissues has been investigated. Three certified reference materials (NIST SRM 1570a spinach leaves, NIST SRM 1573a tomato leaves and BCR CRM 679 white cabbage) were selected for this study, the goal always being to develop a fast procedure that could be robust enough to provide a satisfactory performance for all of them, without any modifications in the conditions applied. The use of a suitable chemical modifier was found to be essential for obtaining a reproducible and sufficiently sensitive signal for boron solutions. In this regard, the performance of the combination of citric acid plus W (added as a permanent modifier) was noteworthy, resulting in well-defined signal profiles, a remarkable analyte stabilization during the pyrolysis step (up to 2100 deg. C) and minimal memory effects. This mixture of modifiers provided a good performance for the direct analysis of solid samples as well, but only if a suitable temperature program, favoring the interaction between the analyte and the modifiers, was used. Thus, such a temperature program, with two pyrolysis steps and the addition of NH 4 NO 3 in order to carry out the in situ sample microdigestion, was optimized. Under these conditions, the peak areas obtained for both solid samples and aqueous standards were comparable. Finally, the analysis of the samples was carried out. In all cases, a good agreement with the certified values was obtained, while R.S.D. values ranged between 6 and 10%. It can be concluded that the method proposed shows significant advantages for the determination of this complicated element in solid samples such as the use of aqueous standards for calibration, a high sample throughput (20 min per sample), a suitable limit of detection (0.3 μg g -1 ) and reduced risk of analyte losses and contamination

  14. Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Cabalin, L.M.; Gonzalez, A. [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain); Ruiz, J. [Department of Applied Physics I, University of Malaga, E-29071 Malaga (Spain); Laserna, J.J., E-mail: laserna@uma.e [Department of Analytical Chemistry, University of Malaga, E-29071 Malaga (Spain)

    2010-08-15

    Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s{sup -1}. Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

  15. Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

    Science.gov (United States)

    Cabalín, L. M.; González, A.; Ruiz, J.; Laserna, J. J.

    2010-08-01

    Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s - 1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

  16. Assessment of statistical uncertainty in the quantitative analysis of solid samples in motion using laser-induced breakdown spectroscopy

    International Nuclear Information System (INIS)

    Cabalin, L.M.; Gonzalez, A.; Ruiz, J.; Laserna, J.J.

    2010-01-01

    Statistical uncertainty in the quantitative analysis of solid samples in motion by laser-induced breakdown spectroscopy (LIBS) has been assessed. For this purpose, a LIBS demonstrator was designed and constructed in our laboratory. The LIBS system consisted of a laboratory-scale conveyor belt, a compact optical module and a Nd:YAG laser operating at 532 nm. The speed of the conveyor belt was variable and could be adjusted up to a maximum speed of 2 m s -1 . Statistical uncertainty in the analytical measurements was estimated in terms of precision (reproducibility and repeatability) and accuracy. The results obtained by LIBS on shredded scrap samples under real conditions have demonstrated that the analytical precision and accuracy of LIBS is dependent on the sample geometry, position on the conveyor belt and surface cleanliness. Flat, relatively clean scrap samples exhibited acceptable reproducibility and repeatability; by contrast, samples with an irregular shape or a dirty surface exhibited a poor relative standard deviation.

  17. Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies

    CERN Document Server

    Crotti, C; Celestino, T; Fontana, S

    2003-01-01

    The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO) sub 4 (dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating techniqu...

  18. Characterization and quantification by mass spectrometry of mobile organic matter from clay rock: influence of the origin and of the sampling

    International Nuclear Information System (INIS)

    Huclier-Markai, S.; Landesman, C.; Montavon, G.; Grambow, B.; Monteau, F.; Fernandez, A.M.; Vinsot, A.

    2012-01-01

    Document available in extended abstract form only. In environmental studies, Natural Organic Matter (NOM) plays a key role on the bioavailability and the toxicity of metallic compounds. If one wants to evaluate the mobility of heavy metals / radionuclides, which is in natura in most of the cases dependant on their interactions with NOM. One part of the organic inventory in the Callovo-Oxfordian formation (COx) exists as small dissolved compounds in the pore water but the weak content and the weak porosity of the formation (∼ 8 % of water in weight) make the complexation study with metal ions difficult. One part of the organic matter attached to the sediment (∼ 1 % in weight) can be mobilized in a synthetic pore water 1 and can be considered as similar to in situ pore water dissolved organic matter (DOM) regarding its size distribution. The collection of clay pore water has been done through percolation experiment, a unique and original experimental process developed to get pore water from a core sample,that have been described previously. From these experiments, it was shown that mobile organic matter concentration could reach 0.01 mol C/L by application of a pressure gradient up to 100 bars. Since part of the OM from the COx is known to be sensitive to air oxidation, the characterization and quantification of DOM were then performed under anoxic conditions (about - 170 mV vs Standard Hydrogen Electrode SHE). In addition, the chemical composition of NOM contained in the pore water from the argillite clay rock has been determined in in-situ like conditions by ESI-MS and APCI-MS, which are suitable techniques to identify the chemical composition of NOM contained in the COx pore water available from boreholes. Mostly low molecular weight molecules were identified, of whom structural features observed were mainly acidic compounds, fatty acids as well as aldehydes and amino acids. Fulvic and Humic Acids have such low concentrations in the COx formation, leading to a

  19. Computer aided testing of steel samples deformation at coexistence liquid and solid phase

    International Nuclear Information System (INIS)

    Hojny, M.; Glowacki, M.

    2007-01-01

    The paper reports the results of experimental and theoretical work leading to construction of a CAE system dedicated to the numerical simulation of plastic deformation of steel at coexistence liquid and solid phase. A coupled thermal-mechanical model including inverse analysis technique was adopted for the solver. The advantage of the solution was the analytical form of both incompressibility and mass conservation conditions. This can prevent usual FEM variational solution problems concerning unintentional specimen volume loss caused by the numerical errors. The only well known machine allowing tests in the discussed temperature range is the GLEEBLE thermo-mechanical simulator. Experiments of deformation of steel in semi-solid state by using this machine are very expensive. Therefore, application of dedicated computer simulation system with inverse method makes tests possible and results in lowering testing cost

  20. Rock fragmentation

    Energy Technology Data Exchange (ETDEWEB)

    Brown, W.S.; Green, S.J.; Hakala, W.W.; Hustrulid, W.A.; Maurer, W.C. (eds.)

    1976-01-01

    Experts in rock mechanics, mining, excavation, drilling, tunneling and use of underground space met to discuss the relative merits of a wide variety of rock fragmentation schemes. Information is presented on novel rock fracturing techniques; tunneling using electron beams, thermocorer, electric spark drills, water jets, and diamond drills; and rock fracturing research needs for mining and underground construction. (LCL)

  1. Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

    OpenAIRE

    Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma; Abdel-Rehim, Mohamed

    2014-01-01

    In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from o...

  2. Rb-Sr systematics in drill core samples of the Eye-Dashwa Lakes pluton at the whole rock and mineral scale

    International Nuclear Information System (INIS)

    Peterman, Z.E.; Futa, K.; Kamineni, D.C.

    1990-01-01

    Twenty-one whole-rock samples from boreholes ATK-1 and ATK-6 define a precise Rb-Sr isochron with an age of 2637 ± 33 Ma and initial 87 Sr/ 86 Sr intercept, IR(Sr), of 0.70144 ± 0.00006. An internal mineral isochron for ATC-1 (991-997) and biotites from ATK-1 (35.63) and ATK-1 (3.84) give younger ages of 2541 ± 14 Ma 2574 ± 25 Ma, and 2534 ± 25 Ma, respectively. Data for samples from fracture zones scatter but correlate around an isochron of 2281 ± 153 Ma. The internal isochron and biotite ages record cooling below about 300 C due to uplift and erosion. The younger age, 2281 ± 153 Ma, records an episode or episodes of brittle failure at relatively high crustal levels. These fractures provided pathways for infiltration of water, which facilitated the mineralogical alteration

  3. Development of Solid Ceramic Dosimeters for the Time-Integrative Passive Sampling of Volatile Organic Compounds in Waters.

    Science.gov (United States)

    Bonifacio, Riza Gabriela; Nam, Go-Un; Eom, In-Yong; Hong, Yong-Seok

    2017-11-07

    Time-integrative passive sampling of volatile organic compounds (VOCs) in water can now be accomplished using a solid ceramic dosimeter. A nonporous ceramic, which excludes the permeation of water, allowing only gas-phase diffusion of VOCs into the resin inside the dosimeter, effectively captured the VOCs. The mass accumulation of 11 VOCs linearly increased with time over a wide range of aqueous-phase concentrations (16.9 to 1100 μg L -1 ), and the linearity was dependent upon the Henry's constant (H). The average diffusivity of the VOCs in the solid ceramic was 1.46 × 10 -10 m 2 s -1 at 25 °C, which was 4 orders of magnitude lower than that in air (8.09 × 10 -6 m 2 s -1 ). This value was 60% greater than that in the water-permeable porous ceramic (0.92 × 10 -10 m 2 s -1 ), suggesting that its mass accumulation could be more effective than that of porous ceramic dosimeters. The mass accumulation of the VOCs in the solid ceramic dosimeter increased in the presence of salt (≥0.1 M) and with increasing temperature (4 to 40 °C) but varied only slightly with dissolved organic matter concentration. The solid ceramic dosimeter was suitable for the field testing and measurement of time-weighted average concentrations of VOC-contaminated waters.

  4. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    International Nuclear Information System (INIS)

    Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; Furtado da Silva, Alessandra; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson Jose

    2005-01-01

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1

  5. Sample preparation composite and replicate strategy for assay of solid oral drug products.

    Science.gov (United States)

    Harrington, Brent; Nickerson, Beverly; Guo, Michele Xuemei; Barber, Marc; Giamalva, David; Lee, Carlos; Scrivens, Garry

    2014-12-16

    In pharmaceutical analysis, the results of drug product assay testing are used to make decisions regarding the quality, efficacy, and stability of the drug product. In order to make sound risk-based decisions concerning drug product potency, an understanding of the uncertainty of the reportable assay value is required. Utilizing the most restrictive criteria in current regulatory documentation, a maximum variability attributed to method repeatability is defined for a drug product potency assay. A sampling strategy that reduces the repeatability component of the assay variability below this predefined maximum is demonstrated. The sampling strategy consists of determining the number of dosage units (k) to be prepared in a composite sample of which there may be a number of equivalent replicate (r) sample preparations. The variability, as measured by the standard error (SE), of a potency assay consists of several sources such as sample preparation and dosage unit variability. A sampling scheme that increases the number of sample preparations (r) and/or number of dosage units (k) per sample preparation will reduce the assay variability and thus decrease the uncertainty around decisions made concerning the potency of the drug product. A maximum allowable repeatability component of the standard error (SE) for the potency assay is derived using material in current regulatory documents. A table of solutions for the number of dosage units per sample preparation (r) and number of replicate sample preparations (k) is presented for any ratio of sample preparation and dosage unit variability.

  6. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

    Science.gov (United States)

    Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

    2018-01-01

    Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

  7. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

    Directory of Open Access Journals (Sweden)

    Ireneusz Sowa

    2018-03-01

    Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

  8. Interfering removal in samples with high amounts of dissolved solids for the determination of arsenic and selenium by TXRF

    International Nuclear Information System (INIS)

    Menegario, Amauri A.; Gomes, Ana Carla F.; Pellegrinotti, Daniel C.; Gine, Maria F.; Krug, Francisco J.; Nascimento Filho, Virgilio F.

    2002-01-01

    A matrix separation flow system coupled with total reflection X-ray fluorescence (TXRF) is proposed to remove Ca ++ , Mg ++ , Na + and K + major cations from samples containing high amounts of totally dissolved solids, using solid-liquid phases in flow system. This system is assembled with a 1.25 mL column of AG50W-X8 resin (in protonated form) and manual commutator, allowed the separation, addition of internal standard and subsequently a 40 μL aliquot of the eluate was deposited in the reflector support, dried in a furnace for 12 hours at 60 ± 5 deg C and analysed by TXRF. All the procedure is carried out in about 90 s and 0.5 mL of sample are required. The proposed approach was applied for determination of As and Se in plant material and sea water samples. When comparing with direct analysis (without separation), a reduction of 2 to 6 times on the limits of detection for these elements was attained. The accuracy of this methodology was satisfactory for As and Se in sea water and Se in rice certified samples. This procedure could be also used for Pb interference removal in the determination of As by X-ray fluorescence. (author)

  9. Development of near-field laser ablation inductively coupled plasma mass spectrometry for sub-micrometric analysis of solid samples

    International Nuclear Information System (INIS)

    Jabbour, Chirelle

    2016-01-01

    A near field laser ablation method was developed for chemical analysis of solid samples at sub-micrometric scale. This analytical technique combines a nanosecond laser Nd:YAG, an atomic Force Microscope (AFM), and an inductively coupled plasma mass spectrometer (ICPMS). In order to improve the spatial resolution of the laser ablation process, the near-field enhancement effect was applied by illuminating, by the laser beam, the apex of the AFM conductive sharp tip maintained at a few nanometers (5 to 30 nm) above the sample surface. The interaction between the illuminated tip and the sample surface enhances locally the incident laser energy and leads to the ablation process. By applying this technique to conducting gold and tantalum samples, and semiconducting silicon sample, a lateral resolution of 100 nm and depths of a few nanometers were demonstrated. Two home-made numerical codes have enabled the study of two phenomena occurring around the tip: the enhancement of the laser electrical field by tip effect, and the induced laser heating at the sample surface. The influence of the main operating parameters on these two phenomena, amplification and heating, was studied. an experimental multi-parametric study was carried out in order to understand the effect of different experimental parameters (laser fluence, laser wavelength, number of laser pulses, tip-to-sample distance, sample and tip nature) on the near-field laser ablation efficiency, crater dimensions and amount of ablated material. (author) [fr

  10. Visualization and quantification of heterogeneous diffusion rates in granodiorite samples by X-ray absorption imaging. Diffusion within gouge materials, altered rim and intact rock matrix

    International Nuclear Information System (INIS)

    Altman, S.J.; Tidwell, V.C.; Uchida, M.

    2001-01-01

    Matrix diffusion is one of the most important contaminant migration retardation processes in crystalline rocks. Performance assessment calculations in various countries assume that only the area of the fracture surface where advection is active provides access to the rock matrix. However, accessibility to the matrix could be significantly enhanced with diffusion into stagnant zones, fracture fillings, and through an alteration rim in the matrix. Laboratory visualization experiments were conducted on granodiorite samples to investigate and quantify diffusion rates within different zones of a Cretaceous granodiorite. Samples were collected from the Kamaishi experimental site in the northern part of the main island of Japan. Diffusion of iodine out of the sample is visualized and rates are measured using x-ray absorption imaging. X-ray images allow for measurements of relative iodine concentration and relative iodine mass as a function of time and two-dimensional space at a sub-millimeter spatial resolution. In addition, two-dimensional heterogeneous porosity fields (at the same resolution as the relative concentration fields) are measured. This imaging technique allows for a greater understanding of the spatial variability of diffusion rates than can be accomplished with standard bulk measurements. It was found that diffusion rates were fastest in partially gouge-filled fractures. Diffusion rates in the recrystallized calcite-based fracture-filling material were up to an order of magnitude lower than in gouge-filled fractures. Diffusion in altered matrix around the fractures was over an order of magnitude lower than that in the gouge-filled fractures. Healed fractures did not appear to have different diffusion rates than the unaltered matrix

  11. Visualization and quantification of heterogeneous diffusion rates in granodiorite samples by X-ray absorption imaging. Diffusion within gouge materials, altered rim and intact rock matrix

    Energy Technology Data Exchange (ETDEWEB)

    Altman, S.J.; Tidwell, V.C. [Sandia National Laboratories, Albuquerque, NM (United States); Uchida, M. [Japan Nuclear Cycle Development Inst., Ibaraki (Japan)

    2001-08-01

    Matrix diffusion is one of the most important contaminant migration retardation processes in crystalline rocks. Performance assessment calculations in various countries assume that only the area of the fracture surface where advection is active provides access to the rock matrix. However, accessibility to the matrix could be significantly enhanced with diffusion into stagnant zones, fracture fillings, and through an alteration rim in the matrix. Laboratory visualization experiments were conducted on granodiorite samples to investigate and quantify diffusion rates within different zones of a Cretaceous granodiorite. Samples were collected from the Kamaishi experimental site in the northern part of the main island of Japan. Diffusion of iodine out of the sample is visualized and rates are measured using x-ray absorption imaging. X-ray images allow for measurements of relative iodine concentration and relative iodine mass as a function of time and two-dimensional space at a sub-millimeter spatial resolution. In addition, two-dimensional heterogeneous porosity fields (at the same resolution as the relative concentration fields) are measured. This imaging technique allows for a greater understanding of the spatial variability of diffusion rates than can be accomplished with standard bulk measurements. It was found that diffusion rates were fastest in partially gouge-filled fractures. Diffusion rates in the recrystallized calcite-based fracture-filling material were up to an order of magnitude lower than in gouge-filled fractures. Diffusion in altered matrix around the fractures was over an order of magnitude lower than that in the gouge-filled fractures. Healed fractures did not appear to have different diffusion rates than the unaltered matrix.

  12. An analytical protocol for the determination of total mercury concentrations in solid peat samples

    DEFF Research Database (Denmark)

    Roos-Barraclough, F; Givelet, N; Martinez-Cortizas, A

    2002-01-01

    Traditional peat sample preparation methods such as drying at high temperatures and milling may be unsuitable for Hg concentration determination in peats due to the possible presence of volatile Hg species, which could be lost during drying. Here, the effects of sample preparation and natural.......12 and 8.52 ng kg(-1) h(-1), respectively). Fertilising the peat slightly increased Hg loss (3.08 ng kg(-1) h(-1) in NPK-fertilised peat compared to 0.28 ng kg(-1) h(-1) in unfertilised peat, when averaged over all temperatures used). Homogenising samples by grinding in a machine also caused a loss of Hg....... A comparison of two Hg profiles from an Arctic peat core, measured in frozen samples and in air-dried samples, revealed that no Hg losses occurred upon air-drying. A comparison of Hg concentrations in several plant species that make up peat, showed that some species (Pinus mugo, Sphagnum recurvum...

  13. Investigation of uranium238, potassium40 and thorium232 level in soil and rock sample from North and South of Kurdofan state ( Western Sudan)

    International Nuclear Information System (INIS)

    Osman, Alshfia Hashiem

    2015-04-01

    In this study 40 soil and rock samples were collected from eight locations (A.B.C.G) F present tow location, 500 grams of soil and rock sample was weighed and closed in plastic containers for weeks so to have secular equilibrium for uranium. Our goal of this study was estimate from North and South of Kurdofan state (Western Sudan). natural radioactivity concentrations in soil rock sample were measured by gamma-ray spectrometry using Nal (TI), calibration process carried out for gamma spectroscopy using MW652 as a reference source -Cs-137 and Co-60 with two energy levels. The concentration of K-40 in location A was found to be range (347.78-51,67)Bq/kg in locations B was found to be range (169,90-125,54)Bq/kg in location C was found to be range (152,14-34,47)Bq/kg in location D was found to be range ( 396. 26-49.90)Bq/kg in location E was found to be range ( 168.70-127.70)Bq/kg in location F was found to be range (432.5-200.1)Bq/kg and in location G was found to be range (684.41-347.86)Bq/kg. The concentration of U-238 in location A was found to be range (483.133-19.4) Bq/kg in location B was found to be range (50.24-24.94)Bq/kg in location C was found to be range ( 69.11-10.58) Bq/kg in location D was found to be range (52.50-15.06)Bq/kg in location E was found to be range (56.66-49.6)Bq/kg in location E was found to be range (56.66-49)Bq/kg in location F was found to be range (46.01-19.40)Bq/kg in location A was found to be range (3227.8-40)Bq/kg in location B was found to be range (88.62-40.04) Bq/Kg in location C was found to be range (119.05-14.04) Bq/kg in location D was found to be range (51.62-16.96)Bq/kg in location E was found to be range (43.89-39.84) Bq/kg in location F was found to be range ( 46.18-24.40)Bq/kg and in location G was found to be range (201.05-137.34)Bq/kg.(Author)

  14. Solid-Phase Extraction Strategies to Surmount Body Fluid Sample Complexity in High-Throughput Mass Spectrometry-Based Proteomics

    Science.gov (United States)

    Bladergroen, Marco R.; van der Burgt, Yuri E. M.

    2015-01-01

    For large-scale and standardized applications in mass spectrometry- (MS-) based proteomics automation of each step is essential. Here we present high-throughput sample preparation solutions for balancing the speed of current MS-acquisitions and the time needed for analytical workup of body fluids. The discussed workflows reduce body fluid sample complexity and apply for both bottom-up proteomics experiments and top-down protein characterization approaches. Various sample preparation methods that involve solid-phase extraction (SPE) including affinity enrichment strategies have been automated. Obtained peptide and protein fractions can be mass analyzed by direct infusion into an electrospray ionization (ESI) source or by means of matrix-assisted laser desorption ionization (MALDI) without further need of time-consuming liquid chromatography (LC) separations. PMID:25692071

  15. Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

    Science.gov (United States)

    Sporkert, Frank; Pragst, Fritz; Hübner, Sandra; Mills, Graham

    2002-05-25

    A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

  16. Polychlorinated biphenyls (PCB) analysis report for solid sample for 219S tank 102

    International Nuclear Information System (INIS)

    Ross, G.A.

    1997-01-01

    One waste sample was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Extraction follows closely method 354 C of SW-846, analysis follows SW-846 method 8082. A cross reference of laboratory sample number to the customer identification is given in a table

  17. Simultaneous Determination of TetracyclinesResidues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method

    Directory of Open Access Journals (Sweden)

    Mehra Mesgari Abbasi

    2011-06-01

    Full Text Available Introduction:Tetracyclines (TCs are widely used in animal husbandry and their residues in milk may resultinharmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. Methods:One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC method using Fluorescence detector.Results: The mean of total TCs residues in all samples (114 samples was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g. Conclusion:This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

  18. Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum samples.

    Science.gov (United States)

    Sajid, Muhammad; Basheer, Chanbasha

    2016-07-15

    In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples.

    Science.gov (United States)

    Ghaedi, M; Ahmadi, F; Soylak, M

    2007-08-17

    A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni2+, Cu2+ and Co2+ ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 microg L(-1) for copper, 0.75 microg L(-1) for nickel and 0.80 microg L(-1) for cobalt. The loading capacity was 0.56 mg g(-1) for Ni2+, 0.50 mg g(-1) for Cu2+ and 0.47 mg g(-1) for Co2+. The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n=3).

  20. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

  1. Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples

    International Nuclear Information System (INIS)

    Ghaedi, M.; Ahmadi, F.; Soylak, M.

    2007-01-01

    A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni 2+ , Cu 2+ and Co 2+ ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 μg L -1 for copper, 0.75 μg L -1 for nickel and 0.80 μg L -1 for cobalt. The loading capacity was 0.56 mg g -1 for Ni 2+ , 0.50 mg g -1 for Cu 2+ and 0.47 mg g -1 for Co 2+ . The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n = 3)

  2. Preconcentration and separation of nickel, copper and cobalt using solid phase extraction and their determination in some real samples

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, M. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of)]. E-mail: m_ghaedi@mail.yu.ac.ir; Ahmadi, F. [Gachsaran Azad University, Gachsaran (Iran, Islamic Republic of); Soylak, M. [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2007-08-17

    A solid phase extraction method has been developed to separate and concentrate trace amounts of nickel, cobalt and copper ions from aqueous samples for the measurement by flame atomic absorption spectrometry. By the passage of aqueous samples through activated carbon modified by dithioxamide (rubeanic acid) (DTO), Ni{sup 2+}, Cu{sup 2+} and Co{sup 2+} ions adsorb quantitatively. The recoveries of analytes at pH 5.5 with 500 mg solid phase were greater than 95% without interference from alkaline, earth alkaline and some metal ions. The enrichment factor was 330. The detection limits by three sigma were 0.50 {mu}g L{sup -1} for copper, 0.75 {mu}g L{sup -1} for nickel and 0.80 {mu}g L{sup -1} for cobalt. The loading capacity was 0.56 mg g{sup -1} for Ni{sup 2+}, 0.50 mg g{sup -1} for Cu{sup 2+} and 0.47 mg g{sup -1} for Co{sup 2+}. The presented procedure was applied to the determination of analytes in tap, river and sea waters, vegetable, soil and blood samples with successfully results (recoveries greater than 95%, R.S.D. lower than 2% for n = 3)

  3. Molecularly Imprinted Polymers (MIP for Selective Solid Phase Extraction of Celecoxib in Urine Samples Followed by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Saeedeh Ansari

    2017-09-01

    Full Text Available In this study, for the analysis of human urine samples, a novel method explained for the determination of celecoxib, a nonsteroidal anti-inflammatory drug (NSAID, using molecularly imprinted solid-phase extraction (MISPE coupled with high-performance liquid chromatography (HPLC. The synthesis of the MIP was performed by precipitation polymerization in methacrylic acid (MAA, ethylene glycol dimethacrylate (EGDMA, chloroform, 2,2′-azobisisobutyronitrile (AIBN and celecoxib as the functional monomer, cross-linker monomer, solvent, initiator and target drug, respectively. The celecoxib imprinted polymer was utilized as a specific sorbent for the solid phase extraction (SPE of celecoxib from samples. The molecularly imprinted polymer (MIP performance was compared with the synthesized non-molecularly imprinted polymer (NIP. Scanning electron microscopy (SEM, FT-IR spectroscopy, UV-VIS spectrophotometry and thermogravimetric analysis (TGA/DTG were used for characterizing the synthesized polymers. Moreover, the MISPE procedure parameters such as pH, eluent solvent flow rate, eluent volume and sorbent mass that probably influence the extraction process have been optimized to achieve the highest celecoxib extraction efficiency. The relative standard deviation (RSD %, recovery percent, limit of detection (LOD and limit of quantification (LOQ of this proposed method were 1.12%, 96%, 8 µg L-1 and 26.7 µg L-1, respectively. The proposed MISPE-HPLC-UV method can be used for the separation and enrichment of trace amounts of celecoxib in human urine and biological samples.

  4. Solid Matter

    CERN Document Server

    Angelo, Joseph A

    2011-01-01

    Supported by a generous quantity of full-color illustrations and interesting sidebars, Solid Matter introduces the basic characteristics and properties of solid matter. It briefly describes the cosmic connection of the elements, leading readers through several key events in human pre-history that resulted in more advanced uses of matter in the solid state. Chapters include:. -Solid Matter: An Initial Perspective. -Physical Behavior of Matter. -The Gravity of Matter. -Fundamentals of Materials Science. -Rocks and Minerals. -Metals. -Building Materials. -Carbon Earth's Most Versatile Element. -S

  5. Novel Electrosorption-Enhanced Solid-Phase Microextraction Device for Ultrafast In Vivo Sampling of Ionized Pharmaceuticals in Fish.

    Science.gov (United States)

    Qiu, Junlang; Wang, Fuxin; Zhang, Tianlang; Chen, Le; Liu, Yuan; Zhu, Fang; Ouyang, Gangfeng

    2018-01-02

    Decreasing the tedious sample preparation duration is one of the most important concerns for the environmental analytical chemistry especially for in vivo experiments. However, due to the slow mass diffusion paths for most of the conventional methods, ultrafast in vivo sampling remains challenging. Herein, for the first time, we report an ultrafast in vivo solid-phase microextraction (SPME) device based on electrosorption enhancement and a novel custom-made CNT@PPY@pNE fiber for in vivo sampling of ionized acidic pharmaceuticals in fish. This sampling device exhibited an excellent robustness, reproducibility, matrix effect-resistant capacity, and quantitative ability. Importantly, the extraction kinetics of the targeted ionized pharmaceuticals were significantly accelerated using the device, which significantly improved the sensitivity of the SPME in vivo sampling method (limits of detection ranged from 0.12 ng·g -1 to 0.25 ng·g -1 ) and shorten the sampling time (only 1 min). The proposed approach was successfully applied to monitor the concentrations of ionized pharmaceuticals in living fish, which demonstrated that the device and fiber were suitable for ultrafast in vivo sampling and continuous monitoring. In addition, the bioconcentration factor (BCF) values of the pharmaceuticals were derived in tilapia (Oreochromis mossambicus) for the first time, based on the data of ultrafast in vivo sampling. Therefore, we developed and validated an effective and ultrafast SPME sampling device for in vivo sampling of ionized analytes in living organisms and this state-of-the-art method provides an alternative technique for future in vivo studies.

  6. Selective solid-phase extraction of Ni(II) by an ion-imprinted polymer from water samples

    International Nuclear Information System (INIS)

    Saraji, Mohammad; Yousefi, Hamideh

    2009-01-01

    A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor (α r ) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 μg L -1 using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.

  7. Comparison of 22G reverse-beveled versus standard needle for endoscopic ultrasound-guided sampling of solid pancreatic lesions

    Science.gov (United States)

    Alatawi, Abdullah; Beuvon, Frédéric; Grabar, Sophie; Leblanc, Sarah; Chaussade, Stanislas; Terris, Benoit; Barret, Maximilien

    2015-01-01

    Objectives Endoscopic ultrasound-guided fine-needle aspiration (EUS-FNA) using standard needles has a high diagnostic value in the evaluation of solid pancreatic masses. Fenestrated needles have been developed to improve the quality of EUS-guided tissue sampling by providing core biopsies (FNB). Methods Patients with solid pancreatic masses of >2 cm were prospectively included in our study and randomized to receive EUS sampling, using either a standard 22G FNA or a 22G Procore® FNB needle. The main study endpoint was the number of needle passes required to obtain a diagnosis in more than 90% of cases. Results We included 100 patients (male = 63, female = 37; mean age = 68.4 years) in our study. We found that 88% of the lesions were malignant, with a mean size of 32 mm. A sample adequate for diagnosis was obtained in more than 90% of cases after the second needle pass in the FNB group, versus the third needle pass in the FNA group. Slide cellularity and presence of tissue microfragments were significantly higher in the FNB group. Sensitivity for the diagnosis of malignancy was 88.4% versus 97.8% for the EUS-FNA and EUS-FNB group, respectively, while specificity for both techniques was 100%. No complications were recorded. Conclusions Although the accuracy of both needle types for proving malignancy was similar, a lower number of passes was required with the FNB needles to achieve the same contributive sample rate as with the FNA needles. FNB also improved the histopathological quality of specimens, suggesting an overall superiority of FNB sampling. PMID:26279842

  8. Micelle assisted thin-film solid phase microextraction: a new approach for determination of quaternary ammonium compounds in environmental samples.

    Science.gov (United States)

    Boyacı, Ezel; Pawliszyn, Janusz

    2014-09-16

    Determination of quaternary ammonium compounds (QACs) often is considered to be a challenging undertaking owing to secondary interactions of the analytes' permanently charged quaternary ammonium head or hydrophobic tail with the utilized labware. Here, for the first time, a micelle assisted thin-film solid phase microextraction (TF-SPME) using a zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) as a matrix modifier is introduced as a novel approach for in-laboratory sample preparation of the challenging compounds. The proposed micelle assisted TF-SPME method offers suppression/enhancement free electrospray ionization of analytes in mass spectrometric detection, minimal interaction of the micelles with the TF-SPME coating, and chromatographic stationary phase and analysis free of secondary interactions. Moreover, it was found that the matrix modifier has multiple functions; when its concentration is found below the critical micelle concentration (CMC), the matrix modifier primarily acts as a surface deactivator; above its CMC, it acts as a stabilizer for QACs. Additionally, shorter equilibrium extraction times in the presence of the modifier demonstrated that micelles also assist in the transfer of analytes from the bulk of the sample to the surface of the coating. The developed micelle assisted TF-SPME protocol using the 96-blade system requires only 30 min of extraction and 15 min of desorption. Together with a conditioning step (15 min), the entire method is 60 min; considering the advantage of using the 96-blade system, if all the blades in the brush are used, the sample preparation time per sample is 0.63 min. Moreover, the recoveries for all analytes with the developed method were found to range within 80.2-97.3%; as such, this method can be considered an open bed solid phase extraction. The proposed method was successfully validated using real samples.

  9. Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Nomura, Cassiana S.; Silva, Cintia S.; Nogueira, Ana R.A.; Oliveira, Pedro V.

    2005-01-01

    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 deg. C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg - 1 and 128 mg kg - 1 , respectively. The relative standard deviations were lower than 6% (n = 5). The

  10. Device for flame combustion of liquid or solid samples in radioactive isotope trace indication

    International Nuclear Information System (INIS)

    Kaartinen, N.H.

    1979-01-01

    The plant or animal tissue containing T and/or 14 C isotope indicator is in a small ignition cage within the combustion chamber. The ignition cage consists of Nichrome which supports the ignition procedure. The combustion chamber is maintained at a temperature above the condensation temperature of the vapours escaping from the tissue (e.g. H 2 O). The thimble type ignition cage burns uniformly together with the sample. It is no longer necessary to make pellets of the sample. (DG) [de

  11. Rock Art

    Science.gov (United States)

    Henn, Cynthia A.

    2004-01-01

    There are many interpretations for the symbols that are seen in rock art, but no decoding key has ever been discovered. This article describes one classroom's experiences with a lesson on rock art--making their rock art and developing their own personal symbols. This lesson allowed for creativity, while giving an opportunity for integration…

  12. Determination of diphenylether herbicides in water samples by solid-phase microextraction coupled to liquid chromatography.

    Science.gov (United States)

    Sheu, Hong-Li; Sung, Yu-Hsiang; Melwanki, Mahaveer B; Huang, Shang-Da

    2006-11-01

    Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden.

  13. Sub-microanalysis of solid samples with near-field enhanced atomic emission spectroscopy

    Science.gov (United States)

    Wang, Xiaohua; Liang, Zhisen; Meng, Yifan; Wang, Tongtong; Hang, Wei; Huang, Benli

    2018-03-01

    A novel approach, which we have chosen to name it as near-field enhanced atomic emission spectroscopy (NFE-AES), was proposed by introducing a scanning tunnelling microscope (STM) system into a laser-induced breakdown spectrometry (LIBS). The near-field enhancement of a laser-illuminated tip was utilized to improve the lateral resolution tremendously. Using the hybrid arrangement, pure metal tablets were analyzed to verify the performance of NFE-AES both in atmosphere and in vacuum. Due to localized surface plasmon resonance (LSPR), the incident electromagnetic field is enhanced and confined at the apex of tip, resulting in sub-micron scale ablation and elemental emission signal. We discovered that the signal-to-noise ratio (SNR) and the spectral resolution obtained in vacuum condition are better than those acquired in atmospheric condition. The quantitative capability of NFE-AES was demonstrated by analyzing Al and Pb in Cu matrix, respectively. Submicron-sized ablation craters were achieved by performing NFE-AES on a Si wafer with an Al film, and the spectroscopic information from a crater of 650 nm diameter was successfully obtained. Due to its advantage of high lateral resolution, NFE-AES imaging of micro-patterned Al lines on an integrated circuit of a SIM card was demonstrated with a sub-micron lateral resolution. These results reveal the potential of the NFE-AES technique in sub-microanalysis of solids, opening an opportunity to map chemical composition at sub-micron scale.

  14. Comparison of alkaline fusion and acid digestion methods for the determination of rhenium in rock and soil samples by ICP-MS

    International Nuclear Information System (INIS)

    Uchida, Shigeo; Tagami, Keiko; Tabei, Ken

    2005-01-01

    A simple acid digestion method was studied in order to analyze many samples at once to understand Re behavior in the terrestrial environment, because, under normal laboratory conditions, digestion methods generally used, such as Carius tube digestions, Teflon vessel digestions and alkaline fusions, can handle only a small number of samples at one time to ensure complete sample digestion. In this study, the Re results for reference materials (RMs) obtained by the acid digestion method were compared with those by the alkaline fusion digestion method to get applicability of the acid digestion method for Re determination in soil by inductively coupled plasma mass spectrometry. Alkaline fusion was chosen for the comparison because it is known to have the highest capability to dissolve Re in geological materials among digestion methods. The average total Re recoveries measured using the 185 Re spike for RMs, such as rock, soil and sediment, were 90.6 ± 4.0% for alkaline fusion and 92.2 ± 7.3% for acid digestion, showing no differences between them. However, Re results obtained by the acid digestion method were usually slightly lower than those by the alkaline fusion (Student's t-test, P -1 , the acid digestion method could dissolve about 80% of the sample Re. Although the acid digestion method is unable to dissolve all Re in the sample, however, the Re discharged to soils could be more extractable than the Re in the dissolution-resistant part; thus, the acid digestion method could be useful for obtaining Re levels in soil samples

  15. Solid recovered fuels in the cement industry--semi-automated sample preparation unit as a means for facilitated practical application.

    Science.gov (United States)

    Aldrian, Alexia; Sarc, Renato; Pomberger, Roland; Lorber, Karl E; Sipple, Ernst-Michael

    2016-03-01

    One of the challenges for the cement industry is the quality assurance of alternative fuel (e.g., solid recovered fuel, SRF) in co-incineration plants--especially for inhomogeneous alternative fuels with large particle sizes (d95⩾100 mm), which will gain even more importance in the substitution of conventional fuels due to low production costs. Existing standards for sampling and sample preparation do not cover the challenges resulting from these kinds of materials. A possible approach to ensure quality monitoring is shown in the present contribution. For this, a specially manufactured, automated comminution and sample divider device was installed at a cement plant in Rohožnik. In order to prove its practical suitability with methods according to current standards, the sampling and sample preparation process were validated for alternative fuel with a grain size >30 mm (i.e., d95=approximately 100 mm), so-called 'Hotdisc SRF'. Therefore, series of samples were taken and analysed. A comparison of the analysis results with the yearly average values obtained through a reference investigation route showed good accordance. Further investigations during the validation process also showed that segregation or enrichment of material throughout the comminution plant does not occur. The results also demonstrate that compliance with legal standards regarding the minimum sample amount is not sufficient for inhomogeneous and coarse particle size alternative fuels. Instead, higher sample amounts after the first particle size reduction step are strongly recommended in order to gain a representative laboratory sample. © The Author(s) 2016.

  16. Solid sample atomic absorption spectroscopy in a chemical contaminant monitoring pilot project

    Energy Technology Data Exchange (ETDEWEB)

    Klein, J.; Schmidt, H.; Dirscherl, C.; Muntau, H.

    1987-09-01

    The Institute for Technology and Hygiene of Food of Animal Origin is developing a practible system of monitoring the distribution of toxic substances in the environment, using the dairy cows as bioindicators. A pilot project has been established to solve basic problems as sampling strategy, sample preparation, analysis and data handling. In the preliminary stage of this study the new technique of SS-AAS turned out to be a useful tool. In order to test overall analytical reliability of the data obtained all analytical procedures applied for the different matrices are controlled by the use of reference material of similar matrix compositions. Results of studies on the distribution of admium and lead are reported; the representativity of small sample amounts of cortical tissue (50-60 mg and 1-2 mg dry mass) has additionally been investigated. Direct analysis of wet tissue aliquots (5-10 mg) was not feasible. A possible method of sample preparation of wet tissue is presented which yields reliable results within 10 min of operation time.

  17. Solid phase extraction for determination of 90Sr in water sample

    International Nuclear Information System (INIS)

    Ometakova, J.

    2009-01-01

    We studied the use of an extraction chromatography for determination of 90 Sr in samples of contaminated water. The aim of the thesis was to compare selected products from the point of view of the strontium yields and time needed. Three commercial products: 3M Empore Strontium Rad Disk, AnaLig, Sr-Resin and two classical methods: liquid-liquid extraction with tributylphosphate and carbonate co-precipitation (to eliminate interferers) were used for separation of 90 Sr. The water sample was used in radiochemical analysis for determination volume activity of 90 Sr. A radiochemical strontium yield was traced by using radionuclide 85 Sr. Samples were counted over a two week period to monitor the ingrowth of 90 Y on TRI CARB LSC counter. Samples were measured using an HPGe detector to find out 85 Sr recoveries at 514 keV line and they were counted directly by Cherenkov counting after the growth of 90 Y using TriCarb LSC counter after a two- week period (author)

  18. Determination of polychlorinated biphenyls in milk samples by saponification-solid-phase microextraction.

    Science.gov (United States)

    Llompart, M; Pazos, M; Landin, P; Cela, R

    2001-12-15

    A saponification-HSSPME procedure has been developed for the extraction of PCBs from milk samples. Saponification of the samples improves the PCB extraction efficiency and allows attaining lower background. A mixed-level fractional design has been used to optimize the sample preparation process. Five variables have been considered: extraction time, agitation, kind of microextraction fiber, concentration, and volume of NaOH aqueous solution. Also the kinetic of the process has been studied with the two fibers (100-microm PDMS and 65-microm PDMS-DVB) included in this study. Analyses were performed on a gas chromatograph equipped with an electron capture detector and a gas chromatograph coupled to a mass selective detector working in MS-MS mode. The proposed method is simple and rapid, and yields high sensitivity, with detection limits below 1 ng/mL, good linearity, and reproducibility. The method has been applied to liquid milk samples with different fat content covering the whole commercial range, and it has been validated with powdered milk certified reference material.

  19. Dynamic flow-through approaches for metal fractionation in environmentally relevant solid samples

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Chomchoei, Roongrat

    2005-01-01

    generations of flow-injection analysis. Special attention is also paid to a novel, robust, non-invasive approach for on-site continuous sampling of soil solutions, capitalizing on flow-through microdialysis, which presents itself as an appealing complementary approach to the conventional lysimeter experiments...

  20. An all-glass solid sampling device for open tubular columns in gas chromatography

    NARCIS (Netherlands)

    Cox, T.P.H.; vd Berg, P.M.J.

    1972-01-01

    An all-glass system for direct sample-introduction of high-boiling compounds onto open tubular columns is described. The standard deviation for quantitative measurements is less than 2.7%. The loss in resolving power of capillary columns, due to this injection system is negligible. The system is

  1. Sample preparation composite and replicate strategy case studies for assay of solid oral drug products.

    Science.gov (United States)

    Nickerson, Beverly; Harrington, Brent; Li, Fasheng; Guo, Michele Xuemei

    2017-11-30

    Drug product assay is one of several tests required for new drug products to ensure the quality of the product at release and throughout the life cycle of the product. Drug product assay testing is typically performed by preparing a composite sample of multiple dosage units to obtain an assay value representative of the batch. In some cases replicate composite samples may be prepared and the reportable assay value is the average value of all the replicates. In previously published work by Harrington et al. (2014) [5], a sample preparation composite and replicate strategy for assay was developed to provide a systematic approach which accounts for variability due to the analytical method and dosage form with a standard error of the potency assay criteria based on compendia and regulatory requirements. In this work, this sample preparation composite and replicate strategy for assay is applied to several case studies to demonstrate the utility of this approach and its application at various stages of pharmaceutical drug product development. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Development of solid materials for UF6 sampling: FY16 Annual Report

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Nicholas [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Savina, Joseph [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Hebden, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

    2016-10-31

    A handheld implementation of the ABACC-developed Cristallini method, which captures uranium hexafluoride samples as an inert salt, was organized in FY17 and succeeded in demonstrating the handheld sampler concept with reactive hexafluoride gases. The Cristallini method relies on the use of a hydrated substrate to react the incoming hexafluoride resulting in the formation of a stable uranyl fluoride salt. The Cristallini method has been demonstrated as a facility modification installed near the sampling tap of a gas centrifuge enrichment plant. While very successful in reducing the hazards of uranium hexafluoride sample, the method still takes a considerable amount of time and can only be used in facilities where the apparatus has been installed; this arrangement generally prohibits the sampling of filled cylinders that have already exited the facility and have been deposited in the on-site tank storage yard. The handheld unit under development will allow the use of the Cristallini method at facilities that have not been converted as well as tanks in the storage yard. The handheld system utilizes an active vacuum system, rather than a passive vacuum system in the facility setup, to drive the uranium hexafluoride onto the adsorbing media. The handheld unit will be battery operated for fully autonomous operation and will include onboard pressure sensing and flushing capability. To date, the system concept of operations was demonstrated with tungsten hexafluoride that showed the active vacuum pump with multiple cartridges of adsorbing media was viable. Concurrently, the hardened prototype system was developed and tested; removable sample cartridges were developed (the only non-COTS component to date); and preparations were made for uranium tests and a domestic field test.

  3. Determination of major, minor and trace elements in rock samples by laser ablation inductively coupled plasma mass spectrometry: Progress in the utilization of borate glasses as targets

    International Nuclear Information System (INIS)

    Leite, Tacito Dantas F.; Escalfoni, Rainerio; Fonseca, Teresa Cristina O. da; Miekeley, Norbert

    2011-01-01

    The present work is a continuation of a research study performed at our laboratory aiming at the multielement analysis of rock samples (basalts and shale) by inductively coupled plasma mass spectrometry in combination with laser ablation using borate glasses as analytical targets. Argon, nitrogen-argon mixtures and helium were evaluated as cell gases, the latter confirming its better performance. Different operational parameters of the laser, such as gas flow, energy, focus, scanning speed and sampling frequency were optimized. External calibration was made with standards prepared by fusion of geological reference materials (basalts 688 and BCR-2, obsidian SRM 278, and shale SGR-1) of different mass fractions in the meta-tetra borate matrix. Coefficients of determination (R 2 ) were > 0.99 for 30 elements from o total of 40 determined. Method validation was then performed using additional certified reference materials (BHVO-2, BIR-1, SCo-1) produced as borate targets in a similar way. Accuracies were better than 10% for most of the elements studied and analytical precisions, calculated from the residual standard deviations of calibration curves were, typically, between 6% and 10%. Additionally, the semiquantitative TotalQuant (registered) technique was applied, which gave, within the expected uncertainty for this calibration technique, concordant results when compared to the quantitative external calibration procedure. Both methods were then used for the analysis of marine shale samples, which are of great geological interest in petroleum prospecting.

  4. Analytical results and sample locality map for rock, stream-sediment, and soil samples, Northern and Eastern Coloado Desert BLM Resource Area, Imperial, Riverside, and San Bernardino Counties, California

    Science.gov (United States)

    King, Harley D.; Chaffee, Maurice A.

    2000-01-01

    INTRODUCTION In 1996-1998 the U.S. Geological Survey (USGS) conducted a geochemical study of the Bureau of Land Management's (BLM) 5.5 million-acre Northern and Eastern Colorado Desert Resource Area (usually referred to as the NECD in this report), Imperial, Riverside, and San Bernardino Counties, southeastern California (figure 1). This study was done in support of the BLM's Coordinated Management Plan for the area. This report presents analytical data from this study. To provide comprehensive coverage of the NECD, we compiled and examined all available geochemical data, in digital form, from previous studies in the area, and made sample-site plots to aid in determining where sample-site coverage and analyses were sufficient, which samples should be re-analyzed, and where additional sampling was needed. Previous investigations conducted in parts of the current study area included the National Uranium Resource Evaluation (NURE) program studies of the Needles and Salton Sea 1? x 2? quadrangles; USGS studies of 12 BLM Wilderness Study Areas (WSAs) (Big Maria Mountains, Chemehuevi Mountains, Chuckwalla Mountains, Coxcomb Mountains, Mecca Hills, Orocopia Mountains, Palen-McCoy, Picacho Peak, Riverside Mountains, Sheephole Valley (also known as Sheep Hole/Cadiz), Turtle Mountains, and Whipple Mountains); and USGS studies in the Needles and El Centro 1? x 2? quadrangles done during the early 1990s as part of a project to identify the regional geochemistry of southern California. Areas where we did new sampling of rocks and stream sediments are mainly in the Chocolate Mountain Aerial Gunnery Range and in Joshua Tree National Park, which extends into the west-central part of the NECD, as shown in figure 1 and figure 2. This report contains analytical data for 132 rock samples and 1,245 stream-sediment samples collected by the USGS, and 362 stream-sediment samples and 189 soil samples collected during the NURE program. All samples are from the Northern and Eastern Colorado

  5. Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

    Science.gov (United States)

    Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

    2015-01-01

    A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

  6. The use of EURACHEM guide for comparison of two 210Pb determination methods in solid environmental samples

    International Nuclear Information System (INIS)

    Al-Masri, M. S.; Hassan, M.; Amin, Y.

    2008-07-01

    Two techniques for determination of 210 Pb in solid environmental samples have been validated and compared according to Eurachem Guide on method validation. The first technique depended on determination of 210 Po, which equilibrium with 210 Pb, by platting it onto a rotating silver disc. Then, Alpha counting of 210 Po was done using an alpha spectrometer. On the other hand, according to its decay scheme, 210 Pb was measured directly through gamma spectrometry by measuring the 46.5 keV. Detection limits, reproducibility and recovery coefficient were the main validation parameters. In addition, uncertainties of measurement were estimated and compared for the two techniques. The comparison results have shown that, the activity of 210 Pb in the environmental samples can choose which technique is appropriated. It was found that Eurachem Guide and comparison of quality statistical validation parameters can be a good tool for selection of the appropriate method for the application. (Authors)

  7. Determination of alpha activity produced by Indian tea samples using solid state nuclear track detection technique

    International Nuclear Information System (INIS)

    Azam, Ameer; Naqvi, A.H.; Srivastava, D.S.

    2001-01-01

    India has first place in the world in the production, consumption and export of tea. The average production of tea in India is about 780 million kg annually. Indian population uses tea as a favourite beverage specially with the breakfast. Tea leaves are perennial plants and they have extension root system spread over deeper layers in the soil. Soil contains uranium as trace element. Hence, uranium is transferred to the leaves as a result of uptake from the soil over the years. Since many of the decay products of uranium are alpha emitters hence tea is a source of alpha radioactivity and can cause damaging effects. Therefore, data on alpha activity of tea samples will be useful in estimating these harmful effects at least qualitatively. In the present study the alpha activity produced by thirteen samples of tea available in the local market was measured

  8. Use of NIR spectroscopy and multivariate process spectra calibration methodology for pharmaceutical solid samples analysis

    OpenAIRE

    Cárdenas Espitia, Vanessa

    2012-01-01

    Accomplish high quality of final products in pharmaceutical industry is a challenge that requires the control and supervision of all the manufacturing steps. This request created the necessity of developing fast and accurate analytical methods. Near infrared spectroscopy together with chemometrics, fulfill this growing demand. The high speed providing relevant information and the versatility of its application to different types of samples lead these combined techniques as one of the most app...

  9. Hexagonal boron nitride nanosheets as adsorbents for solid-phase extraction of polychlorinated biphenyls from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Jia, Shiliang; Wang, Zhenhua; Ding, Ning [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Elaine Wong, Y.-L. [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Chen, Xiangfeng, E-mail: xiangfchensdas@163.com [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Qiu, Guangyu [Department of Physics and Materials Science, City University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Dominic Chan, T.-W., E-mail: twdchan@cuhk.edu.hk [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong)

    2016-09-14

    The adsorptive potential of hexagonal boron nitride nanosheets (h-BNNSs) for solid-phase extraction (SPE) of pollutants was investigated for the first time. Seven indicators of polychlorinated biphenyls (PCBs) were selected as target analytes. The adsorption of PCBs on the surface of the h-BNNSs in water was simulated by the density functional theory and molecular dynamics. The simulation results indicated that the PCBs are adsorbed on the surface by π–π, hydrophobic, and electrostatic interactions. The PCBs were extracted with an h-BNNS-packed SPE cartridge, and eluted by dichloromethane. Gas chromatography–tandem mass spectrometry working in the multiple reaction monitor mode was used for the sample quantification. The effect of extraction parameters, including the flow rate, pH value, breakthrough volume, and the ionic strength, were investigated. Under the optimal working conditions, the developed method showed low limits of detection (0.24–0.50 ng L{sup −1}; signal-to-noise ratio = 3:1), low limits of quantification (0.79–1.56 ng L{sup −1}; signal-to-noise ratio = 10:1), satisfactory linearity (r > 0.99) within the concentration range of 2–1000 ng L{sup −1}, and good precision (relative standard deviation < 12%). The PCBs concentration in environmental water samples was determined by the developed method. This results demonstrate that h-BNNSs have high analytical potential in the enrichment of pollutants. - Highlights: • The hexagonal boron nitride nanosheets were synthesized. • The nanosheets were used as adsorbent for solid-phase extraction. • The h-BN demonstrates remarkable adsorption of PCBs from water samples. • The method was successfully applied in determination of PCBs in water samples.

  10. Solid phase speciation of arsenic by sequential extraction in standard reference materials and industrially contaminated soil samples

    International Nuclear Information System (INIS)

    Herreweghe, Samuel van; Swennen, Rudy; Vandecasteele, Carlo; Cappuyns, Valerie

    2003-01-01

    Leaching experiments, a mineralogical survey and larger samples are preferred when arsenic is present as discrete mineral phases. - Availability, mobility, (phyto)toxicity and potential risk of contaminants is strongly affected by the manner of appearance of elements, the so-called speciation. Operational fractionation methods like sequential extractions have been applied for a long time to determine the solid phase speciation of heavy metals since direct determination of specific chemical compounds can not always be easily achieved. The three-step sequential extraction scheme recommended by the BCR and two extraction schemes based on the phosphorus-like protocol proposed by Manful (1992, Occurrence and Ecochemical Behaviours of Arsenic in a Goldsmelter Impacted Area in Ghana, PhD dissertation, at the RUG) were applied to four standard reference materials (SRM) and to a batch of samples from industrially contaminated sites, heavily contaminated with arsenic and heavy metals. The SRM 2710 (Montana soil) was found to be the most useful reference material for metal (Mn, Cu, Zn, As, Cd and Pb) fractionation using the BCR sequential extraction procedure. Two sequential extraction schemes were developed and compared for arsenic with the aim to establish a better fractionation and recovery rate than the BCR-scheme for this element in the SRM samples. The major part of arsenic was released from the heavily contaminated samples after NaOH-extraction. Inferior extraction variability and recovery in the heavily contaminated samples compared to SRMs could be mainly contributed to subsample heterogeneity

  11. Isotopic abundance measurements on solid nuclear-type samples by glow discharge mass spectrometry

    International Nuclear Information System (INIS)

    Betti, M.; Rasmussen, G.; Koch, L.

    1996-01-01

    A double-focusing glow discharge mass spectrometer (GDMS) installed in a glovebox for nuclear sample screening has been employed for isotopic measurements. Isotopic compositions of zirconium, silicon, lithium, boron, uranium and plutonium which are elements of nuclear concern have been determined. Interferences arising from the matrix sample and the discharge gas (Ar) for each of these elements are discussed. The GDMS results are compared with those from thermal ionization mass spectrometry (TIMS). For boron and lithium at μg/g-ng/g levels, the two methods gave results in good agreement. In samples containing uranium the isotopic composition obtained by GDMS was in agreement with those from TIMS independently of the enrichment. Attempts for the determination of plutonium isotopic composition were also made. In this case, due to the interferences of uranium at mass 238 and americium at mass 241, the GDMS raw data are complementary with those values obtained from physical non-destructive techniques. (orig.). With 2 figs., 4 tabs

  12. Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

    2011-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

  13. Critical issues in soft rocks

    OpenAIRE

    Milton Assis Kanji

    2014-01-01

    This paper discusses several efforts made to study and investigate soft rocks, as well as their physico-mechanical characteristics recognized up to now, the problems in their sampling and testing, and the possibility of its reproduction through artificially made soft rocks. The problems in utilizing current and widespread classification systems to some types of weak rocks are also discussed, as well as other problems related to them. Some examples of engineering works in soft rock or in soft ...

  14. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

    1995-12-01

    Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

  15. Simultaneous determination of platinum group elements and rhenium in rock samples using isotope dilution inductively coupled plasma mass spectrometry after cation exchange separation followed by solvent extraction

    International Nuclear Information System (INIS)

    Shinotsuka, Kazunori; Suzuki, Katsuhiko

    2007-01-01

    A simple and precise determination method for platinum group elements (PGEs) and Re in rock samples was developed using isotope dilution coupled with inductively coupled plasma mass spectrometry (ID-ICP-MS). Cation exchange separation was employed for simplicity, because it is applicable to group separation and simultaneous isotopic measurement in contrast with the widely used anion exchange separation which entails separate elution. However, its application to ID-ICP-MS has been limited due to spectral interferences from impurities retained in the PGE fraction even after ion chromatography. To overcome this limitation, solvent extraction using N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform was successfully applied for further purification. After the examination of optimum experimental parameters in cation exchange separation and solvent extraction using synthetic PGE solution, the established procedure was applied to the determination of PGEs and Re in some geochemical reference materials. The obtained results agreed well with the literature data determined using the different digestion methods (NiS fire assay and the use of a high-pressure asher) within the analytical uncertainties of each other. Significant difference in reproducibility between Ru, Ir, Pt and Os group, and Pd and Re group was observed in the results for BHVO-2 and JA-2. By considering the error factors affecting analytical reproducibility, we concluded that the difference is ascribed to the sample heterogeneity of minor minerals enriched in Ru, Ir, Pt and Os

  16. Determination of polycyclic aromatic hydrocarbons in drinking water samples by solid-phase nanoextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Huiyong; Campiglia, Andres D

    2008-11-01

    A novel alternative is presented for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAH) from water samples. The new approachwhich we have named solid-phase nanoextraction (SPNE)takes advantage of the strong affinity that exists between PAH and gold nanoparticles. Carefully optimization of experimental parameters has led to a high-performance liquid chromatography method with excellent analytical figures of merit. Its most striking feature correlates to the small volume of water sample (500 microL) for complete PAH analyses. The limits of detection ranged from 0.9 (anthracene) to 58 ng.L (-1) (fluorene). The relative standard deviations at medium calibration concentrations vary from 3.2 (acenaphthene) to 9.1% (naphthalene). The analytical recoveries from tap water samples of the six regulated PAH varied from 83.3 +/- 2.4 (benzo[ k]fluoranthene) to 95.7 +/- 4.1% (benzo[ g,h,i]perylene). The entire extraction procedure consumes less than 100 microL of organic solvents per sample, which makes it environmentally friendly. The small volume of extracting solution makes SPNE a relatively inexpensive extraction approach.

  17. Magnetic solid-phase extraction of tetracyclines using ferrous oxide coated magnetic silica microspheres from water samples.

    Science.gov (United States)

    Lian, Lili; Lv, Jinyi; Wang, Xiyue; Lou, Dawei

    2018-01-26

    A novel magnetic solid-phase extraction approach was proposed for extraction of potential residues of tetracyclines (TCs) in tap and river water samples, based on Fe 3 O 4 @SiO 2 @FeO magnetic nanocomposite. Characterized results showed that the received Fe 3 O 4 @SiO 2 @FeO had distinguished magnetism and core-shell structure. Modified FeO nanoparticles with an ∼5 nm size distribution were homogeneously dispersed on the surface of the silica shell. Owing to the strong surface affinity of Fe (II) toward TCs, the magnetic nanocomposite could be applied to efficiently extract three TCs antibiotics, namely, oxytetracycline, tetracycline and chlortetracycline from water samples. Several factors, such as sorbent amount, pH condition, adsorption and desorption time, desorption solvent, selectivity and sample volume, influencing the extraction performance of TCs were investigated and optimized. The developed method showed excellent linearity (R > 0.9992) in the range of 0.133-333 μg L -1 , under optimized conditions. The limits of detection were between 0.027 and 0.107 μg L -1 for oxytetracycline, tetracycline and chlortetracycline, respectively. The feasibility of this method was evaluated by analysis of tap and river water samples. The recoveries at the spiked concentration levels ranged from 91.0% to 104.6% with favorable reproducibility (RSD < 4%). Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Solid-phase microextraction for gas chromatographic/mass spectrometric analysis of dimethoate in human biological samples.

    Science.gov (United States)

    Gallardo, E; Barroso, M; Margalho, C; Cruz, A; Vieira, D N; López-Rivadulla, M

    2006-01-01

    A new, simple and rapid procedure for the determination of dimethoate in urine and blood samples was developed using direct immersion solid-phase microextraction and gas chromatography/mass spectrometry. This technique required only 0.1 mL of sample, and ethion was used as internal standard. Two types of coated fibre were compared (100 microm polydimethylsiloxane, and 65 microm Carbowax/divinylbenzene). Other parameters, such as extraction temperature, adsorption and desorption time, salt addition, agitation and pH, were optimized to enhance the sensitivity of the method. Limits of detection (LODs) and quantitation (LOQs) were 50 and 100 ng/mL for urine and 200 and 500 ng/mL for blood, respectively. The method was found to be linear between the LOQ and 40 microg/mL for urine, and between the LOQ and 50 microg/mL for blood, with correlation coefficients ranging from 0.9923-0.9996. Precision (intra- and interday) and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The mean absolute recoveries of dimethoate were 1.24 and 0.50% for urine and blood, respectively. Because of its simplicity and the fact that small volumes of sample are used, the described method can be successfully used in the diagnosis of poisoning by this pesticide, namely in those situations where the sample volume is limited, as frequently occurs in forensic toxicology. Copyright 2006 John Wiley & Sons, Ltd.

  19. Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

    Science.gov (United States)

    Crevelin, Eduardo J.; Salami, Fernanda H.; Alves, Marcela N. R.; De Martinis, Bruno S.; Crotti, Antônio E. M.; Moraes, Luiz A. B.

    2016-05-01

    Amphetamine-type stimulants (ATS) are among illicit stimulant drugs that are most often used worldwide. A major challenge is to develop a fast and efficient methodology involving minimal sample preparation to analyze ATS in biological fluids. In this study, a urine pool solution containing amphetamine, methamphetamine, ephedrine, sibutramine, and fenfluramine at concentrations ranging from 0.5 pg/mL to 100 ng/mL was prepared and analyzed by atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) and multiple reaction monitoring (MRM). A urine sample and saliva collected from a volunteer contributor (V1) were also analyzed. The limit of detection of the tested compounds ranged between 0.002 and 0.4 ng/mL in urine samples; the signal-to-noise ratio was 5. These results demonstrated that the ASAP-MS/MS methodology is applicable for the fast detection of ATS in urine samples with great sensitivity and specificity, without the need for cleanup, preconcentration, or chromatographic separation. Thus ASAP-MS/MS could potentially be used in clinical and forensic toxicology applications.

  20. Solid-Phase Extraction and Large-Volume Sample Stacking-Capillary Electrophoresis for Determination of Tetracycline Residues in Milk

    Directory of Open Access Journals (Sweden)

    Gabriela Islas

    2018-01-01

    Full Text Available Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. Under optimal conditions, the proposed method had a linear range of 29 to 200 µg·L−1, with limits of detection ranging from 18.6 to 23.8 µg·L−1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation in all cases. The enrichment factors obtained were from 50.33 to 70.85 for all the TCs compared with a conventional capillary zone electrophoresis (CZE. This method is adequate to analyze tetracyclines below the most restrictive established maximum residue limits. The proposed method was employed in the analysis of 15 milk samples from different brands. Two of the tested samples were positive for the presence of oxytetracycline with concentrations of 95 and 126 µg·L−1. SPE-LVSS-CE is a robust, easy, and efficient strategy for online preconcentration of tetracycline residues in complex matrices.

  1. A solid phase extraction-ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples.

    Science.gov (United States)

    Olkowska, Ewa; Polkowska, Żaneta; Namieśnik, Jacek

    2013-11-15

    A new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE-for sample preparation) coupled with ion chromatography-conductivity detection (IC-CD-for the final determination). Mean recoveries of analytes between 79% and 93%, and overall method quantification limits in the range from 0.0018 to 0.038 μg/mL for surface water and CRM samples were achieved. The methodology was applied to the determination of individual alkyl benzyl quaternary ammonium compounds in environmental samples (reservoir water) and enables their presence in such types of waters to be confirmed. In addition, it is a simpler, less time-consuming, labour-intensive, avoiding use of toxic chloroform and significantly less expensive methodology than previously described approaches (liquid-liquid extraction coupled with liquid chromatography-mass spectrometry). Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

    Science.gov (United States)

    Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Goud, D Raghavender; Dubey, D K; Pardasani, Deepak

    2015-05-15

    Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. The physical principles of rock magnetism

    CERN Document Server

    Stacey, Frank

    1974-01-01

    Developments in Solid Earth Geophysics 5: The Physical Principles of Rock Magnetism explores the physical principles of rock magnetism, with emphasis on the properties of finely divided magnetic materials. It discusses the origin and stability of rock magnetizations, the role of remanent magnetism in interpreting magnetic surveys, magnetic anisotropy as an indicator of rock fabric, and the relationship between piezomagnetic changes and seismic activity. Organized into 13 chapters, this volume discusses the properties of solids, magnetite and hematite grains, and rocks with magnetite grains

  4. Testing the homogeneity of candidate reference materials by solid sampling - AAS and INAA

    International Nuclear Information System (INIS)

    Rossbach, M.; Grobecker, K.-H.

    2002-01-01

    The necessity to quantify a natural material's homogeneity with respect to its elemental distribution prior to chemical analysis of a given aliquot is emphasised. Available instruments and methods to obtain the relevant information are described. Additionally the calculation of element specific, relative homogeneity factors, H E , and of a minimum sample mass M 5% to achieve 5% precision on a 95% confidence level is given. Especially, in the production and certification of Certified Reference Materials (CRMs) this characteristic information should be determined in order to provide the user with additional inherent properties of the CRM to enable more economical use of the expensive material and to evaluate further systematic bias of the applied analytical technique. (author)

  5. 'Escher' Rock

    Science.gov (United States)

    2004-01-01

    [figure removed for brevity, see original site] Chemical Changes in 'Endurance' Rocks [figure removed for brevity, see original site] Figure 1 This false-color image taken by NASA's Mars Exploration Rover Opportunity shows a rock dubbed 'Escher' on the southwestern slopes of 'Endurance Crater.' Scientists believe the rock's fractures, which divide the surface into polygons, may have been formed by one of several processes. They may have been caused by the impact that created Endurance Crater, or they might have arisen when water leftover from the rock's formation dried up. A third possibility is that much later, after the rock was formed, and after the crater was created, the rock became wet once again, then dried up and developed cracks. Opportunity has spent the last 14 sols investigating Escher, specifically the target dubbed 'Kirchner,' and other similar rocks with its scientific instruments. This image was taken on sol 208 (Aug. 24, 2004) by the rover's panoramic camera, using the 750-, 530- and 430-nanometer filters. The graph above shows that rocks located deeper into 'Endurance Crater' are chemically altered to a greater degree than rocks located higher up. This chemical alteration is believed to result from exposure to water. Specifically, the graph compares ratios of chemicals between the deep rock dubbed 'Escher,' and the more shallow rock called 'Virginia,' before (red and blue lines) and after (green line) the Mars Exploration Rover Opportunity drilled into the rocks. As the red and blue lines indicate, Escher's levels of chlorine relative to Virginia's went up, and sulfur down, before the rover dug a hole into the rocks. This implies that the surface of Escher has been chemically altered to a greater extent than the surface of Virginia. Scientists are still investigating the role water played in influencing this trend. These data were taken by the rover's alpha particle X-ray spectrometer.

  6. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nischkauer, Winfried [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); Herincs, Esther [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria); University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Puschenreiter, Markus; Wenzel, Walter [University of Natural Resources and Life Sciences, Department of Forest and Soil Sciences, Institute of Soil Research, Konrad Lorenz Straße 24, A-3430 Tulln (Austria); Limbeck, Andreas, E-mail: A.Limbeck@tuwien.ac.at [Vienna University of Technology, Institute of Chemical Technologies and Analytics, Division of Instrumental Analytical Chemistry, Getreidemarkt 9/164-IAC, A-1060 Vienna (Austria)

    2013-11-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g{sup −1}, 0.14 μg g{sup −1} and 0.13 μg g{sup −1} were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was

  7. Determination of Pt, Pd and Rh in Brassica Napus using solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Nischkauer, Winfried; Herincs, Esther; Puschenreiter, Markus; Wenzel, Walter; Limbeck, Andreas

    2013-01-01

    Conventional approaches for the analysis of platinum group elements (PGEs) in plant material suffer from sample digestion which results in sample dilution and therefore requires high sample intakes to maintain the sensitivity. The presented solid-sampling method avoids sample digestion while improving sensitivity when compared to digestion-based inductively coupled plasma optical emission spectrometry (ICP-OES) methods and allows the analysis of sample masses of 5 mg or less. Detection limits of 0.38 μg g −1 , 0.14 μg g −1 and 0.13 μg g −1 were obtained for Pt, Pd and Rh, respectively using a sample intake of 5 mg. The reproducibility of the procedure ranged between 4.7% (Pd) relative standard deviation (RSD, n = 7) and 7.1% (Rh) RSD for 25 ng analytes. For quantification, aqueous standards were applied on paper filter strips and dried. Only the dried filters were introduced into the electrothermal vaporization unit. This approach successfully removed memory-effects observed during analysis of platinum which occurred only if liquid standards came into contact with the graphite material of the furnace. The presented method for overcoming the Pt-memory-effects may be of further interest for the analysis of other carbide-forming analytes as it does not require any technical modification of the graphite furnace (e.g., metal inlays, pyrolytic coating). Owing to lack of suitable certified reference materials, the proposed method was compared with conventional ICP-OES analysis of digested samples and a good agreement was obtained. As a result of the low sample consumption, it was possible to determine the spatial distribution of PGEs within a single plant. Significant differences in PGE concentrations were observed between the shoots (stem, leaves) and the roots. Pd was mainly found in the roots, whereas Pt and Rh were also found in higher concentrations in the shoots. - Highlights: • The uptake of Pt, Pd and Rh by hydroponically grown plants was investigated

  8. Simultaneous Effects of Total Solids Content, Milk Base, Heat Treatment Temperature and Sample Temperature on the Rheological Properties of Plain Stirred Yogurt

    Directory of Open Access Journals (Sweden)

    Attilio Converti

    2006-01-01

    Full Text Available Response surface methodology was used to establish a relationship between total solids content, milk base, heat treatment temperature, and sample temperature, and consistency index, flow behaviour index, and apparent viscosity of plain stirred yogurts. Statistical treatments resulted in developments of mathematical models. All samples presented shear thinning fluid behaviour. The increase of the content of total solids (9.3–22.7 % and milk base heat treatment temperature (81.6–98.4 °C resulted in a significant increase in consistency index and a decrease in flow behaviour index. Increase in the sample temperature (1.6–18.4 °C caused a decrease in consistency index and increase in flow behaviour index. Apparent viscosity was directly related to the content of total solids. Rheological properties of yogurt were highly dependent on the content of total solids in milk.

  9. Rational calculation of migrated component amount for metasomatically altered rocks--taking albitized trachyte at uranium deposit No.470 as an sample

    International Nuclear Information System (INIS)

    Liu Dezheng

    2006-01-01

    On the basis of overall confirming the reasonableness of available method for calculating migrated component amount, the author has further improved the true constant component fixed calculation method proposed by the author in 2000, i.e, the calculation of actual true migrated mass and atomic number of metasomatically atered rocks, by using two method of measuring rock density. (authors)

  10. Halloysite Nanotubes as a New Adsorbent for Solid Phase Extraction and Spectrophotometric Determination of Iron in Water and Food Samples

    Science.gov (United States)

    Samadi, A.; Amjadi, M.

    2016-07-01

    Halloysite nanotubes (HNTs) have been introduced as a new solid phase extraction adsorbent for preconcentration of iron(II) as a complex with 2,2-bipyridine. The cationic complex is effectively adsorbed on the sorbent in the pH range of 3.5-6.0 and efficiently desorbed by trichloroacetic acid. The eluted complex has a strong absorption around 520 nm, which was used for determination of Fe(II). After optimizing extraction conditions, the linear range of the calibration graph was 5.0-500 μg/L with a detection limit of 1.3 μg/L. The proposed method was successfully applied for the determination of trace iron in various water and food samples, and the accuracy was assessed through the recovery experiments and analysis of a certified reference material (NIST 1643e).

  11. Developing a New Sampling And Analysis Method For Hydrazine And Monomethyl Hydrazine: Using a Derivatizing Agent With Solid Phase Microextraction

    Science.gov (United States)

    Allen, John

    2001-01-01

    Solid phase microextraction (SPME) will be used to develop a method for detecting monomethyl hydrazine (MMH) and hydrazine (Hz). A derivatizing agent, pentafluorobenzoyl chloride (PFBCI), is known to react readily with MMH and Hz. The SPME fiber can either be coated with PFBCl and introduced into a gaseous stream containing MMH, or PFBCl and MMH can react first in a syringe barrel and after a short equilibration period a SPME is used to sample the resulting solution. These methods were optimized and compared. Because Hz and MMH can degrade the SPME, letting the reaction occur first gave better results. Only MMH could be detected using either of these methods. Future research will concentrate on constructing calibration curves and determining the detection limit.

  12. A Headspace Solid Phase Microextraction (HS-SPME method for the chromatographic determination of alkylpyrazines in cocoa samples

    Directory of Open Access Journals (Sweden)

    Pini Gláucia F.

    2004-01-01

    Full Text Available A Headspace Solid Phase Microextraction (HS-SPME procedure for isolation and determination of alkylpyrazines in cocoa liquor, using Gas Chromatography with Flame Ionization Detection (GC-FID for the separation and detection of the analytes, is presented here. The HS-SPME operational conditions were optimized using extractions of samples spiked with known amounts of alkylpyrazines typically found on cocoa products. The maximum extraction efficiency was obtained using SPME fibers coated with 65 µm Carbowax/divinylbenzene. Additionally, the best results were achieved with extraction temperature of 60 ºC, 15 min of sample/headspace equilibration time and 45 min extraction time. It was also observed that suspending the samples in saturated aqueous NaCl solution during extractions resulted in a significant increment on the peak areas. This procedure was found to be effective to determine the so-called pyrazinic ratios (quotient between peak areas of alkylpyrazines, which are useful as quality parameters for cocoa liquor.

  13. A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants.

    Science.gov (United States)

    Heub, Sarah; Tscharner, Noe; Kehl, Florian; Dittrich, Petra S; Follonier, Stéphane; Barbe, Laurent

    2016-01-01

    A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17β-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 µl of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

  14. Determination of trace amounts of plutonium in environmental samples by RIMS using a high repetition rate solid state laser system

    International Nuclear Information System (INIS)

    Gruening, C.; Kratz, J.V.; Trautmann, N.; Waldek, A.; Huber, G.; Passler, G.; Wendt, K.

    2001-01-01

    A reliable and easy to handle high repetition rate solid state laser system has been set up for routine applications of Resonance Ionization Mass Spectrometry (RIMS). It consists of three Titanium-Sapphire (Ti:Sa) lasers pumped by one Nd:YAG laser, providing up to 3 W of tunable laser light each in a wavelength range from 725 nm to 895 nm. The isotope shifts for 238 Pu to 244 Pu have been measured in an efficient ionization scheme with λ 1 =420.76 nm, λ 2 =847.28 nm and λ 3 =767.53 nm. An overall detection efficiency of the RIMS apparatus of ε=1x10 -5 is routinely reached, resulting in a detection limit of 2x10 6 atoms (0.8 fg) of plutonium. The isotopic compositions of synthetic samples and the NIST standard reference material SRM996 were measured. The content of 238 Pu to 242 Pu has been determined in dust samples from the surroundings of a nuclear power plant and 244 Pu was determined in urine samples for the National Radiation Protection Board (NRPB), U.K. Routine operation of plutonium ultratrace detection could thus be established

  15. Optimization and application of octadecyl-modified monolithic silica for solid-phase extraction of drugs in whole blood samples.

    Science.gov (United States)

    Namera, Akira; Saito, Takeshi; Ota, Shigenori; Miyazaki, Shota; Oikawa, Hiroshi; Murata, Kazuhiro; Nagao, Masataka

    2017-09-29

    Monolithic silica in MonoSpin for solid-phase extraction of drugs from whole blood samples was developed to facilitate high-throughput analysis. Monolithic silica of various pore sizes and octadecyl contents were synthesized, and their effects on recovery rates were evaluated. The silica monolith M18-200 (20μm through-pore size, 10.4nm mesopore size, and 17.3% carbon content) achieved the best recovery of the target analytes in whole blood samples. The extraction proceeded with centrifugal force at 1000rpm for 2min, and the eluate was directly injected into the liquid chromatography-mass spectrometry system without any tedious steps such as evaporation of extraction solvents. Under the optimized condition, low detection limits of 0.5-2.0ngmL -1 and calibration ranges up to 1000ngmL -1 were obtained. The recoveries of the target drugs in the whole blood were 76-108% with relative standard deviation of less than 14.3%. These results indicate that the developed method based on monolithic silica is convenient, highly efficient, and applicable for detecting drugs in whole blood samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Evidence on unusual way of cocaine smuggling: cocaine-polymethyl methacrylate (PMMA) solid solution--study of clandestine laboratory samples.

    Science.gov (United States)

    Gostic, T; Klemenc, S

    2007-07-04

    An abandoned clandestine laboratory was seized in Slovenia. All confiscated exhibits were analysed in a forensic laboratory, where the following analytical methods were applied: capillary gas chromatography coupled with mass spectrometry (GC-MS) combined also by solid-phase micro extraction (SPME) and pyrolysis (Py) technique, Fourier transform infrared spectrometry (FTIR) and scanning electron microscopy with energy dispersive X-ray detector (SEM-EDX). The most interesting analytical findings can be summarised as follows: at the crime scene some plastic pieces, which contained cocaine dissolved (as solid solution) in polymethyl methacrylate-plexiglass (PMMA), were found. The highest cocaine concentration measured in the plastic sample was about 15% by weight. Two larger lumps of material (12 and 3 kg) were composed mainly of PMMA and CaCO3 and contained only 0.4 and 0.5% of cocaine, respectively. As for the low cocaine concentration, we assume that those two lumps of material represent discarded waste product--residue after the isolation of cocaine from plastic. Higher quantities of pure solvents (41 l) and solvent mixtures (87 l) were seized. We identified three types of pure solvents (acetone, gasoline and benzine) and two different types of solvent mixtures (benzine/acetone and gasoline/acetone). The total seized volume (87 l) of solvent mixtures holds approximately 395 g of solid residue formed mainly of PMMA and cocaine. Obviously solvent mixtures were used for isolation of cocaine from the plastic. Small quantities of relatively pure cocaine base were identified on different objects. There were two cotton sheets, most probably used for filtration. One sheet had traces of cocaine base (76% purity) on the surface, while cocaine in hydrochloride form (96%) was identified on the other sheet. GC-MS analyses of micro traces isolated from analytical balances showed the presence of cocaine and some common adulterants: phenacetine, lidocaine and procaine. A cocaine

  17. Metrological system for y-ray spectrometry measurement of the specific activity and mass fraction of natural radioactive elements in soil and rock samples

    International Nuclear Information System (INIS)

    Khaikovich, I.M.; Fominykh, V.I.; Kirisyuk, E.M.; Belyachkov, Y.A.

    1994-01-01

    In the last few years a great deal of attention has been devoted to the study of the radiation conditions, which in some regions change markedly as a result of intense human activity. One reason for radioactive contamination of an area is dissemination during extraction and processing of radioactive ores or other minerals of natural radioactive elements with a high content of potassium, uranium (radium), and thorium. Estimation of the level of radioactive contamination is one of the main problems of ecological monitoring, and the quality of the measurements sometimes plays a deciding role in the fate of the object being investigated. This also pertains to, in particular, estimation of radioactive contamination of minerals employed for building homes and factories and other industrial structures. In order to draw unequivocal and well-founded conclusions from measurements of the content of natural radioactive elements in soil and rock samples, collected at the object being investigated, a great deal of attention must be devoted during the organization of the measurements to the metrological system

  18. Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

    Science.gov (United States)

    Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

    2016-08-15

    Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Recreating Rocks

    DEFF Research Database (Denmark)

    Posth, Nicole R

    2008-01-01

    Nicole Posth and colleagues spent a month touring South African rock formations in their quest to understand the origin of ancient iron and silicate layers.......Nicole Posth and colleagues spent a month touring South African rock formations in their quest to understand the origin of ancient iron and silicate layers....

  20. Low-impact sampling under an active solid low-level radioactive waste disposal unit using horizontal drilling technology

    International Nuclear Information System (INIS)

    Puglisi, C.V.; Vold, E.L.

    1995-01-01

    The purpose of this project was to determine the performance of the solid low-level radioactive waste (LLRW) disposal units located on a mesa top at TA-54, Area G, Los Alamos National Laboratory (LANL), Los Alamos, NM, and to provide in-situ (vadose zone) site characterization information to Area G's Performance Assessment. The vadose zone beneath an active disposal unit (DU 37), was accessed by utilizing low-impact, air-rotary horizontal drilling technology. Core samples were pulled, via wire-line core method, in 3 horizontal holes fanning out below DU 37 at approximately 5 foot intervals depending on recovery percentage. Samples were surveyed and prepared in-field following Environmental Restoration (ER) guidelines. Samples were transferred from the field to the CST-9 Radvan for initial radiological screening. Following screening, samples were delivered to CST-3 analytical lab for analyses including moisture content, 23 inorganics, 60 volatile organic compounds (VOC's), 68 semivolatile organic compounds (SVOC's), tritium, lead 210, radium 226 ampersand 228, cesium 137, isotopic plutonium, americium 241, strontium 90, isotopic uranium, and isotopic thorium. Other analyses included matric potential, alpha spectroscopy, gamma spectroscopy, and gross alpha/beta. The overall results of the analysis identified only tritium as having migrated from the DU. Am-241, Eu-152, and Pu-238 were possibly identified above background but the results are not definitive. Of all organics analysed for, only ethyl acetate was tentatively identified slightly above background. All inorganics were found to be well below regulatory limits. Based on the results of the above mentioned analyses, it was determined that Area G's disposal units are performing well and no significant liquid phase migration of contaminants has occurred

  1. Influence of sampling frequency and load calculation methods on quantification of annual river nutrient and suspended solids loads.

    Science.gov (United States)

    Elwan, Ahmed; Singh, Ranvir; Patterson, Maree; Roygard, Jon; Horne, Dave; Clothier, Brent; Jones, Geoffrey

    2018-01-11

    Better management of water quality in streams, rivers and lakes requires precise and accurate estimates of different contaminant loads. We assessed four sampling frequencies (2 days, weekly, fortnightly and monthly) and five load calculation methods (global mean (GM), rating curve (RC), ratio estimator (RE), flow-stratified (FS) and flow-weighted (FW)) to quantify loads of nitrate-nitrogen (NO 3 - -N), soluble inorganic nitrogen (SIN), total nitrogen (TN), dissolved reactive phosphorus (DRP), total phosphorus (TP) and total suspended solids (TSS), in the Manawatu River, New Zealand. The estimated annual river loads were compared to the reference 'true' loads, calculated using daily measurements of flow and water quality from May 2010 to April 2011, to quantify bias (i.e. accuracy) and root mean square error 'RMSE' (i.e. accuracy and precision). The GM method resulted into relatively higher RMSE values and a consistent negative bias (i.e. underestimation) in estimates of annual river loads across all sampling frequencies. The RC method resulted in the lowest RMSE for TN, TP and TSS at monthly sampling frequency. Yet, RC highly overestimated the loads for parameters that showed dilution effect such as NO 3 - -N and SIN. The FW and RE methods gave similar results, and there was no essential improvement in using RE over FW. In general, FW and RE performed better than FS in terms of bias, but FS performed slightly better than FW and RE in terms of RMSE for most of the water quality parameters (DRP, TP, TN and TSS) using a monthly sampling frequency. We found no significant decrease in RMSE values for estimates of NO 3 - N, SIN, TN and DRP loads when the sampling frequency was increased from monthly to fortnightly. The bias and RMSE values in estimates of TP and TSS loads (estimated by FW, RE and FS), however, showed a significant decrease in the case of weekly or 2-day sampling. This suggests potential for a higher sampling frequency during flow peaks for more precise

  2. The indicating FTA elute cartridge a solid sample carrier to detect high-risk HPV and high-grade cervical lesions

    NARCIS (Netherlands)

    Bie, R.P. de; Schmeink, C.E.; Bakkers, J.M.J.E.; Snijders, P.J.L.M.; Quint, W.G.V.; Massuger, L.F.A.G.; Bekkers, R.L.M.; Melchers, W.J.G.

    2011-01-01

    The clinically validated high-risk human papillomavirus (hrHPV) Hybrid Capture 2 (HC2) and GP5+/6+-PCR assays were analyzed on an Indicating FTA Elute cartridge (FTA cartridge). The FTA cartridge is a solid dry carrier that allows safe transport of cervical samples. FTA cartridge samples were

  3. Ordered nanoporous carbon as an effective adsorbent in solid-phase microextraction of toluene and chlorinated toluenes in water samples

    Directory of Open Access Journals (Sweden)

    Mansoor Anbia

    2016-09-01

    Full Text Available Ordered nanoporous carbon (CMK-3 has been synthesized and immobilized onto a copper wire, and subsequently applied to headspace solid phase microextraction (HS-SPME of toluene, 4-chlorotoluene, 2,4-dichlorotoluene and 2,6-dichlorotoluene following gas chromatography–flame ionization detection (GC–FID. The structural order and textural properties of the prepared materials have been characterized by N2 sorption analyses, scanning electron microscopy (SEM and X-ray diffraction (XRD. Five experimental parameters such as extraction temperature, extraction time, salt concentration and stirring speed have been evaluated and optimized by means of a Taguchi’s OA16(45 orthogonal array experimental design. The experimental results indicate that extraction temperature and extraction time are the most significant factors in the analysis procedure. The optimum extraction conditions were as follows: 12 mL sample volume; ambient temperature; 10% (w/v NaCl; 35 min extraction time and stirring rate of 600 rpm. Under the optimized conditions for all analyzed compounds, the linearity was from 2.5 to 400 μg L−1, and limit of detections (LODs were between 0.02 and 0.08 μg L−1. The relative standard deviation values were ⩽5.25% and recovery values were between 85.60% and 104.12%. This method has been successfully used for preconcentration and analysis of above mentioned compounds in different real water samples.

  4. Effect of Binding Components in Complex Sample Matrices on Recovery in Direct Immersion Solid-Phase Microextraction: Friends or Foe?

    Science.gov (United States)

    Alam, Md Nazmul; Pawliszyn, Janusz

    2018-02-20

    The development of matrix compatible coatings for solid-phase microextraction (SPME) has enabled direct extraction of analytes from complex sample matrices. The direct immersion (DI) mode of SPME when utilized in conjunction with such extraction phases facilitates extraction of a wide range of analytes from complex matrices without the incurrence of fouling or coating saturation. In this work, mathematical models and computational simulations were employed to investigate the effect of binding components present in complex samples on the recovery of small molecules varying in logP for extractions carried out using the direct immersion approach. The presented findings corroborate that the studied approach indeed enables the extraction of both polar and nonpolar analytes from complex matrices, provided a suitable sorbent is employed. Further results indicated that, in certain cases, the kinetics of extraction of a given analyte in its free form might be dependent on the desorption kinetics of their bound form from matrix components, which might lower total recoveries of analytes with high affinity for the matrix. However, the binding of analytes to matrix components also enables SPME to extract a balanced quantity of different logP analytes, facilitated by multiphase equilibria, with a single extraction device.

  5. Method optimization for non-equilibrium solid phase microextraction sampling of HAPs for GC/MS analysis

    Science.gov (United States)

    Zawadowicz, M. A.; Del Negro, L. A.

    2010-12-01

    Hazardous air pollutants (HAPs) are usually present in the atmosphere at pptv-level, requiring measurements with high sensitivity and minimal contamination. Commonly used evacuated canister methods require an overhead in space, money and time that often is prohibitive to primarily-undergraduate institutions. This study optimized an analytical method based on solid-phase microextraction (SPME) of ambient gaseous matrix, which is a cost-effective technique of selective VOC extraction, accessible to an unskilled undergraduate. Several approaches to SPME extraction and sample analysis were characterized and several extraction parameters optimized. Extraction time, temperature and laminar air flow velocity around the fiber were optimized to give highest signal and efficiency. Direct, dynamic extraction of benzene from a moving air stream produced better precision (±10%) than sampling of stagnant air collected in a polymeric bag (±24%). Using a low-polarity chromatographic column in place of a standard (5%-Phenyl)-methylpolysiloxane phase decreased the benzene detection limit from 2 ppbv to 100 pptv. The developed method is simple and fast, requiring 15-20 minutes per extraction and analysis. It will be field-validated and used as a field laboratory component of various undergraduate Chemistry and Environmental Studies courses.

  6. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Yamamoto

    2014-01-01

    Full Text Available Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS, has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera, Tokushima (Ulva prolifera, and Ehime prefecture (Ulva linza. Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera and Tokushima prefecture (Ulva prolifera. Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum. Multivariant statistical analysis (PCA enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  7. Determination of volatile compounds in four commercial samples of Japanese green algae using solid phase microextraction gas chromatography mass spectrometry.

    Science.gov (United States)

    Yamamoto, Masayoshi; Baldermann, Susanne; Yoshikawa, Keisuke; Fujita, Akira; Mase, Nobuyuki; Watanabe, Naoharu

    2014-01-01

    Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS), has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera), Tokushima (Ulva prolifera), and Ehime prefecture (Ulva linza). Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera) and Tokushima prefecture (Ulva prolifera). Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum). Multivariant statistical analysis (PCA) enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  8. Zincon-modified activated carbon for solid-phase extraction and preconcentration of trace lead and chromium from environmental samples.

    Science.gov (United States)

    Li, Zhenhua; Chang, Xijun; Hu, Zheng; Huang, Xinping; Zou, Xiaojun; Wu, Qiong; Nie, Rong

    2009-07-15

    A new method that utilizes zincon-modified activated carbon (AC-ZCN) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III) and Pb(II) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 4, the maximum adsorption capacity of Cr(III) and Pb(II) onto the AC-ZCN were 17.9 and 26.7 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 1 mL of 0.1 mol L(-1) HCl. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3 sigma) of this method for Cr(III) and Pb(II) were 0.91 and 0.65 ng mL(-1), respectively. The relative standard deviation under optimum condition is less than 3.5% (n=8). The method has been applied for the determination of Cr(III) and Pb(II) in biological materials and water samples with satisfactory results.

  9. Determination of soy proteins in food samples by dispersive solid-phase immunoextraction and dynamic long-wavelength fluorometry

    International Nuclear Information System (INIS)

    Molina-Delgado, María Ángeles; Aguilar-Caballos, María Paz; Gomez-Hens, Agustina

    2013-01-01

    We report on a method for the determination of soy proteins in food samples via dispersive solid-phase immunoextraction using gold-coated magnetic nanoparticles (NPs) as a support. Soy proteins were first extracted using anti-soy protein antibodies immobilized on the NPs, and then quantified by measuring the increase in fluorescence of the long-wavelength fluorophore cresyl violet in the presence of the anionic surfactant sodium dodecyl sulfate at neutral pH in a flow system. The method involves the use of two standard or sample aliquots. The fluorescence intensity of one aliquot is directly measured whereas that of the other aliquot is measured after immunoextraction. The difference between the peak heights of both aliquots serves as the analytical information that is directly proportional to the protein concentration. The limit of detection is 0.35 mg L −1 , the linear range is from 1 to 15 mg L −1 , and the relative standard deviation is < 5 %. Proteins such as bovine serum albumin and globulins do not interfere at the same concentration level. The method was applied to the analysis of soy-based beverages and gave recoveries in the range between 80.0 and 107.3 %. (author)

  10. Application of dried spot cards as a rapid sample treatment method for determining hydroxytyrosol metabolites in human urine samples. Comparison with microelution solid-phase extraction.

    Science.gov (United States)

    Serra, Aida; Rubió, Laura; Macià, Alba; Valls, Rosa-M; Catalán, Úrsula; de la Torre, Rafael; Motilva, Maria-José

    2013-11-01

    Two different rapid sample pretreatment strategies, dried spot cards, and microelution solid-phase extraction plates (μSPE), with ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) have been developed and validated for the determination of hydroxytyrosol and its metabolites in spiked human urine samples. Hydroxytyrosol, hydroxytyrosol-3'-O-glucuronide, hydroxytyrosol-4'-O-glucuronide, hydroxytyrosol-3-O-sulphate, and homovanillic alcohol-4'-O-glucuronide were used as the target compounds. Using the FTA DMPK-A dried urine spot card under optimum conditions, with 5 μL of preconcentrated urine volume and 100 μL of methanol/water (50/50, v/v) as the elution solvent, the extraction recovery (%R) of the compounds studied was higher than 80%, and the matrix effect (%ME) was less than 8%. The stability of these cards and punching at the centre or side of the card were also studied, obtaining an excellent stability after 7 days of storage and complete homogeneity across the surface of the dried drop. The different μSPE parameters that affect the efficiency were also studied, and under optimum conditions, the %R and the %ME were higher than 70% and lower than 17%, respectively. The linearity range in dried urine spot cards was 2.5-20 μM for all the metabolites, with the exception of hydroxytyrosol-3-O-sulphate and hydroxytyrosol, which were 0.3-70 μM and 2.5-50 μM respectively. With regards to μSPE, the linearity range was 0.5-5 μM for all the studied compounds, except for hydroxytyrosol-3-O-sulphate, which was 0.08-5 μM. The quantification limits (LOQs) were 0.3-2.5 μM and 0.08-0.5 μM in dried spot cards and in μSPE, respectively. The two developed methods were then applied and compared for determining hydroxytyrosol and its metabolites in human 24 h-urine samples after a sustained consumption (21 days) of a phenol-enriched virgin olive oil. The metabolites identified were hydroxytyrosol in its glucuronide and sulphate

  11. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    International Nuclear Information System (INIS)

    Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

    2012-01-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 °C and 2400 °C, respectively. Slopes of calibration curves (50–750 pg Cr, R 2 > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3–17.7 μg g −1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g −1 Cr. The limit of detection was 3.3 ng g −1 Cr. - Highlights: ► Direct solid sampling is first time employed for Cr in plant materials. ► Calibration curves with liquids and solids are coincident. ► Microanalysis of plants for Cr is validated by reference materials. ► The proposed HR-CS GF AAS method is environmental friendly.

  12. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    Energy Technology Data Exchange (ETDEWEB)

    Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

  13. A general assignment method for oriented sample (OS) solid-state NMR of proteins based on the correlation of resonances through heteronuclear dipolar couplings in samples aligned parallel and perpendicular to the magnetic field.

    Science.gov (United States)

    Lu, George J; Son, Woo Sung; Opella, Stanley J

    2011-04-01

    A general method for assigning oriented sample (OS) solid-state NMR spectra of proteins is demonstrated. In principle, this method requires only a single sample of a uniformly ¹⁵N-labeled membrane protein in magnetically aligned bilayers, and a previously assigned isotropic chemical shift spectrum obtained either from solution NMR on micelle or isotropic bicelle samples or from magic angle spinning (MAS) solid-state NMR on unoriented proteoliposomes. The sequential isotropic resonance assignments are transferred to the OS solid-state NMR spectra of aligned samples by correlating signals from the same residue observed in protein-containing bilayers aligned with their normals parallel and perpendicular to the magnetic field. The underlying principle is that the resonances from the same residue have heteronuclear dipolar couplings that differ by exactly a factor of two between parallel and perpendicular alignments. The method is demonstrated on the membrane-bound form of Pf1 coat protein in phospholipid bilayers, whose assignments have been previously made using an earlier generation of methods that relied on the preparation of many selectively labeled (by residue type) samples. The new method provides the correct resonance assignments using only a single uniformly ¹⁵N-labeled sample, two solid-state NMR spectra, and a previously assigned isotropic spectrum. Significantly, this approach is equally applicable to residues in alpha helices, beta sheets, loops, and any other elements of tertiary structure. Moreover, the strategy bridges between OS solid-state NMR of aligned samples and solution NMR or MAS solid-state NMR of unoriented samples. In combination with the development of complementary experimental methods, it provides a step towards unifying these apparently different NMR approaches. Copyright © 2011 Elsevier Inc. All rights reserved.

  14. Archive of information about geological samples available for research from the Ohio State University Byrd Polar and Climate Research Center (BPCRC) Polar Rock Repository

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — The Polar Rock Repository (PRR) operated by the Byrd Polar and Climate Research Center (BPCRC) at the Ohio State University is a partner in the Index to Marine and...

  15. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  16. Art Rocks with Rock Art!

    Science.gov (United States)

    Bickett, Marianne

    2011-01-01

    This article discusses rock art which was the very first "art." Rock art, such as the images created on the stone surfaces of the caves of Lascaux and Altimira, is the true origin of the canvas, paintbrush, and painting media. For there, within caverns deep in the earth, the first artists mixed animal fat, urine, and saliva with powdered minerals…

  17. Order-parameter-aided temperature-accelerated sampling for the exploration of crystal polymorphism and solid-liquid phase transitions

    International Nuclear Information System (INIS)

    Yu, Tang-Qing; Vanden-Eijnden, Eric; Chen, Pei-Yang; Chen, Ming; Samanta, Amit; Tuckerman, Mark

    2014-01-01

    The problem of predicting polymorphism in atomic and molecular crystals constitutes a significant challenge both experimentally and theoretically. From the theoretical viewpoint, polymorphism prediction falls into the general class of problems characterized by an underlying rough energy landscape, and consequently, free energy based enhanced sampling approaches can be brought to bear on the problem. In this paper, we build on a scheme previously introduced by two of the authors in which the lengths and angles of the supercell are targeted for enhanced sampling via temperature accelerated adiabatic free energy dynamics [T. Q. Yu and M. E. Tuckerman, Phys. Rev. Lett. 107, 015701 (2011)]. Here, that framework is expanded to include general order parameters that distinguish different crystalline arrangements as target collective variables for enhanced sampling. The resulting free energy surface, being of quite high dimension, is nontrivial to reconstruct, and we discuss one particular strategy for performing the free energy analysis. The method is applied to the study of polymorphism in xenon crystals at high pressure and temperature using the Steinhardt order parameters without and with the supercell included in the set of collective variables. The expected fcc and bcc structures are obtained, and when the supercell parameters are included as collective variables, we also find several new structures, including fcc states with hcp stacking faults. We also apply the new method to the solid-liquid phase transition in copper at 1300 K using the same Steinhardt order parameters. Our method is able to melt and refreeze the system repeatedly, and the free energy profile can be obtained with high efficiency

  18. Creep in rock salt with temperature. Testing methods and results

    International Nuclear Information System (INIS)

    Charpentier, J.P.; Berest, P.

    1985-01-01

    The growing interest shown in the delayed behaviour of rocks at elevated temperature has led the Solid Mechanics Laboratory to develop specific equipment designed for creep tests. The design and dimensioning of these units offer the possibility of investigating a wide range of materials. The article describes the test facilities used (uni-axial and tri-axial creep units) and presents the experimental results obtained on samples of Bresse salt [fr

  19. Uranium favorability of tertiary sedimentary rocks of the western Okanogan highlands and of the upper Columbia River valley, Washington. [Measurement and sampling of surface sections, collection of samples from isolated outcrops, and chemical and mineralogical analyses of samples; no known uranium deposits

    Energy Technology Data Exchange (ETDEWEB)

    Marjaniemi, D.K.; Robins, J.W.

    1975-08-01

    Tertiary sedimentary rocks in the northern portions of the western Okanogan highlands and in the upper Columbia River valley were investigated during a regional study to determine the favorability for potential uranium resources of the Tertiary sedimentary rocks of northeastern Washington. This project involved measurement and sampling of surface sections, collection of samples from isolated outcrops, and chemical and mineralogical analyses of samples. No portion of the project area of this report is rated of high or of medium favorability for potential uranium resources. Low favorability ratings are given to Oroville, Tonasket, and Pine Creek areas of the Okanogan River valley; to the Republic graben; and to the William Lakes, Colville, and Sheep Creek areas of the upper Columbia River valley. All these areas contain some fluvial, poorly sorted feldspathic or arkosic sandstones and conglomerates. These rocks are characterized by very low permeability and a consistently high siliceous matrix suggesting very low initial permeability. There are no known uranium deposits in any of these areas, and low level uranium anomalies are rare.

  20. NMR studies of the molecules dynamics to the solid-liquid interfaces: from graded porous materials to oil rocks; Etudes RMN de la dynamique des molecules aux interfaces solide-liquide: des materiaux poreux calibres aux roches petroliferes

    Energy Technology Data Exchange (ETDEWEB)

    Godefroy, S

    2001-11-01

    Low field NMR relaxation for laboratory or in-situ applications provides critical information for oil recovery such as porosity, saturation, and permeability of rocks. In addition, pore size distribution and wettability can also be obtained in some cases. The technique relies on the measurement of proton longitudinal (T{sub 1}) or transverse (T{sub 2}) nuclear relaxation times. For better predictions, the surface micro-dynamics and the chemical properties of the liquids entrapped in the pore space are important and must be characterized. It is well known that the NMR relaxation is enhanced by the paramagnetic impurities at the pore surface but many other parameters influence the relaxation time distributions. These parameters are used to derive the petrophysical properties of the rocks. We propose here an original method to probe the dynamics of water and oil at the pore surface. In the present study, we used both nuclear relaxation at 2.2 MHz and field cycling Nuclear Magnetic Relaxation Dispersion (NMRD) techniques. We applied these two techniques to different kinds of water or oil saturated macroporous media (grain packings, outcrop and reservoir rocks with SiO{sub 2} or CaCO{sub 3} surfaces). We studied the dependence of NMR relaxation on pore size, magnetic field and temperature. Varying the pore size and the surface density of paramagnetic impurities of water saturated grain packings allowed experimental evidence for the two limiting regimes of the water relaxation in pores (surface- and diffusion-limited regimes). NMRD technique (evolution of 1/T{sub 1} with the magnetic field) allowed us to probe liquid surface dynamics in water or oil fully saturated grain packing, outcrop rocks or reservoir rocks (water- and oil-wet surfaces). We evidenced a two-dimensional molecular surface diffusion and directly estimated important parameters such as correlation times, residence times and molecular self-diffusion on the surface. Finally, we proved that the temperature

  1. Major- and minor-metal composition of three distinct solid material fractions associated with Juan de Fuca hydrothermal fluids (northeast Pacific), and calculation of dilution fluid samples

    Science.gov (United States)

    Hinkley, T.K.; Seeley, J.L.; Tatsumoto, M.

    1988-01-01

    Three distinct types of solid material are associated with each sample of the hydrothermal fluid that was collected from the vents of the Southern Juan de Fuca Ridge. The solid materials appear to be representative of deposits on ocean floors near mid-ocean ridges, and interpretation of the chemistry of the hydrothermal solutions requires understanding of them. Sr isotopic evidence indicates that at least two and probably all three of these solid materials were removed from the solution with which they are associated, by precipitation or adsorption. This occurred after the "pure" hydrothermal fluid was diluted and thoroughly mixed with ambient seawater. The three types of solid materials, are, respectively, a coarse Zn- and Fe-rich material with small amounts of Na and Ca; a finer material also rich in Zn and Fe, but with alkali and alkaline-earth metals; and a scum composed of Ba or Zn, with either considerable Fe or Si, and Sr. Mineral identification is uncertain because of uncertain anion composition. Only in the cases of Ba and Zn were metal masses greater in solid materials than in the associated fluids. For all other metals measured, masses in fluids dwarf those in solids. The fluids themselves contain greater concentrations of all metals measured, except Mg, than seawater. We discuss in detail the relative merits of two methods of determining the mixing proportions of "pure" hydrothermal solution and seawater in the fluids, one based on Sr isotopes, and another previously used method based on Mg concentrations. Comparison of solute concentrations in the several samples shows that degree of dilution of "pure" hydrothermal solutions by seawater, and amounts of original solutes that were removed from it as solid materials, are not related. There is no clear evidence that appreciable amounts of solid materials were not conserved (lost) either during or prior to sample collection. ?? 1988.

  2. Natural radionuclides in the environment. A contribution for the localization and characterization of natural hot particles in solid samples; Natuerliche Radionuklide in der Umwelt. Ein Beitrag zur Lokalisierung und Charakterisierung natuerlicher Heisser Teilchen in festen Proben

    Energy Technology Data Exchange (ETDEWEB)

    Boehnke, A.

    2006-07-01

    In the present thesis appearance, spreading, origin, and mineralogical properties of natural hot particles are studied and the radioecological relevance of these particles judged. For this first relevent quaestions on radioactivity in the environment and on hot particles are theoretically treated. In the following detailedly the method of the autoradiography and solid-state track detectors is considered, which make possible to quote the precise position, the number and distribution of radioactive particles on the cutting area or surface of a sample. Basing on these methodical considerations by laboratory experiments determined track pattern formations of alpha emitters are documentated and interpreted. Starting from the knowledge obtained from this in the further part of the thesis a detection technique is developed, by means of which it is possible, to determine and mark the position of natural hot particles in sold samples. Thereafter follows a description of the electron-microscopical studies for the identification of the localized natural hot particles. Using the developed detection technique, as well as the electron-microscopical methods, a broad spectrum of samples - anthropogeneous depositions (industrial residues, industry products, by-products) and natural depositions (rocks, sediments, minerals) - is studied.

  3. Rocking pneumonia

    OpenAIRE

    Rijkers, Ger T.; Rodriguez Gomez, Maria

    2017-01-01

    Ever since Chuck Berry coined the term “rocking pneumonia” in his 1956 song “Roll over Beethoven”, pneumonia has been mentioned frequently in modern blues and rock songs. We analyzed the lyrics of these songs to examine how various elements of pneumonia have been represented in popular music, specifically the cause of pneumonia, the risk groups, comorbidity (such as the boogie woogie flu), the clinical symptoms, and treatment and outcome. Up to this day, songwriters suggest that pneumonia is ...

  4. Eriochrome Blue Black modified activated carbon as solid phase extractor for removal of Pb(II ions from water samples

    Directory of Open Access Journals (Sweden)

    Hassan M. Albishri

    2017-05-01

    Full Text Available In the current study, a sensitive and simple method for the removal of lead Pb(II, from water samples prior to its determination by inductively coupled plasma optical emission spectrometry (ICP-OES, was investigated. The method utilized activated carbon (AC physically modified with Eriochrome Blue Black (EBB as a solid-phase extractant. Surface properties of the AC-EBB phase were characterized by FT-IR and SEM. The separation parameters for effective adsorption of lead Pb(II, including effects of pH, initial concentration of Pb(II, coexisting ions and shaking time using batch method were studied. The optimum pH value for the separation of Pb(II on the new sorbent was 7.0, and the maximum static adsorption capacity of Pb(II onto the AC-EBB was 127.896 mg/g at this pH and after 1 h contact time. The Pb(II adsorption data were modeled using Langmuir adsorption isotherms. Results demonstrated that the adsorption of Pb(II onto activated carbon followed pseudo second-order kinetic model.

  5. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry.

    Science.gov (United States)

    Amin, Alaa S; El-Sharjawy, Abdel-Azeem M; Kassem, Mohammed A

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L(-1) of Tl(III) with relative standard deviation (RSD) of 1.40% (n=10). The detection and quantification limits are 150 and 495 ng L(-1) using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31×10(7) L mol(-1)cm(-1) and 0.00156 ng cm(-2), respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry

    Science.gov (United States)

    Amin, Alaa S.; El-Sharjawy, Abdel-Azeem M.; Kassem, Mohammed A.

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L-1 of Tl(III) with relative standard deviation (RSD) of 1.40% (n = 10). The detection and quantification limits are 150 and 495 ng L-1 using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31 × 107 L mol-1 cm-1 and 0.00156 ng cm-2, respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples.

  7. Magnetic solid-phase extraction of five pyrethroids from environmental water samples followed by ultrafast liquid chromatography analysis.

    Science.gov (United States)

    Yu, Xi; Sun, Ying; Jiang, Chunzhu; Sun, Xiumin; Gao, Yan; Wang, Yuanpeng; Zhang, Hanqi; Song, Daqian

    2012-08-30

    In this study, the polystyrene-coated magnetic nanoparticles (MNPs/PSt) were successfully prepared and characterized by Fourier transform infrared spectroscopy, transmission electron microscopy and vibrating sample magnetometry. The as-prepared MNPs/PSt were used as the adsorbent in magnetic solid phase extraction of five pyrethroids, including lambda-cyhalothrin, deltamethrin, esfenvalerate, permethrin, bifenthrin, in environmental water samples. The five pyrethroids were determined by ultra fast liquid chromatography-ultraviolet spectrometry. The influencing factors, including amount of MNPs/Pst, extraction time, pH value, type and volume of desorption solvent and desorption time, were examined and optimized. The extraction recoveries obtained with merely 50mg of MNPs/Pst were very satisfactory. The whole extraction process could be completed within 0.5h. The MNPs/PSt can be reused after an easy washing process. Thus, a simple, green, economical, time saving and effective method for pyrethroids analysis in environmental water samples was established. A high enrichment factor of 500 was achieved and the limits of detection for lambda-cyhalothrin, deltamethrin, esfenvalerate, permethrin, bifenthrin were 0.015±0.001 ng mL(-1), 0.012±0.001 ng mL(-1), 0.026±0.001 ng mL(-1), 0.020±0.001 ng mL(-1), 0.013±0.001 ng mL(-1), respectively. Recoveries obtained by analyzing spiked water samples at three concentration levels (0.100±0.001 ng mL(-1), 1.000±0.001 ng mL(-1), 10.000±0.001 ng mL(-1)) were between 78.97±8.38% and 96.05±8.38%. The standard curves for the five pyrethroids showed good linearity with the correlation coefficients in the range of 0.9994-0.9999. The intra-day and inter-day precision were satisfactory with the RSDs in the range of 2.05-5.52% and 2.73-8.38%, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Gas chromatographic determination of 1,1-dimethylhydrazine in water samples by solid-phase microextraction with derivatization

    Directory of Open Access Journals (Sweden)

    Madi Abilev

    2014-10-01

    Full Text Available 1,1-Dimethylhydrazine (1,1-DMH used as a rocket fuel component is highly reactive and unstable compound. It greatly complicates its accurate and express determination in environmental samples. Goal of this work was to develop a method for its express determination in water samples based on solid-phase microextraction with preliminary derivatization. Acetone was selected as reagent for derivatization because during its reaction with 1,1-DMH, volatile and hydrophobic acetone dimethylhydrazone (ADMH was formed. It was established that fiber based on 100-micron polydimethylsiloxane provides the most efficient extraction of ADMH from water at extraction time 2 min. Optimal concentration of acetone was 30 mg/mL. The minimum time for reaction of 1,1-DMH with acetone is 10 minutes. Addition of acids and alkali reduced ADMH response that may be caused by degradation of 1,1-DMH and reduction of derivatization rate. Addition of salt allowed to increase the response of ADMH however made impossible the quantitative determination of 1,1-DMH. Dependence of ADMH response on the concentration of 1,1-DMH at optimized parameters is linear in the concentrations range of 0.1-100 mg/L and can be used for quantitative determination of 1,1-DMH in water. Detection limit of the developed method is 0.02 mg/L. Reproducibility index of the method in the whole range of concentrations did not exceed 7%, accuracy index - 15%. Developed method is simple, inexpensive, accurate, automated and can be recommended for implementation in laboratories conducting environmental monitoring in areas of rocket-carriers fall.

  9. Solid-phase microextraction of phthalate esters in water sample using different activated carbon-polymer monoliths as adsorbents.

    Science.gov (United States)

    Lirio, Stephen; Fu, Chung-Wei; Lin, Jhih-Yun; Hsu, Meng-Ju; Huang, Hsi-Ya

    2016-07-13

    In this study, the application of different activated carbon-polymer (AC-polymer) monoliths as adsorbents for the solid-phase microextraction (SPME) of phthalate esters (PAEs) in water sample were investigated. The activated carbon (AC) was embedded in organic polymers, poly(butyl methacrylate-co-ethylene dimethacrylate) (poly(BMA-EDMA)) or poly(styrene-co-divinylbenzene) (poly(STY-DVB)), via a 5-min microwave-assisted or a 15-min water bath heating polymerization. Preliminary investigation on the performance of the native poly(BMA-EDMA) and poly(STY-DVB) demonstrated remarkable adsorption efficiencies for PAEs. However, due to the strong hydrophobic, π-π, and hydrogen bonding interactions between the analytes and polymers, low extraction recoveries were achieved. In contrast, the presence of AC in native polymers not only enhanced the adsorption efficiencies but also assisted the PAE desorption, especially for AC-poly(STY-DVB) with extraction recovery ranged of 76.2-99.3%. Under the optimized conditions, the extraction recoveries for intra-, inter-day and column-to-column were in the range of 76.5-100.8% (<3.7% RSDs), 77.2-97.6% (<5.6% RSDs) and 75.5-99.7% (<6.2% RSDs), respectively. The developed AC-poly(STY-DVB) monolithic column showed good mechanical stability, which can be reused for more than 30 extraction times without any significant loss in the extraction recoveries of PAEs. The AC-poly(STY-DVB) monolithic column was successfully applied in SPME of PAEs in water sample with extraction recovery ranged of 78.8%-104.6% (<5.5% RSDs). Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Adsorptive behavior and solid-phase microextraction of bare stainless steel sample loop in high performance liquid chromatography.

    Science.gov (United States)

    Zhang, Wenpeng; Zhang, Zixin; Meng, Jiawei; Zhou, Wei; Chen, Zilin

    2014-10-24

    In this work, we interestingly happened to observe the adsorption of stainless steel sample loop of HPLC. The adsorptive behaviors of the stainless steel loop toward different kinds of compounds were studied, including polycyclic aromatic hydrocarbons (PAHs), halogeno benzenes, aniline derivatives, benzoic acid derivatives, phenols, benzoic acid ethyl ester, benzaldehyde, 1-phenyl-ethanone and phenethyl alcohol. The adsorptive mechanism was probably related to hydrophobic interaction, electron-rich element-metal interaction and hydrogen bond. Universal adsorption of stainless steels was also testified. Inspired by its strong adsorptive capability, bare stainless steel loop was developed as a modification-free in-tube device for solid-phase microextraction (SPME), which served as both the substrate and sorbent and possessed ultra-high strength and stability. Great extraction efficiency toward PAHs was obtained by stainless steel loop without any modification, with enrichment factors of 651-834. By connecting the stainless steel loop onto a six-port valve, an online SPME-HPLC system was set up and an SPME-HPLC method has been validated for determination of PAHs. The method has exceptionally low limits of detection of 0.2-2pg/mL, which is significantly lower than that of reported methods with different kinds of sorbents. Wide linear range (0.5-500 and 2-1000pg/mL), good linearity (R(2)≥0.9987) and good reproducibility (RSD≤2.9%) were also obtained. The proposed method has been applied to determine PAHs in environmental samples. Good recoveries were obtained, ranging from 88.5% to 93.8%. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Vortex-homogenized matrix solid-phase dispersion for the extraction of short chain chlorinated paraffins from indoor dust samples.

    Science.gov (United States)

    Chen, Yu-Hsuan; Chang, Chia-Yu; Ding, Wang-Hsien

    2016-11-11

    A simple and effective method for determining short chain chlorinated paraffins (SCCPs) in indoor dust is presented. The method employed a modified vortex-homogenized matrix solid-phase dispersion (VH-MSPD) prior to its detection by gas chromatography - electron-capture negative-ion mass spectrometry (GC-ECNI-MS) operating in the selected-ion-monitoring (SIM) mode. Under the best extraction conditions, 0.1-g of dust sample was dispersed with 0.1-g of silica gel by using vortex (2min) instead of using a mortar and pestle (3min). After that step, the blend was transferred to a glass column containing 3-g acidic silica gel, 2-g basic silica gel, and 2-g of deactivated silica gel, used as clean-up co-sorbents. Then, target analytes were eluted with 5mL of n-hexane/dichloromethane (2:1, v/v) mixture. The extract was evaporated to dryness under a gentle stream of nitrogen. The residue was then re-dissolved in n-hexane (10μL), and subjected to GC-ECNI-MS analysis. The limits of quantitation (LOQs) ranged from 0.06 to 0.25μg/g for each SCCP congener. Precision was less than 7% for both intra- and inter-day analysis. Trueness was above 89%, which was calculated by mean extraction recovery. The VH-MSPD combined with GC-ECNI-MS was successfully applied to quantitatively detect SCCPs from various indoor dust samples, and the concentrations ranged from 1.2 to 31.2μg/g. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Aseptically Sampled Organics in Subsurface Rocks From the Mars Analog Rio Tinto Experiment: An Analog For The Search for Deep Subsurface Life on Mars.}

    Science.gov (United States)

    Bonaccorsi, R.; Stoker, C. R.

    2005-12-01

    The subsurface is the key environment for searching for life on planets lacking surface life. Subsurface ecosystems are of great relevance to astrobiology including the search for past/present life on Mars. The surface of Mars has conditions preventing current life but the subsurface might preserve organics and even host some life [1]. The Mars-Analog-Rio-Tinto-Experiment (MARTE) is performing a simulation of a Mars drilling experiment. This comprises conventional and robotic drilling of cores in a volcanically-hosted-massive-pyrite deposit [2] from the Iberian Pyritic Belt (IBP) and life detection experiments applying anti-contamination protocols (e.g., ATP Luminometry assay). The RT is considered an important analog of the Sinus Meridiani site on Mars and an ideal model analog for a deep subsurface Martian environment. Former results from MARTE suggest the existence of a relatively complex subsurface life including aerobic and anaerobic chemoautotrophs and strict anaerobic methanogens sustained by Fe and S minerals in anoxic conditions. A key requirement for the analysis of a subsurface sample on Mars is a set of simple tests that can help determine if the sample contains organic material of biological origin, and its potential for retaining definitive biosignatures. We report here on the presence of bulk organic matter Corg (0.03-0.05 Wt%), and Ntot (0.01-0.04 Wt%) and amount of measured ATP (Lightning MVP, Biocontrol) in weathered rocks (tuffs, gossan, pyrite stockwork from Borehole #8; >166m). This provides key insight on the type of trophic system sustaining the subsurface biosphere (i.e., heterotrophs vs. autotrophs) at RT. ATP data (Relative-Luminosity-Units, RLU) provide information on possible contamination and distribution of viable biomass with core depth (BH#8, and BH#7, ~3m). Avg. 153 RLU, i.e., surface vs. center of core, suggest that cleaness/sterility can be maintained when using a simple sterile protocol under field conditions. Results from this

  13. Characterization of rock samples localized in some sites of the Mexican Pacific coast; Caracterizacion de muestras de rocas localizadas en algunos sitios de la costa del Pacifico Mexicano

    Energy Technology Data Exchange (ETDEWEB)

    Pena, P.; Torre, J. de la; Falcon, T.; Segovia, N. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, 11801 Mexico D.F. (Mexico); Azorin, J. [Universidad Autonoma Metropolitana-Iztapalapa C.P. 09340 Mexico D.F. (Mexico)

    1999-07-01

    Geophysical studies in zones of high seismicity have showed differences in the content of radioactive material that is used in the study of the geochemical behavior of the subsoil. In an emanometric mapping of radon in soil realized in the Mexican Pacific coast were finding distinct levels in zones with different lithology. With the finality to know the mineralization types in two zones of study which are localized in the Guerrero coast and they belonging to terrains named Guerrero and Xolapa it was determined the mineralogic characteristics in two types of rocks. The identification of the rocks was realized by X-ray diffraction and was determined the elemental chemical composition using a scanning electron microscope. It was indicated in the results obtained that in the two types of rocks were found minerals such as: quartz, albite, microcline anortite, ferroactinolite and biotite. However, it was found differences between them by the presence of their mineralogic compounds because in the rock belonging to Xolapa terrain were presented whereas in the rock localized in the Guerrero terrain were presented sodic and potassic feldspars. The analysis by the Elemental Chemical Composition technique (Energy Dispersive Spectroscopy) corroborated the results obtained by the X-ray diffraction technique. (Author)

  14. Geochemical characterization of fluoride in water, table salt, active sediment, rock and soil samples, and its possible relationship with the prevalence of enamel fluorosis in children in four municipalities of the department of Huila (Colombia).

    Science.gov (United States)

    Martignon, Stefania; Opazo-Gutiérrez, Mario Omar; Velásquez-Riaño, Möritz; Orjuela-Osorio, Iván Rodrigo; Avila, Viviana; Martinez-Mier, Esperanza Angeles; González-Carrera, María Clara; Ruiz-Carrizosa, Jaime Alberto; Silva-Hermida, Blanca Cecilia

    2017-06-01

    Fluoride is an element that affects teeth and bone formation in animals and humans. Though the use of systemic fluoride is an evidence-based caries preventive measure, excessive ingestion can impair tooth development, mainly the mineralization of tooth enamel, leading to a condition known as enamel fluorosis. In this study, we investigated the geochemical characterization of fluoride in water, table salt, active sediment, rock and soil samples in four endemic enamel fluorosis sentinel municipalities of the department of Huila, Colombia (Pitalito, Altamira, El Agrado and Rivera), and its possible relationship with the prevalence of enamel fluorosis in children. The concentration of fluoride in drinking water, table salt, active sediment, rock, and soil was evaluated by means of an ion selective electrode and the geochemical analyses were performed using X-ray fluorescence. Geochemical analysis revealed fluoride concentrations under 15 mg/kg in active sediment, rock and soil samples, not indicative of a significant delivery to the watersheds studied. The concentration of fluoride in table salt was found to be under the inferior limit (less than 180 μg/g) established by the Colombian regulations. Likewise, exposure doses for fluoride water intake did not exceed the recommended total dose for all ages from 6 months. Although the evidence does not point out at rocks, soils, fluoride-bearing minerals, fluoridated salt and water, the hypothesis of these elements as responsible of the current prevalence of enamel fluorosis cannot be discarded since, aqueducts might have undergone significant changes overtime.

  15. Application of direct solid sample analysis for the determination of chlorine in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos de Gois, Jefferson; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Welz, Bernhard [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil)

    2015-03-01

    This work describes a methodology developed to carry out Cl determination in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis. The solid samples were directly weighed into graphite ‘cups’ and inserted into the graphite furnace. The RF power and the carrier gas flow rate were optimized at 1300 W and 0.7 L min{sup −1}, respectively. Calibration could be carried out using aqueous standard solutions with pre-dried modifiers (Pd + Nd or Pd + Ca) or using solid certified reference materials with the same pre-dried modifiers or without the use of modifiers. The limit of quantification was determined as 5 μg g{sup −1} under optimized conditions and the Cl concentration was determined in five certified reference materials with certified concentrations for Cl, in addition to three certified reference materials, for which certified values for Cl were unavailable; in the latter case, the results were compared with those obtained using high-resolution continuum source molecular absorption spectrometry. Good agreement at a 95% statistical confidence level was achieved between determined and certified or reference values. - Highlights: • Direct determination of chlorine in solid biological materials is described for the first time using ICP-MS. • Calibration against aqueous standards is feasible. • The method is accurate and sensitive, regardless of the composition of the solid sample.

  16. Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap

    Science.gov (United States)

    Zhang, Ying; Mao, Xuefei; Liu, Jixin; Wang, Min; Qian, Yongzhong; Gao, Chengling; Qi, Yuehan

    2016-04-01

    In this work, a solid sampling device consisting of a tungsten coil trap, porous carbon vaporizer and on-line ashing furnace of a Ni-Cr coil was interfaced with inductively coupled plasma mass spectrometry (ICP-MS). A modified double gas circuit system was employed that was composed of carrier and supplemental gas lines controlled by separate gas mass flow controllers. For Cd determination in food samples using the assembled solid sampling ICP-MS, the optimal ashing and vaporization conditions, flow rate of the argon-hydrogen (Ar/H2) (v:v = 24:1) carrier gas and supplemental gas, and minimum sampling mass were investigated. Under the optimized conditions, the limit of quantification was 0.5 pg and the relative standard deviation was within a 10.0% error range (n = 10). Furthermore, the mean spiked recoveries for various food samples were 99.4%-105.9% (n = 6). The Cd concentrations measured by the proposed method were all within the certified values of the reference materials or were not significantly different (P > 0.05) from those of the microwave digestion ICP-MS method, demonstrating the good accuracy and precision of the solid sampling ICP-MS method for Cd determination in food samples.

  17. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization. Final report

    International Nuclear Information System (INIS)

    Loge, G.

    1994-01-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U 3 O 8 . Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF 4 were found to be a kinetic bottleneck to the formation of UF 6 . This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid

  18. Analysis of microcontaminants in aqueous samples by fully automated on-line solid-phase extraction-gas chromatography-mass selective detection.

    NARCIS (Netherlands)

    Louter, A.J.H.; van Beekvelt, C.A.; Cid Montanes, P.; Slobodník, J.; Vreuls, J.J.; Brinkman, U.A.T.

    1996-01-01

    The trace-level analysis of unknown organic pollutants in water requires the use of fast and sensitive methods which also provide structural information. In the present study, an on-line technique was used which combines sample preparation by means of solid-phase extraction (SPE) on a small

  19. Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

    Science.gov (United States)

    Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

    2015-01-01

    A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

  20. Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

    Science.gov (United States)

    A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was appli...

  1. A Lab on a chip device for rapid identification of Avian Influenza virus by on-chip sample preparation and solid phase PCR

    DEFF Research Database (Denmark)

    Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

    2009-01-01

    In this paper, we describe a novel lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid phase PCR on microchip. The device can handle viral samples in an automatic way. Moreover, multiplex PCR and sequence detection are done in one-step, which greatly simplifies...

  2. Expanding the use of polymeric ionic liquids in headspace solid-phase microextraction: Determination of ultraviolet filters in water samples.

    Science.gov (United States)

    Trujillo-Rodríguez, María J; Nan, He; Anderson, Jared L

    2018-03-09

    Three crosslinked polymeric ionic liquid (PIL) sorbent coatings were used in headspace solid-phase microextraction for the determination of a group of ultraviolet filters. The developed crosslinked PIL-based materials include two polycations and a double confined PIL. The method, in combination with gas chromatography-mass spectrometry, is simple, solvent free, and does not require of any derivatization step. After proper optimization of the methodologies with each developed fiber, the analytical performance was compared with a commercial polyacrylate fiber. A study of the normalized calibration slopes, obtained by dividing the calibration slope of each analyte by the coating volume, revealed that the crosslinked fibers can be used as alternatives to commercial fibers for the determination of the selected group of compounds. In particular, the coating nature of the PIL containing the 1-vinylbenzyl-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide IL as monomer and the 1,12-di(3-vinylbenzylimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide IL as crosslinker is the most suitable for the extraction of the selected compounds despite their coating volume, being 3.6 times lower than the commercial polyacrylate fiber. For this fiber, wide linear ranges, correlation coefficients higher than 0.990, limits of detection ranging from 2.8 ng L -1 to 26 ng L -1 and relative standard deviations ranging from 2.5 to 15% were achieved. Finally, all proposed PIL-based fibers were applied towards the analysis of tap water, pool water and lake water, with the majority of the ultraviolet filters being detected and quantified in the last two types of samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Determination of UV filters in high ionic strength sample solutions using matrix-compatible coatings for solid-phase microextraction.

    Science.gov (United States)

    An, Jiwoo; Anderson, Jared L

    2018-05-15

    A double-confined polymeric ionic liquid (PIL) sorbent coating was fabricated for the determination of nine ultraviolet (UV) filters in sample solutions containing high salt content by direct immersion solid-phase microextraction (DI-SPME) coupled to high-performance liquid chromatography (HPLC). The IL monomer and crosslinker cations and anions, namely, 1-vinyl-3-decylimidazolium styrenesulfonate ([VImC 10 ][SS]) and 1,12-di(3-vinylbenzylimidazolium) dodecane distyrenesulfonate ([(VBIm) 2 C 12 ] 2[SS]), were co-polymerized to create a highly stable sorbent coating which allowed for up to 120 direct-immersion extractions in 25% NaCl (w/v) solution without a decrease in its extraction capability. Extraction and desorption parameters such as desorption solvent, agitation rate, extraction time, desorption solvent volume, and desorption time were evaluated and optimized. The analytical performance of the styrenesulfonate anion-based PIL fiber, PIL fiber containing chloride anions, and a commercially available polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber were compared. Coefficients of determination (R 2 ) for the styrenesulfonate anion-based PIL fiber ranged from 0.995 to 0.999 and the limits of detection (LODs) varied from 0.1 to 5 µg L -1 . The developed method was successfully applied in real water samples including tap, pool, and lake water, and acceptable relative recovery values were obtained. The lifetime of the PIL fiber containing chloride anions as well as the PDMS/DVB fiber were considerably shorter than the PIL fiber containing the styrenesulfonate anion, with both fibers showing a notable decrease in reproducibility and significant damage to the sorbent coating surface after 40 and 70 extractions, respectively. The R 2 values for the chloride anion containing PIL fiber were at or higher than 0.991 with LODs ranging from 0.5 to 5 µg L -1 . For the PDMS/DVB fiber, R 2 values ranged from 0.992 to 0.999 and LODs were found to be as low as 0.2

  4. Source rock

    Directory of Open Access Journals (Sweden)

    Abubakr F. Makky

    2014-03-01

    Full Text Available West Beni Suef Concession is located at the western part of Beni Suef Basin which is a relatively under-explored basin and lies about 150 km south of Cairo. The major goal of this study is to evaluate the source rock by using different techniques as Rock-Eval pyrolysis, Vitrinite reflectance (%Ro, and well log data of some Cretaceous sequences including Abu Roash (E, F and G members, Kharita and Betty formations. The BasinMod 1D program is used in this study to construct the burial history and calculate the levels of thermal maturity of the Fayoum-1X well based on calibration of measured %Ro and Tmax against calculated %Ro model. The calculated Total Organic Carbon (TOC content from well log data compared with the measured TOC from the Rock-Eval pyrolysis in Fayoum-1X well is shown to match against the shale source rock but gives high values against the limestone source rock. For that, a new model is derived from well log data to calculate accurately the TOC content against the limestone source rock in the study area. The organic matter existing in Abu Roash (F member is fair to excellent and capable of generating a significant amount of hydrocarbons (oil prone produced from (mixed type I/II kerogen. The generation potential of kerogen in Abu Roash (E and G members and Betty formations is ranging from poor to fair, and generating hydrocarbons of oil and gas prone (mixed type II/III kerogen. Eventually, kerogen (type III of Kharita Formation has poor to very good generation potential and mainly produces gas. Thermal maturation of the measured %Ro, calculated %Ro model, Tmax and Production index (PI indicates that Abu Roash (F member exciting in the onset of oil generation, whereas Abu Roash (E and G members, Kharita and Betty formations entered the peak of oil generation.

  5. Magnetic mineralogy and rock magnetic properties of silicate and carbonatite rocks from Oldoinyo Lengai volcano (Tanzania)

    Science.gov (United States)

    Mattsson, H. B.; Balashova, A.; Almqvist, B. S. G.; Bosshard-Stadlin, S. A.; Weidendorfer, D.

    2018-06-01

    Oldoinyo Lengai, a stratovolcano in northern Tanzania, is most famous for being the only currently active carbonatite volcano on Earth. The bulk of the volcanic edifice is dominated by eruptive products produced by silica-undersaturated, peralkaline, silicate magmas (effusive, explosive and/or as cumulates at depth). The recent (2007-2008) explosive eruption produced the first ever recorded pyroclastic flows at this volcano and the accidental lithics incorporated into the pyroclastic flows represent a broad variety of different rock types, comprising both extrusive and intrusive varieties, in addition to various types of cumulates. This mix of different accidental lithics provides a unique insight into the inner workings of the world's only active carbonatite volcano. Here, we focus on the magnetic mineralogy and the rock magnetic properties of a wide selection of samples spanning the spectrum of Oldoinyo Lengai rock types compositionally, as well from a textural point of view. Here we show that the magnetic properties of most extrusive silicate rocks are dominated by magnetite-ulvöspinel solid solutions, and that pyrrhotite plays a larger role in the magnetic properties of the intrusive silicate rocks. The natrocarbonatitic lavas, for which the volcano is best known for, show distinctly different magnetic properties in comparison with the silicate rocks. This discrepancy may be explained by abundant alabandite crystals/blebs in the groundmass of the natrocarbonatitic lavas. A detailed combination of petrological/mineralogical studies with geophysical investigations is an absolute necessity in order to understand, and to better constrain, the overall architecture and inner workings of the subvolcanic plumbing system. The results presented here may also have implications for the quest in order to explain the genesis of the uniquely natrocarbonatitic magmas characteristic of Oldoinyo Lengai.

  6. Intellektuaalne rock

    Index Scriptorium Estoniae

    2007-01-01

    Briti laulja-helilooja ja näitleja Toyah Willcox ning Bill Rieflin ansamblist R.E.M. ja Pat Mastelotto King Krimsonist esinevad koos ansamblitega The Humans ja Tuner 25. okt. Tallinnas Rock Cafés ja 27. okt Tartu Jaani kirikus

  7. Investigating the resetting of OSL signals in rock surfaces

    DEFF Research Database (Denmark)

    Sohbati, Reza; Murray, Andrew S.; Jain, Mayank

    2011-01-01

    were insensitive. Dose recovery tests using solar simulator and IR diodes on both K-feldspar grains and solid slices taken from the inner parts of the rocks are discussed. Preheat plateau results using surface grains and slices show that significant thermal transfer in naturally bleached samples can...... be avoided by keeping preheat temperatures low. Equivalent doses from surface K-feldspar grains were highly scattered and much larger than expected (0.02 Gy to >100 Gy), while solid surface slices gave more reproducible small doses (mean = 0.17±0.02 Gy, n = 32). Neither crushing nor partial bleaching were...... factors were derived for two samples. These indicate that, for instance, bleaching at a depth of 2 mm into these samples occurs at about ∼28% of the rate at the surface. We conclude that it should be possible to derive meaningful burial doses of >1 Gy from such cobbles; younger samples would probably...

  8. Igneous Rocks

    Science.gov (United States)

    Doe, Bruce R.

    “Igneous Rocks was written for undergraduate geology majors who have had a year of college-level chemistry and a course in mineralogy … and for beginning graduate students. Geologists working in industry, government, or academia should find this text useful as a guide to the technical literature up to 1981 and as an overview of topics with which they have not worked but which may have unanticipated pertinence to their own projects.” So starts the preface to this textbook.As one who works part time in research on igneous rocks, especially as they relate to mineral deposits, I have been looking for such a book with this avowed purpose in a field that has a choking richness of evolving terminology and a bewildering volume of interdisciplinary literature. In addition to the standard topics of igneous petrology, the book contains a chapter on the role of igneous activity in the genesis of mineral deposits, its value to geothermal energy, and the potential of igneous rocks as an environment for nuclear waste disposal. These topics are presented rather apologetically in the preface, but the author is to be applauded for including this chapter. The apology shows just how new these interests are to petrology. Recognition is finally coming that, for example, mineral deposits are not “sports of nature,” a view held even by many economic geologists as recently as the early 1960's; instead they are perfectly ordinary geochemical features formed by perfectly ordinary geologic processes. In fact, the mineral deposits and their attendant alteration zones probably have as much to tell us about igneous rocks as the igneous rocks have to tell us about mineral deposits.

  9. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

  10. Investigation of the Effect of Small Hardening Spots Created on the Sample Surface by Laser Complex with Solid-State Laser

    Science.gov (United States)

    Nozdrina, O.; Zykov, I.; Melnikov, A.; Tsipilev, V.; Turanov, S.

    2018-03-01

    This paper describes the results of an investigation of the effect of small hardening spots (about 1 mm) created on the surface of a sample by laser complex with solid-state laser. The melted area of the steel sample is not exceed 5%. Steel microhardness change in the region subjected to laser treatment is studied. Also there is a graph of the deformation of samples dependence on the tension. As a result, the yield plateau and plastic properties changes were detected. The flow line was tracked in the series of speckle photographs. As a result we can see how mm surface inhomogeneity can influence on the deformation and strength properties of steel.

  11. Box-Behnken design in modeling of solid-phase tea waste extraction for the removal of uranium from water samples

    International Nuclear Information System (INIS)

    Khajeh, Mostafa; Jahanbin, Elham; Ghaffari-Moghaddam, Mansour; Moghaddam, Zahra Safaei; Bohlooli, Mousa

    2015-01-01

    In this study, the solid-phase tea waste procedure was used for separation, preconcentration and determination of uranium from water samples by UV-Vis spectrophotometer. In addition, Box-Behnken experimental design was employed to investigated the influence of six variables including pH, mass of adsorbent, eluent volume, amount of 1-(2-pyridylazo)-2-naphthol (PAN); and sample and eluent flow rates on the extraction of analyte. High determination coefficient (R 2 ) of 0.972 and adjusted-R 2 of 0.943 showed the satisfactory adjustment of the polynomial regression model. This method was used for the extraction of uranium from real water samples.

  12. Characterization of solid heterogeneous waste fuel - the effect of sampling and preparation method; Karaktaerisering av fasta inhomogena avfallsbraenslen - inverkan av metoder foer provtagning och provberedning

    Energy Technology Data Exchange (ETDEWEB)

    Wikstroem-Blomqvist, Evalena; Franke, Jolanta; Johansson, Ingvar

    2007-12-15

    The aim of the project is to evaluate the possibilities to simplify the methods used during sampling and laboratory preparation of heterogeneous waste materials. Existing methods for solid fuel material is summarized and evaluated in the project. As a result of the project two new simplified methods, one for field sampling and one for laboratory preparation work has been suggested. One large challenge regarding waste sampling is to achieve a representative sample due to the considerable heterogeneity of the material. How do you perform a sampling campaign that will give rise to representative results without too large costs? The single largest important source of error is the sampling procedure, equivalent to about 80% of the total error. Meanwhile the sample reduction and laboratory work only represents 15 % and 5 % respectively. Thus, to minimize the total error it is very important that the sampling is well planned in a testing program. In the end a very small analytical sample (1 gram) should reflected a large heterogeneous sample population of 1000 of tons. In this project two sampling campaigns, the fall of 2006 and early winter 2007, were conducted at the waste power plant Renova in Gothenburg, Sweden. The first campaign consisted of three different sample sizes with different number of sub-samples. One reference sample (50 tons and 48 sub-samples), two samples consisting of 16 tons and 8 sub-samples and finally two 4 tons consisting of 2 sub-samples each. During the second sampling campaign, four additional 4 ton samples were taken to repeat and thus evaluate the simplified sampling method. This project concludes that the simplified sampling methods only consisting of two sub-samples and a total sample volume of 4 tons give rise to results with as good quality and precision is the more complicated methods tested. Moreover the results from the two sampling campaigns generated equivalent results. The preparation methods used in the laboratory can as well be

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

    Science.gov (United States)

    Burkhardt, M.R.; Soliven, P.P.; Werner, S.L.; Vaught, D.G.

    1999-01-01

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

  14. 3Wave propagation in rock samples under medium and low temperature conditions. Characteristics of methane hydrate-BSR phenomena; Chu teion ryoiki ni okeru ganseki shiryo no hado denpa tokusei. 1. Methane hydrate BSR gensho no kosatsu suitei

    Energy Technology Data Exchange (ETDEWEB)

    Rokugawa, S; Kato, Y; Matsushima, J; Sano, A [The University of Tokyo, Tokyo (Japan). Faculty of Engineering

    1997-10-22

    In relation to sea-bottom pseudo reflection face and methane hydrate in seismic exploration records, fundamental experimental studies have been made. In order to get a handhold to elucidate phenomena accompanying methane hydrate, the studies have investigated wave propagation behavior of rock samples and sandy sediments under medium and low temperature conditions. The experiments have used a constant-temperature cooling water circulating equipment to control temperatures of each sample. The samples were placed in a cooler box with the vibration transmitter and receiver fixedly installed, and changes of the waves against temperature change were measured. Sand-stones and two kinds of tuffs were used as rock samples for the measurement. Artificial sand sample soaked in water was used as a substitute for a methane hydrate layer. As a result of the experiments, the relation between the hydrate layer and the gas layer was comprehended. In addition, the blanking phenomenon was thought occurring as a result of the nearly whole substance presenting the speed of ice due to freezing of the sediments, rather than by what is described in the ground homogeneousness theory. 5 refs., 9 figs.

  15. Sequential injection system incorporating a micro extraction column for automatic fractionation of metal ions in solid samples

    DEFF Research Database (Denmark)

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    as to the kinetics of the leaching processes and chemical associations in different soil geological phases. Special attention is also paid to the potentials of the microcolumn flowing technique for automatic processing of solid materials with variable homogeneity, as demonstrated with the sewage amended CRM483 soil...

  16. White Rock

    Science.gov (United States)

    2002-01-01

    (Released 19 April 2002) The Science 'White Rock' is the unofficial name for this unusual landform which was first observed during the Mariner 9 mission in the early 1970's. As later analysis of additional data sets would show, White Rock is neither white nor dense rock. Its apparent brightness arises from the fact that the material surrounding it is so dark. Images from the Mars Global Surveyor MOC camera revealed dark sand dunes surrounding White Rock and on the floor of the troughs within it. Some of these dunes are just apparent in the THEMIS image. Although there was speculation that the material composing White Rock could be salts from an ancient dry lakebed, spectral data from the MGS TES instrument did not support this claim. Instead, the White Rock deposit may be the erosional remnant of a previously more continuous occurrence of air fall sediments, either volcanic ash or windblown dust. The THEMIS image offers new evidence for the idea that the original deposit covered a larger area. Approximately 10 kilometers to the southeast of the main deposit are some tiny knobs of similarly bright material preserved on the floor of a small crater. Given that the eolian erosion of the main White Rock deposit has produced isolated knobs at its edges, it is reasonable to suspect that the more distant outliers are the remnants of a once continuous deposit that stretched at least to this location. The fact that so little remains of the larger deposit suggests that the material is very easily eroded and simply blows away. The Story Fingers of hard, white rock seem to jut out like icy daggers across a moody Martian surface, but appearances can be deceiving. These bright, jagged features are neither white, nor icy, nor even hard and rocky! So what are they, and why are they so different from the surrounding terrain? Scientists know that you can't always trust what your eyes see alone. You have to use other kinds of science instruments to measure things that our eyes can

  17. Thermal conductivity of unsaturated clay-rocks

    Directory of Open Access Journals (Sweden)

    D. Jougnot

    2010-01-01

    Full Text Available The parameters used to describe the electrical conductivity of a porous material can be used to describe also its thermal conductivity. A new relationship is developed to connect the thermal conductivity of an unsaturated porous material to the thermal conductivity of the different phases of the composite, and two electrical parameters called the first and second Archie's exponents. A good agreement is obtained between the new model and thermal conductivity measurements performed using packs of glass beads and core samples of the Callovo-Oxfordian clay-rocks at different saturations of the water phase. We showed that the three model parameters optimised to fit the new model against experimental data (namely the thermal conductivity of the solid phase and the two Archie's exponents are consistent with independent estimates. We also observed that the anisotropy of the effective thermal conductivity of the Callovo-Oxfordian clay-rock was mainly due to the anisotropy of the thermal conductivity of the solid phase.

  18. Geologic report of the Maquoketa Shale, New Albany Shale, and Borden Group rocks in the Illinois Basin as potential solid waste repository sites

    International Nuclear Information System (INIS)

    Droste, J.B.; Vitaliano, C.J.

    1976-06-01

    We have evaluated the Illinois Basin in order to select a ''target site'' for a possible solid nuclear waste repository. In the process we have been mindful of geology (particularly stratigraphy and lithology and structure), terrane, population density, land use, land ownership and accessibility. After taking these restrictions into account, we have singled out a strip of land in south central Indiana in which we have selected four potential sites worthy of further exploration. In three of the sites the geology, lithology, and depth below the surface are more than adequate for crypt purposes in two separate formations--the Maquoketa Shale of the Ordovician System and the New Albany Shale-Borden Group of the Upper Devonian-Mississippian Systems. The interval between the two is several hundred feet. The geology and associated features in the fourth site are undoubtedly similar to those in the first three. In all four selections a sizeable proportion of the land is in public ownership and the population density in the nonpublicly owned land is low. The geology, lithology, and position of the target formations have been projected into the sites in question from data provided by drill core records of the Indiana Geological Survey. Precise details would, of course, require exploratory drilling on the selected site

  19. Utilizing a sequential injection system furnished with an extraction microcolumn as a novel approach for executing sequential extractions of metal species in solid samples

    DEFF Research Database (Denmark)

    Chomchoei, R.; Hansen, Elo Harald; Shiowatana, J.

    2007-01-01

    This communication presents a novel approach to perform sequential extraction of elements in solid samples by using a sequential injection (SI) system incorporating a specially designed extraction microcolumn. Based on the operation of the syringe pump, different modes of extraction are potentially...... that the system entails many advantages such as being fully automated, and besides being characterised by rapidity, ease of operation and robustness, it is less prone to risks of contamination and personal errors as encountered in traditional batch systems. Moreover, improvement of the precision and accuracy...... of the chemical fractionation of metal in solids as compared with previous reports are obtained. The system ensures that extraction is performed at designated pH values. Variation of sample weight to column volume ratios do not affect the amounts of extractable metals, nor do extraction flow rates ranging from 50...

  20. STEALTH: a Lagrange explicit finite difference code for solids, structural, and thermohydraulic analysis. Volume 2: sample and verification problems. Computer code manual

    International Nuclear Information System (INIS)

    Hofmann, R.

    1982-08-01

    STEALTH sample and verification problems are presented to help users become familiar with STEALTH capabilities, input, and output. Problems are grouped into articles which are completely self-contained. The pagination in each article is A.n, where A is a unique alphabetic-character article identifier and n is a sequential page number which starts from 1 on the first page of text for each article. Articles concerning new capabilities will be added as they become available. STEALTH sample and verification calculations are divided into the following general categories: transient mechanical calculations dealing with solids; transient mechanical calculations dealing with fluids; transient thermal calculations dealing with solids; transient thermal calculations dealing with fluids; static and quasi-static calculations; and complex boundary interaction calculations

  1. Disc cutter wear and rock texture in hard rock TBM tunneling

    International Nuclear Information System (INIS)

    Koizumi, Yu; Tsusaka, Kimikazu; Tanimoto, Chikaosa; Nakagawa, Shigeo; Fujita, Naoya

    2008-01-01

    Disc cutter wear in TBM tunneling is caused by initial fragmentation of a solid rock face (the primary fragmentation) and fragmentation of residual rock pieces between a cutterhead and the face (the secondary fragmentation). In two projects through sedimentary and granitic rocks, the authors investigated the relationships between the rate of cutter wear caused by the primary fragmentation, point load index and the grain size and contents of abrasive minerals. As a result, it was found that the tensile strength and the mineral contents of rocks significantly influenced the cutter wear in both projects and thus it is necessary to take into account of rock type. (author)

  2. 'Mister Badger' Pushing Mars Rock

    Science.gov (United States)

    1976-01-01

    Viking's soil sampler collector arm successfully pushed a rock on the surface of Mars during the afternoon of Friday, October 8. The irregular-shaped rock was pushed several inches by the Lander's collector arm, which displaced the rock to the left of its original position, leaving it cocked slightly upward. Photographs and other information verified the successful rock push. Photo at left shows the soil sampler's collector head pushing against the rock, named 'Mister Badger' by flight controllers. Photo at right shows the displaced rock and the depression whence it came. Part of the soil displacement was caused by the collector s backhoe. A soil sample will be taken from the site Monday night, October 11. It will then be delivered to Viking s organic chemistry instrument for a series of analyses during the next few weeks. The sample is being sought from beneath a rock because scientists believe that, if there are life forms on Mars, they may seek rocks as shelter from the Sun s intense ultraviolet radiation.

  3. Determination of molybdenum, ruthenium, rhodium, and palladium in radioinactive simulated waste of the nuclear fuel cycle by solid sampling graphite furnace atomic absorption spectrometry (GFAAS)

    International Nuclear Information System (INIS)

    Schmiedel, G.; Mainka, E.; Ache, H.J.

    1989-01-01

    In relation with insoluble particles in the nuclear fuel cycle waste, the solid sampling GFAAS was used to determine molybdenum, ruthenium, rhodium, and palladium in such waste. Two methods for the direct determination of these elements are described. The samples must be handled in glove boxes or moreover in hot cells with a robot. The determination of the elements by the cup-in-tube technique needs a very sensitive balance (microbalance) for weighing in μg-range and the handling of this method is not practical in glove boxes and hot cells. An alternative technique of solid sampling GFAAS, which can be used without great problems in glove boxes and hot cells is the slurry technique. In this case two methods have been used. One method uses graphite powder as a diluter, the other is the direct suspension of the sample in a matrix modifier solution. In the case of slurry technique with predilution of the sample with graphite powder, recoveries between 91 and 102% and RSD between 4 and 8% were obtained, whereas in the case of slurry technique with direct suspension of the waste sample recoveries between 91 and 103% and RSD between 14 and 20% for the above mentioned elements were obtained. (orig.)

  4. Monitoring and Method development of Hg in Istanbul Airborne Particulates by Solid Sampling Continuum Source-High Resolution Electrothermal Atomic Absorption Spectromerty

    Directory of Open Access Journals (Sweden)

    Soydemir E.

    2014-07-01

    Full Text Available In this work, a method has been developed and monitoring for the determination of mercury in PM2.5 airborne particulates by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. The PM2.5 airborne particulates were collected on quartz filters using high volume samplers (500 L/min in Istanbul (Turkey for 96 hours every month in one year. At first, experimental conditions as well as the validation tests were optimized using collected filter. For this purpose, the effects of atomization temperature, amount of sample intoduced in to the furnace, addition of acids and/or KMnO4 on the sample, covering of graphite tube and platform or using of Ag nanoparticulates, Au nanoparticulates, and Pd solutions on the accuracy and precision were investigated. After optimization of the experimental conditions, the mercury concentrations were determined in the collected filter. The filters with PM2.5 airborne particulates were dried, divided into small fine particles and then Hg concentrations were determined directly. In order to eliminate any error due to the sensitivity difference between aqueous standards and solid samples, the quantification was performed using solid calibrants. The limit of detection, based on three times the standard deviations for ten atomizations of an unused filter, was 30 ng/g. The Hg content was dependent on the sampling site, season etc, ranging from samples, addition of AuNPs, AgNPs and Pd solution for amalgamation effects on the recoveries were investigated. The results were compared using statistical tests.

  5. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Science.gov (United States)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  6. Rock stresses (Grimsel rock laboratory)

    International Nuclear Information System (INIS)

    Pahl, A.; Heusermann, S.; Braeuer, V.; Gloeggler, W.

    1989-01-01

    On the research and development project 'Rock Stress Measurements' the BGR has developed and tested several test devices and methods at GTS for use in boreholes at a depth of 200 m and has carried out rock mechanical and engineering geological investigations for the evaluation and interpretation of the stress measurements. The first time a computer for data processing was installed in the borehole together with the BGR-probe. Laboratory tests on hollow cylinders were made to study the stress-deformation behavior. To validate and to interprete the measurement results some test methods were modelled using the finite-element method. The dilatometer-tests yielded high values of Young's modulus, whereas laboratory tests showed lower values with a distinct deformation anisotropy. Stress measurements with the BGR-probe yielded horizontal stresses being higher than the theoretical overburden pressure and vertical stresses which agree well with the theoretical overburden pressure. These results are comparable to the results of the hydraulic fracturing tests, whereas stresses obtained with CSIR-triaxial cells are generally lower. The detailed geological mapping of the borehole indicated relationships between stress and geology. With regard to borehole depth different zones of rock structure joint frequency, joint orientation, and orientation of microfissures as well as stress magnitude, stress direction, and degree of deformation anisotropy could be distinguished. (orig./HP) [de

  7. [Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

    Science.gov (United States)

    Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2014-05-01

    To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

  8. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Orani, Anna Maria; Han, Eunmi; Mandjukov, Petko; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

  9. Rock strength under explosive loading

    International Nuclear Information System (INIS)

    Rimer, N.; Proffer, W.

    1993-01-01

    This presentation emphasizes the importance of a detailed description of the nonlinear deviatoric (strength) response of the surrounding rock in the numerical simulation of underground nuclear explosion phenomenology to the late times needed for test ban monitoring applications. We will show how numerical simulations which match ground motion measurements in volcanic tuffs and in granite use the strength values obtained from laboratory measurements on small core samples of these rocks but also require much lower strength values after the ground motion has interacted with the rock. The underlying physical mechanisms for the implied strength reduction are not yet well understood, and in fact may depend on the particular rock type. However, constitutive models for shock damage and/or effective stress have been used successfully at S-Cubed in both the Geophysics Program (primarily for DARPA) and the Containment Support Program (for DNA) to simulate late time ground motions measured at NTS in many different rock types

  10. An evaluation of a single-step extraction chromatography separation method for Sm-Nd isotope analysis of micro-samples of silicate rocks by high-sensitivity thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Li Chaofeng; Li Xianhua; Li Qiuli; Guo Jinghui; Li Xianghui; Liu Tao

    2011-01-01

    Graphical abstract: Distribution curve of all eluting fractions for a BCR-2 (1-2-3.5-7 mg) on LN column using HCl and HF as eluting reagent. Highlights: → This analytical protocol affords a simple and rapid analysis for Sm and Nd isotope in minor rock samples. → The single-step separation method exhibits satisfactory separation effect for complex silicate samples. → Corrected 143 Nd/ 144 Nd data show excellent accuracy even if the 140 Ce 16 O + / 144 Nd 16 O + ratio reached to 0.03. - Abstract: A single-step separation scheme is presented for Sm-Nd radiogenic isotope system on very small samples (1-3 mg) of silicate rock. This method is based on Eichrom LN Spec chromatographic material and affords a straightforward separation of Sm-Nd from complex matrix with good purity and satisfactory blank levels, suitable for thermal ionization mass spectrometry (TIMS). This technique, characterized by high efficiency (single-step Sm-Nd separation) and high sensitivity (TIMS on NdO + ion beam), is able to process rapidly (3-4 h), with low procedure blanks ( 143 Nd/ 144 Nd ratios and Sm-Nd concentrations are presented for eleven international silicate rock reference materials, spanning a wide range of Sm-Nd contents and bulk compositions. The analytical results show a good agreement with recommended values within ±0.004% for the 143 Nd/ 144 Nd isotopic ratio and ±2% for Sm-Nd quantification at the 95% confidence level. It is noted that the uncertainty of this method is about 3 times larger than typical precision achievable with two-stage full separation followed by state-of-the-art conventional TIMS using Nd + ion beams which require much larger amounts of Nd. Hence, our single-step separation followed by NdO + ion beam technique is preferred to the analysis for microsamples.

  11. Thermal Inertia of Rocks and Rock Populations

    Science.gov (United States)

    Golombek, M. P.; Jakosky, B. M.; Mellon, M. T.

    2001-01-01

    The effective thermal inertia of rock populations on Mars and Earth is derived from a model of effective inertia versus rock diameter. Results allow a parameterization of the effective rock inertia versus rock abundance and bulk and fine component inertia. Additional information is contained in the original extended abstract.

  12. Microbial Leaching of Some Valuable Elements From Egyptian Phosphate Rock

    International Nuclear Information System (INIS)

    Kamal, H.M.; Hassanein, R.A.; Mahdy, H.M.A.; Mahmoud, K.F.; Abouzeid, M.A.

    2012-01-01

    Four phosphate rock samples representing different phosphate mineralization modes in Egypt were selected from Abu Tartar, Nile valley and Red sea areas. Factors affecting the phosphate rock solubilization and some of the contained valuable elements by Aspergillus niger, Penicillium sp. and Pseudomonas fluorescence, were studied with especial orientation towards the completion of phosphate rock samples solubilization especially die low grade one. Effect of nitrogen source type on leaching efficiency by Aspergillus niger when two nitrogen sources on the phosphate bioleaching efficiency, it is clear that the ammonium chloride is more favorable as nitrogen source than sodium nitrate in the bioleaching of phosphate rocks. When Aspergillus niger was applied under die following conditions: 50 g/1 of sucrose as a carbon source, 0.1 N of ammonium chloride as a nitrogen source, 10 days incubation period, 0.5% solid: liquid ratio for P 2 O 5 and 5% for U and REE and - 270 mesh of grain size. The optimum leaching of P 2 O 5 , U and REE from phosphate rock samples reached (23.27%, 17.4%, 11.4%, respectively), while at -60 mesh they reached to 16.58%, 28.9%, 30.2% respectively. The optimum conditions for the maximal leaching efficiencies of P 2 O 5 , U and REE when applying the Penicillium sp. from the phosphate rock samples were: 100 g/1 of sucrose as a carbon source for P 2 O 5 and U and 10 g/1 for REE, 7,15 and 10 days incubation period for P 2 O 5 , U and REE, respectively, 0.5% solid: liquid ratio for P 2 O 5 and 5% for U and REE. Finally, the application of phosphate rock samples grinded to -270 mesh of grain size for P 2 O 5 and (-60 to -140) for U and REE. The studied leaching efficiency of P 2 O 5 , U and REE gave at -270 mesh 33.66%, 24.3%, 15.9% respectively, while at -60 mesh they gave 33.76%, 26.7%, 17.8% and at -140 mesh gave 31.32%, 27.9%, 17.6%, respectively.The optimum conditions for the P 2 O 5 leaching efficiency when applying the Pseudomonas fluorescence were

  13. A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)

  14. Sampling and analytical procedures for the determination of VOCs released into air from natural and anthropogenic sources: A comparison between SPME (Solid Phase Micro Extraction) and ST (Solid Trap) methods

    International Nuclear Information System (INIS)

    Tassi, F.; Capecchiacci, F.; Buccianti, A.; Vaselli, O.

    2012-01-01

    In the present study, two sampling and analytical methods for VOC determination in fumarolic exhalations related to hydrothermal-magmatic reservoirs in volcanic and geothermal areas and biogas released from waste landfills were compared: (a) Solid Traps (STs), consisting of three phase (Carboxen B, Carboxen C and Carbosieve S111) absorbent stainless steel tubes and (b) Solid Phase Micro Extraction (SPME) fibers, composed of DiVinylBenzene (DVB), Carboxen and PolyDimethylSiloxane. These techniques were applied to pre-concentrate VOCs discharged from: (i) low-to-high temperature fumaroles collected at Vulcano Island, Phlegrean Fields (Italy), and Nisyros Island (Greece), (ii) recovery wells in a solid waste disposal site located near Florence (Italy). A glass condensing system cooled with water was used to collect the dry fraction of the fumarolic gases, in order to allow more efficient VOC absorption avoiding any interference by water vapor and acidic gases, such as SO 2 , H 2 S, HF and HCl, typically present at relatively high concentrations in these fluids. Up to 37 organic species, in the range of 40–400 m/z, were determined by coupling gas chromatography to mass spectrometry (GC–MS). This study shows that the VOC compositions of fumaroles and biogas determined via SPME and ST are largely consistent and can be applied to the analysis of VOCs in gases released from different natural and anthropogenic environments. The SPME method is rapid and simple and more appropriate for volcanic and geothermal emissions, where VOCs are present at relatively high concentrations and prolonged gas sampling may be hazardous for the operator. The ST method, allowing the collection of large quantities of sample, is to be preferred to analyze the VOC composition of fluids from diffuse emissions and air, where these compounds are present at relatively low concentrations.

  15. Accelerated solvent extraction (ASE) - a fast and automated technique with low solvent consumption for the extraction of solid samples (T12)

    International Nuclear Information System (INIS)

    Hoefler, F.

    2002-01-01

    Full text: Accelerated solvent extraction (ASE) is a modern extraction technique that significantly streamlines sample preparation. A common organic solvent as well as water is used as extraction solvent at elevated temperature and pressure to increase extraction speed and efficiency. The entire extraction process is fully automated and performed within 15 minutes with a solvent consumption of 18 ml for a 10 g sample. For many matrices and for a variety of solutes, ASE has proven to be equivalent or superior to sonication, Soxhlet, and reflux extraction techniques while requiring less time, solvent and labor. First ASE has been applied for the extraction of environmental hazards from solid matrices. Within a very short time ASE was approved by the U.S. EPA for the extraction of BNAs, PAHs, PCBs, pesticides, herbicides, TPH, and dioxins from solid samples in method 3545. Especially for the extraction of dioxins the extraction time with ASE is reduced to 20 minutes in comparison to 18 h using Soxhlet. In food analysis ASE is used for the extraction of pesticide and mycotoxin residues from fruits and vegetables, the fat determination and extraction of vitamins. Time consuming and solvent intensive methods for the extraction of additives from polymers as well as for the extraction of marker compounds from herbal supplements can be performed with higher efficiencies using ASE. For the analysis of chemical weapons the extraction process and sample clean-up including derivatization can be automated and combined with GC-MS using an online ASE-APEC-GC system. (author)

  16. Radioactivities (dose rates) of rocks in Japan

    International Nuclear Information System (INIS)

    Matsuda, Hideharu; Minato, Susumu

    1995-01-01

    The radioactive distribution (radiation doses) of major rocks in Japan was monitored to clarify the factors influencing terrestrial gamma-ray absorbed dose rates. The rock samples were reduced to powder and analyzed by well-type NaI(Tl) scintillation detector and pulse height analyzer. Terrestrial gamma-ray dose rates were estimated in terms of gamma radiation dose rate 1 m above the ground. The radioactivity concentration was highest in acidic rock which contains much SiO 2 among igneous rock, followed by neutral rock, basic rock, and ultrabasic rock. The radioactive concentration was 30-40% lower in acidic and clastic rocks than those of the world average concentration. Higher radioactive concentration was observed in soils than the parent rocks of sedimentary rock and metamorphic rock. The gamma radiation dose rate was in proportion to the radioactive concentration of the rocks. To clarify the radioactive effect in the change course of rocks into soils, comparative measurement of outcrop and soil radioactive concentrations is important. (S.Y.)

  17. Test procedures for salt rock

    International Nuclear Information System (INIS)

    Dusseault, M.B.

    1985-01-01

    Potash mining, salt mining, design of solution caverns in salt rocks, disposal of waste in salt repositories, and the use of granular halite backfill in underground salt rock mines are all mining activities which are practised or contemplated for the near future. Whatever the purpose, the need for high quality design parameters is evident. The authors have been testing salt rocks in the laboratory in a number of configurations for some time. Great care has been given to the quality of sample preparation and test methodology. This paper describes the methods, presents the elements of equipment design, and shows some typical results

  18. Applicability of solid-phase microextraction combined with gas chromatography atomic emission detection (GC-MIP AED) for the determination of butyltin compounds in sediment samples

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela 15782 (Spain)

    2004-11-01

    The performance of solid-phase microextraction (SPME) applied to the determination of butyltin compounds in sediment samples is systematically evaluated. Matrix effects and influence of blank signals on the detection limits of the method are studied in detail. The interval of linear response is also evaluated in order to assess the applicability of the method to sediments polluted with butyltin compounds over a large range of concentrations. Advantages and drawbacks of including an SPME step, instead of the classic liquid-liquid extraction of the derivatized analytes, in the determination of butyltin compounds in sediment samples are considered in terms of achieved detection limits and experimental effort. Analytes were extracted from the samples by sonication using glacial acetic acid. An aliquot of the centrifuged extract was placed on a vial where compounds were ethylated and concentrated on a PDMS fiber using the headspace mode. Determinations were carried out using GC-MIP AED. (orig.)

  19. Box-Behnken design in modeling of solid-phase tea waste extraction for the removal of uranium from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Khajeh, Mostafa; Jahanbin, Elham; Ghaffari-Moghaddam, Mansour; Moghaddam, Zahra Safaei [Zabol Univ. (Iran, Islamic Republic of). Dept. of Chemistry; Bohlooli, Mousa [Zabol Univ. (Iran, Islamic Republic of). Dept. of Biology

    2015-07-01

    In this study, the solid-phase tea waste procedure was used for separation, preconcentration and determination of uranium from water samples by UV-Vis spectrophotometer. In addition, Box-Behnken experimental design was employed to investigated the influence of six variables including pH, mass of adsorbent, eluent volume, amount of 1-(2-pyridylazo)-2-naphthol (PAN); and sample and eluent flow rates on the extraction of analyte. High determination coefficient (R{sup 2}) of 0.972 and adjusted-R{sup 2} of 0.943 showed the satisfactory adjustment of the polynomial regression model. This method was used for the extraction of uranium from real water samples.

  20. Increase by order of magnitude in quality factor during Cherenkov radiation detection in samples on solid carriers in glass cuvettes Kavalier

    International Nuclear Information System (INIS)

    Podracka, E.; Tykva, R.

    The method of measuring Cherenkov radiation is discussed developed by the authors, based on measuring samples on a solid carrier in glass scintillation cuvettes Kavalier. Increased interaction of emitted beta particles and modified measurement configuration were achieved by putting polyethylene foils of 0.3 mm in thickness and 17 mm in diameter straight to the sample or inserting a polyethylene tube of 13 mm in length and 15 mm in diameter down to the bottom of the cuvette in whose axis the sample is mounted. The application of the said technique can increase the quality factor by an order of magnitude when Czechoslovak-made cuvettes are used and a significantly higher value of quality factor can be obtained than when peak standard cuvettes imported from abroad and the original Huelsen and Prenzel's procedure are used. (B.S.)

  1. Ultrathin-shell boron nitride hollow spheres as sorbent for dispersive solid-phase extraction of polychlorinated biphenyls from environmental water samples.

    Science.gov (United States)

    Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Chen, Fan; Wu, Chi-Man Lawrence; Zhao, Rusong; Cheng, Chuange

    2014-11-21

    Boron nitride hollow spheres with ultrathin-shells were synthesized and used as sorbents for dispersive solid-phase extraction of aromatic pollutants at trace levels from environmental water samples. Polychlorinated biphenyls (PCBs) were selected as target compounds. Sample quantification and detection were performed by gas chromatography-tandem mass spectrometry. Extraction parameters influencing the extraction efficiency were optimized through response surface methodology using the Box-Behnken design. The proposed method achieved good linearity within the concentration range of 0.15-250 ng L(-1) PCBs, low limits of detection (0.04-0.09 ng L(-1), S/N=3:1), good repeatability of the extractions (relative standard deviation, spring waters were analyzed using the developed method. Results demonstrated that the hexagonal boron nitride-based material has significant potential as a sorbent for organic pollutant extraction from environmental water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Determination of quaternary ammonium compounds in seawater samples by solid-phase extraction and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Bassarab, P; Williams, D; Dean, J R; Ludkin, E; Perry, J J

    2011-02-04

    A method for the simultaneous determination of two biocidal quaternary ammonium compounds; didecyldimethylammonium chloride (didecyldimethyl quat) and dodecylbenzyldimethylammonium chloride (benzyl quat), in seawater by solid phase extraction (SPE) followed by liquid chromatography-mass spectrometry (LC-MS) was developed. The optimised procedure utilised off-line extraction of the analytes from seawater using polymeric (Strata-X) SPE cartridges. Recoveries ranged from 80 to 105%, with detection limits at the low parts-per-trillion (ng/l) level for both analytes. To demonstrate sensitivity, environmental concentrations were measured at three different locations along the North East coast of England with measured values in the range 120-270ng/l. Copyright © 2010 Elsevier B.V. All rights reserved.

  3. Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection.

    Science.gov (United States)

    Wang, Jun-Xia; Jiang, Dong-Qing; Gu, Zhi-Yuan; Yan, Xiu-Ping

    2006-12-22

    Determination of polybrominated diphenyl ethers (PBDEs) in environmental samples has raised great concerns due to the widespread use of PBDEs and their potential risk to humans. Solid-phase microextraction (SPME) is a fast, simple, cost-effective, and green sample preparation technique and is widely used for environmental analysis, but reports on the application of SPME for determination of PBDEs are very limited, and only a few publications dealing with commercial SPME fibers are available for extraction of PBDEs. Herein, we report a novel SPME method using multiwalled carbon nanotubes (MWCNTs) as the SPME fiber coating for gas chromatography with electron-capture detection (GC-ECD) of PBDEs in environmental samples. The MWCNTs coating gave much higher enhancement factors (616-1756) than poly (5% dibenzene-95% dimethylsiloxane) coating (139-384) and activated carbon coating (193-423). Thirty-minute extraction of 10 mL of sample solution using the MWCNTs coated fiber for GC-ECD determination yielded the limits of detection of 3.6-8.6 ng L(-1) and exhibited good linearity of the calibration functions (r(2)>0.995). The precision (RSD%, n=4) for peak area and retention time at the 500 ng L(-1) level was 6.9-8.8% and 0.6-0.9%, respectively. The developed method was successfully applied for the analysis of real samples including local river water, wastewater, and milk samples. The recovery of the PBDEs at 500 ng L(-1) spiked in these samples ranged from 90 to 119%. No PBDEs were detected in the river water and skimmed milk samples, whereas in the wastewater sample, 134-215 ng L(-1) of PBDEs were found. The PBDEs were detected in all whole fat milk samples, ranging from 13 to 484 ng L(-1). In a semiskimmed milk sample, only BDE-47 was found at 21 ng L(-1).

  4. Evaluation of the efficiency of injection of polyacrylamide in different reservoir-rock samples; Avaliacao da eficiencia de injecao de poliacrilamida em diferentes amostras de rocha-reservatorio

    Energy Technology Data Exchange (ETDEWEB)

    Marcelino, Cleuton P.; Valentim, Adriano C.M.; Medeiros, Ana Catarina R. de; Girao, Joaquim H.S.; Barcia, Rosangela B. [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil)

    2004-07-01

    Water soluble polymers have been used extensively in the petroleum recovery, due to their ability in increasing the viscosity of the injection water and to reduce water/oil mobility ratio and the water relative permeability in the reservoir. This reduction acts favorably as a secondary effect, and it reestablishes part of the pressure in the reservoir after the flow of the polymer, causing a correction of the injection profile in the wells through the restructuring of the resident fluids in the porous media. Nevertheless, some parameters influence the improve of this mechanism, such as petrophysics properties, chemical composition of the rock, adsorption, resistance factor and the residual resistance factor. Many paper in the area of polymers applied to the enhanced petroleum recovery indicate a high efficiency in the injection of different partially hydrolysed polyacrylamides, in different concentrations, or even in different injection conditions, as: temperature, flow, among others. In this work it was evaluated the behavior and efficiency of partially hydrolysed polyacrylamide flooding on outcrop cores from Botucatu, Rio Bonito, Clashach and Assu, using core flow tests and computer simulations. (author)

  5. Preconcentration and Determination of Perfluoroalkyl Substances (PFASs in Water Samples by Bamboo Charcoal-Based Solid-Phase Extraction Prior to Liquid Chromatography–Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Ze-Hui Deng

    2018-04-01

    Full Text Available In this work, bamboo charcoal was used as solid-phase extraction adsorbent for the enrichment of six perfluoroalkyl acids (PFAAs in environmental water samples before liquid chromatography–tandem mass spectrometry analysis. The specific porous structure, high specific surface area, high porosity, and stability of bamboo charcoal were characterized. Several experimental parameters which considerably affect extraction efficiency were investigated and optimized in detail. The experimental data exhibited low limits of detection (LODs (0.01–1.15 ng/L, wide linear range (2–3 orders of magnitude and R ≥ 0.993 within the concentration range of 0.1–1000 ng/L, and good repeatability (2.7–5.0%, n = 5 intraday and 4.8–8.3%, n = 5 interday and reproducibility (5.3–8.0%, n = 3. Bamboo charcoal was successfully used for the enrichment and determination of PFAAs in real environmental water samples. The bamboo charcoal-based solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry analysis possessed great potential in the determination of trace PFAA levels in environmental water samples.

  6. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

    International Nuclear Information System (INIS)

    He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

    2010-01-01

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  7. Preparation and characterization of magnetic carboxylated nanodiamonds for vortex-assisted magnetic solid-phase extraction of ziram in food and water samples.

    Science.gov (United States)

    Yılmaz, Erkan; Soylak, Mustafa

    2016-09-01

    A simple and rapid vortex-assisted magnetic solid phase extraction (VA-MSPE) method for the separation and preconcentration of ziram (zinc dimethyldithiocarbamate), subsequent detection of the zinc in complex structure of ziram by flame atomic absorption spectrometry (AAS) has been developed. The ziram content was calculated by using stoichiometric relationship between the zinc and ziram. Magnetic carboxylated nanodiamonds (MCNDs) as solid-phase extraction adsorbent was prepared and characterized by Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) spectrometry and scanning electron microscopy (SEM). These magnetic carboxylated nanodiamonds carrying the ziram could be easily separated from the aqueous solution by applying an external magnetic field; no filtration or centrifugation was necessary. Some important factors influencing the extraction efficiency of ziram such as pH of sample solution, amount of adsorbent, type and volume of eluent, extraction and desorption time and sample volume were studied and optimized. The total extraction and detection time was lower than 10min The preconcentration factor (PF), the precision (RSD, n=7), the limit of detection (LOD) and limit of quantification (LOQ) were 160, 7.0%, 5.3µgL(-1) and 17.5µgL(-1), respectively. The interference of various ions has been examined and the method has been applied for the determination of ziram in various waters, foodstuffs samples and synthetic mixtures. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Plasma emission induced by an Nd-YAG laser at low pressure on solid organic sample, its mechanism, and analytical application

    International Nuclear Information System (INIS)

    Suliyanti, Maria Margaretha; Sardy, Sar; Kusnowo, Anung; Hedwig, Rinda; Abdulmadjid, Syahrun Nur; Kurniawan, Koo Hendrik; Lie, T.J.; Pardede, Marincan; Kagawa, Kiichiro; Tjia, M.O.

    2005-01-01

    An Nd-YAG laser (1064 nm, 120 mJ, 8 ns) was focused on various types of solid organic samples such as a black acrylic plate, a black polyvinyl chloride plastic sheet, and a methoxy polyaniline film coated on the surface of a glass substrate, under a surrounding air pressure of 2 Torr. A modulated plasma technique was used to study the mechanism of excitation of the emission of the organic material. As a result, we conclude that ablated atoms and molecules are excited by a shock-wave mechanism, similar to the case of hard samples such as metal. The ablation speed of hydrogen emission (H I 656.2 nm) was examined and the results show that the release speed of the ablated atoms is relatively low (less than Mach 10) and persists for a longer period of time (around 1 μs); this phenomenon can be understood by assuming that the soft target absorbs recoil energy, causing a low release speed of ablated atoms which would form the shock wave. This was overcome by placing a subtarget on the back of the soft sample so as to enhance the repelling force, thus increasing the release speed of the atoms. A possible application of the low-pressure plasma on an organic solid was demonstrated in the detection of chlorine in a black polyvinyl chloride plastic sheet

  9. Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

    International Nuclear Information System (INIS)

    Ameli, Akram; Alizadeh, Naader

    2011-01-01

    Highlights: ► Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. ► This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. ► Proposed method, is particularly effective in sample clean-up and selective monitoring of salicylate in physiological samples. - Abstract: Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5 × 10 −8 to 5 × 10 −4 and 1.2 × 10 −6 to 5 × 10 −4 mol mL −1 and the detection limit was 4 × 10 −8 mol L −1 . The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

  10. Highly selective solid phase extraction and preconcentration of Azathioprine with nano-sized imprinted polymer based on multivariate optimization and its trace determination in biological and pharmaceutical samples

    International Nuclear Information System (INIS)

    Davarani, Saied Saeed Hosseiny; Rezayati zad, Zeinab; Taheri, Ali Reza; Rahmatian, Nasrin

    2017-01-01

    In this research, for first time selective separation and determination of Azathioprine is demonstrated using molecularly imprinted polymer as the solid-phase extraction adsorbent, measured by spectrophotometry at λ max 286 nm. The selective molecularly imprinted polymer was produced using Azathioprine and methacrylic acid as a template molecule and monomer, respectively. A molecularly imprinted solid-phase extraction procedure was performed in column for the analyte from pharmaceutical and serum samples. The synthesized polymers were characterized by infrared spectroscopy (IR), field emission scanning electron microscopy (FESEM). In order to investigate the effect of independent variables on the extraction efficiency, the response surface methodology (RSM) based on Box–Behnken design (BBD) was employed. The analytical parameters such as precision, accuracy and linear working range were also determined in optimal experimental conditions and the proposed method was applied to analysis of Azathioprine. The linear dynamic range and limits of detection were 2.5–0.01 and 0.008 mg L ‐1 respectively. The recoveries for analyte were higher than 95% and relative standard deviation values were found to be in the range of 0.83–4.15%. This method was successfully applied for the determination of Azathioprine in biological and pharmaceutical samples. - Graphical abstract: A new-nano sized imprinted polymer was synthesized and applied as sorbent in SPE in order to selective recognition, preconcentration, and determination of Azathioprine with the response surface methodology based on Box–Behnken design and was successfully investigated for the clean-up of human blood serum and pharmaceutical samples. - Highlights: • The nanosized-imprinted polymer has been synthesized by precipitation polymerization technique. • A molecularly imprinted solid-phase extraction procedure was performed for determination of Azathioprine. • The Azathioprine-molecular imprinting

  11. Modeling an in-register, parallel "iowa" aβ fibril structure using solid-state NMR data from labeled samples with rosetta.

    Science.gov (United States)

    Sgourakis, Nikolaos G; Yau, Wai-Ming; Qiang, Wei

    2015-01-06

    Determining the structures of amyloid fibrils is an important first step toward understanding the molecular basis of neurodegenerative diseases. For β-amyloid (Aβ) fibrils, conventional solid-state NMR structure determination using uniform labeling is limited by extensive peak overlap. We describe the characterization of a distinct structural polymorph of Aβ using solid-state NMR, transmission electron microscopy (TEM), and Rosetta model building. First, the overall fibril arrangement is established using mass-per-length measurements from TEM. Then, the fibril backbone arrangement, stacking registry, and "steric zipper" core interactions are determined using a number of solid-state NMR techniques on sparsely (13)C-labeled samples. Finally, we perform Rosetta structure calculations with an explicitly symmetric representation of the system. We demonstrate the power of the hybrid Rosetta/NMR approach by modeling the in-register, parallel "Iowa" mutant (D23N) at high resolution (1.2Å backbone rmsd). The final models are validated using an independent set of NMR experiments that confirm key features. Copyright © 2015 Elsevier Ltd. All rights reserved.

  12. Textural and fluid phase analysis of rock salt subjected to the combined effects of pressure, heat and gamma radiation

    International Nuclear Information System (INIS)

    Huertas, F.; Major, J.C.; Del Olmo, C.

    1992-01-01

    The formation of colloidal sodium by radiolytic processes is a main concern with respect to the safety of disposal of high-level radioactive waste in salt formations. The research work seeks to assess the irradiation damage in natural rock salt when exposed to a different dose, dose rate, temperature and time of gamma irradiation. The work encompasses four major tasks: (i) detailed characterization of both solid and fluid phases of natural rock salt; (ii) gamma irradiation of salt samples; (iii) determination of the amount of colloidal sodium present in irradiated samples; (iv) calculation of radiation damage. 40 refs., 36 figs., 34 tabs

  13. Acquisition of reproducible transmission near-infrared (NIR) spectra of solid samples with inconsistent shapes by irradiation with isotropically diffused radiation using polytetrafluoroethylene (PTFE) beads.

    Science.gov (United States)

    Lee, Jinah; Duy, Pham Khac; Yoon, Jihye; Chung, Hoeil

    2014-06-21

    A bead-incorporated transmission scheme (BITS) has been demonstrated for collecting reproducible transmission near-infrared (NIR) spectra of samples with inconsistent shapes. Isotropically diffused NIR radiation was applied around a sample and the surrounding radiation was allowed to interact homogeneously with the sample for transmission measurement. Samples were packed in 1.40 mm polytetrafluoroethylene (PTFE) beads, ideal diffusers without NIR absorption, and then transmission spectra were collected by illuminating the sample-containing beads using NIR radiation. When collimated radiation was directly applied, a small portion of the non-fully diffused radiation (NFDR) propagated through the void space of the packing and eventually degraded the reproducibility. Pre-diffused radiation was introduced by placing an additional PTFE disk in front of the packing to diminish NFDR, which produced more reproducible spectral features. The proposed scheme was evaluated by analyzing two different solid samples: density determination for individual polyethylene (PE) pellets and identification of mining locality for tourmalines. Because spectral collection was reproducible, the use of the spectrum acquired from one PE pellet was sufficient to accurately determine the density of nine other pellets with different shapes. The differentiation of tourmalines, which are even more dissimilar in appearance, according to their mining locality was also feasible with the help of the scheme.

  14. Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of ecstasy compounds and amphetamines in biological samples

    Directory of Open Access Journals (Sweden)

    H. A. Mashayekhi

    2014-09-01

    Full Text Available A novel approach for the determination of ecstasy and amphetamines (3,4-methylenedioxymethylamphetamine (MDMA, Ecstasy, 3,4-methylenedioxyamphetamine (MDA, 3,4-methylenedioxyethylamphetamine (MDEA and 3,4-methylenedioxypropylamphetamine (MDPA in biological samples is presented. The analytes were extracted from the matrix and transferred to a small volume of a high density, water insoluble solvent using solid-phase extraction (SPE followed by dispersive liquid-liquid microextraction (DLLME. This combination not only resulted in a high enrichment factor, but also it could be used in complex matrices (biological samples. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, were studied and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.5-500 µg L-1 and 1.0-500 µg L-1 with detection limits in the range of 0.1-0.3 µg L-1 and 0.2-0.7 µg L-1 in urine and plasma samples, respectively. The results showed that SPE-DLLME is a suitable method for the determination of ecstasy components and amphetamines in biological and water samples. DOI: http://dx.doi.org/10.4314/bcse.v28i3.3

  15. Ultrasound-assisted extraction and solid-phase extraction for the simultaneous determination of five amide herbicides in fish samples by gas chromatography with electron capture detection.

    Science.gov (United States)

    Qu, Zhipeng; Bai, Xiuzhi; Zhang, Ting; Yang, Zhaoguang

    2017-03-01

    An efficient sample extraction and clean-up method was developed for simultaneous determination of five amide herbicides (alachlor, acetochlor, propisochlor, metazachlor, and butachlor) in fish samples. The protocol consisted of ultrasound-assisted solvent extraction and solid-phase extraction clean-up. In detail, aliquots of homogenized fish flesh were thoroughly mixed with 20 mL of n-hexane and then extracted with ultrasonication for 40 min. Each sample was centrifuged and the supernatant was collected for the subsequent clean-up. For the sample preparation, the above supernatant was processed with a C 18 column with 3 mL of dichloromethane/n-hexane (1:1, v/v) as the eluant. Then the samples were analyzed by gas chromatography with electron capture detection. The correlation coefficients of the five calibration curves were 0.9976-0.9998 (n = 3). The limits of detection (S/N = 3, n = 11) and limits of quantification (S/N = 10, n = 11) were 0.19-0.42 and 0.63-1.39 μg/kg, respectively. The recoveries of this method were 71.2-92.6% with good precision (<4.7% relative standard deviations, n = 6). The developed method was successfully applied to monitor the five amide herbicides in fish samples collected from different cities. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

    Science.gov (United States)

    Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

    2016-06-01

    Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

    2015-12-01

    The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

  18. A sensitive method for determining total vanadium in water samples using colorimetric-solid-phase extraction-fiber optic reflectance spectroscopy

    International Nuclear Information System (INIS)

    Filik, Hayati; Yanaz, Zeynep

    2009-01-01

    A selective colorimetric-solid-phase extraction (C-SPE) method for the determination of total vanadium in water samples was developed. This method introduced a new variation of C-SPE. The colour reaction is based on the reaction of vanadium(V) ternary complex formed with 1-(2-Pyridylazo)-2-naphtol (PAN) in the presence hydrogen peroxide (H 2 O 2 ). In this technique, the target analytes in samples are extracted onto solid matrix loaded with a colorimetric reagent and then quantified directly on the adsorbent surface by using a miniature fiber optic reflectance spectrometer. The measurements were carried out at a wavelength of 589.4 nm since it yielded the largest divergence different in reflectance spectra before and after reaction with the vanadium. The overall time required for the C-SPE procedure was ∼20 min. The amount of concentrated V is then determined in a few seconds by using miniature reflectance spectrometer. At the optimal conditions, a calibration curve was constructed, revealing a linear range of 0.05-0.52 mg L -1 and a detection limit as low as 0.01 mg L -1 while the RSD lower than 2.8%. In order to verify the accuracy of the method, a certified reference water samples (TMDA) were analysed and the results obtained were in good agreement with the certified values. The proposed method was applied to the determination of vanadium in tap water, seawater samples with a recovery for the spiked samples in the range of 98-102%.

  19. Solid phase microextraction sampling of high explosive residues in the presence of radionuclides and radionuclide surrogate metals

    International Nuclear Information System (INIS)

    Duff, M.C.; Crump, S.L.; Ray, R.J.; Beals, D.; Cotham, W.E.; Mount, K.; Koons, R.D.; Leggitt, J.

    2008-01-01

    The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) evidence while maintaining evidentiary value. One experimental method for the isolation of HE residue involves using solid phase microextraction (SPME) fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ( 239/240 Pu, 238 U, 237 Np, 85 Sr, 133 Ba, 137 Cs, 60 Co and 226 Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection. (author)

  20. Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching

    Science.gov (United States)

    Song, Q.; Putcha, L.; Harm, D. L. (Principal Investigator)

    2001-01-01

    A chromatographic method for the quantitation of promethazine (PMZ) and its three metabolites in urine employing on-line solid-phase extraction and column-switching has been developed. The column-switching system described here uses an extraction column for the purification of PMZ and its metabolites from a urine matrix. The extraneous matrix interference was removed by flushing the extraction column with a gradient elution. The analytes of interest were then eluted onto an analytical column for further chromatographic separation using a mobile phase of greater solvent strength. This method is specific and sensitive with a range of 3.75-1400 ng/ml for PMZ and 2.5-1400 ng/ml for the metabolites promethazine sulfoxide, monodesmethyl promethazine sulfoxide and monodesmethyl promethazine. The lower limits of quantitation (LLOQ) were 3.75 ng/ml with less than 6.2% C.V. for PMZ and 2.50 ng/ml with less than 11.5% C.V. for metabolites based on a signal-to-noise ratio of 10:1 or greater. The accuracy and precision were within +/- 11.8% in bias and not greater than 5.5% C.V. in intra- and inter-assay precision for PMZ and metabolites. Method robustness was investigated using a Plackett-Burman experimental design. The applicability of the analytical method for pharmacokinetic studies in humans is illustrated.

  1. Final Report For The Initial Solid Phase Characterization Of The 2011 Grab Samples And Composite For The C-109 Hard Heel Study

    International Nuclear Information System (INIS)

    Page, J.S.; Cooke, G.A.; Pestovich, J.A.

    2011-01-01

    On May 3, 2011, solid phase characterization subsamples were taken from six of the eight grab samples that had been collected from tank 241-C-109 in April, 2011 and delivered to the 222-S Laboratory. These subsamples were characterized in order to guide the creation of the composite for the C-109 hard heel study. Visual observation showed that there was a large variability in the physical characteristics of the eight individual grab samples. Several of the grab samples consisted of 'stone-like' cobbles (several > 25 mm in diameter) while the other grab samples were of a finer granular composition referred to as 'bulk material'. Half of the six subsamples taken for this initial SPC were of crushed cobbles and half were of the bulk material. Scanning electron microscopy was performed on all six subsamples, and X-ray diffraction was performed on all three of the 'bulk material' samples and one of the crushed cobble samples. The crushed cobbles were found to be composed primarily of gibbsite (Al(OHh) 3 ). Analysis by X-ray diffraction indicated gibbsite to be the only crystalline phase detected, and scanning electron microscopy showed the crushed cobbles to consist primarily of aggregates of euhedral to subhedral gibbsite crystals that were 20 to 100 μm in size. The aggregates, having a moderate amount of pore space, were cemented primarily by recrystallized gibbsite making them resistant to crushing. The bulk material consisted of coarse to fine-grained pebble-sized (2 to 20 mm) particles. The X-ray diffraction analysis showed them to be a mixture of natrophosphate (Na 7 (PO 4 ) 2 F·19(H 2 O)) and gibbsite crystals in varying amounts in each of the three subsamples (i.e., some grab samples were primarily natrophosphate while others were mixed with gibbsite). The scanning electron microscopy analysis of the bulk material showed the crystals to be euhedral to anhedral (rounded) in shape. Trace phases, too minor to be detected by XRD, were observed in the SEM analysis

  2. Utility of solid phase spectrophotometry for the modified determination of trace amounts of cadmium in food samples.

    Science.gov (United States)

    Amin, Alaa S; Gouda, Ayman A

    2012-05-01

    A modified selective, highly sensitive and accurate procedure for the determination of trace amounts of cadmium which reacts with 1-(2-benzothiazolylazo)-2-hydroxy-3-naphthoic acid (BTAHNA) to give a deep violet complex with high molar absorptivity (7.05×10(6)Lmol(-1) cm(-1), 3.92×10(7)Lmol(-1)cm(-1), 1.78×10(8)Lmol(-1)cm(-1), and 4.10×10(8)Lmol(-1)cm(-1)), fixed on a Dowex 1-X8 type anion-exchange resin for 10mL, 100mL, 500mL, and 1000mL, respectively. Calibration is linear over the range 0.2-3.5μgL(-1) with RSD of ⩽1.14% (n=10). The detection and quantification limits were calculated. Increasing the sample volume can enhance the sensitivity. The method has been successfully applied for the determination of Cd(II) in food