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Sample records for solid granite samples

  1. 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)

  2. Trace Analysis of Irradiated Granite Samples from Hiroshima by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Amr, M.A.; Helal, N.F.; Zahran, N.F.; Becker, J.S.; Pickhardt, C.; Dietze, H.J.

    1999-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is widely accepted as a rapid and sensitive technique for trace elemental analysis of solid materials and for local analysis of inhomogeneous materials (such as geological samples). Due to its direct solid sample analysis capability, LA-ICP-MS (using a quadrupole based ICP-MS and at the Research Center Juelich developed laser ablation system: Nd-YAG-laser, 226 nm, 10 Hz and 5 ns) is applied for the analysis of geological (granite) samples from Hiroshima. In order to prepare homogeneous targets, these samples were melted together with a lithium-borate mixture in a muffle furnace at 1050 degree c. Furthermore, for investigating of matrix effects the powder of these samples is mixed with graphite and pressed as targets for laser ablation. The quantification of the analysis results was carried out using granite (GM) as standard reference material. The relative sensitivity coefficients (RSCs) for most elements, which were determined for correction of the measured values, varied between 0.3 and 3

  3. Characterization of natural colloids sampled from a fractured granite groundwater

    Energy Technology Data Exchange (ETDEWEB)

    Baik, Min Hoon; Keum, Dong Kwon; Hahn, Pil Soo [Korea Atomic Energy Research Institute, Taejeon (Korea); Vilks, Peter [AECL Whiteshell Laboratories (Canada)

    2000-02-01

    This study was carried out as a part of international joint study of KAERI with AECL. The main purpose of this study is to analyze the physicochemical characteristics and sorption properties of natural colloids sampled from the deep fractured granite groundwater located in the Underground Research Laboratory (URL) of AECL. Physicochemical characteristics such as composition, size distribution, and concentrations of natural colloids was analyzed. This study will be basic data for the analysis of the effect of colloids on the radionuclide migration in a geological medium. This study may provide information for the evaluation of the roles and effects of colloids in the safety and performance assessment of a possible future radioactive waste repository. 20 refs., 8 figs., 8 tabs. (Author)

  4. The correlation between selenium adsorption and the mineral and chemical composition of Taiwan local granite samples

    Energy Technology Data Exchange (ETDEWEB)

    Wang, TsingHai; Chiang, Chu-Ling; Wang, Chu-Fang [National Tsing Hua Univ., Hsinchu, Taiwan (China). Biomedical Engineering and Environmental Sciences

    2015-07-01

    Selenium-79 (Se-79) is a radioactive isotope of selenium, which is considered as one of the highly mobile nuclides since Se-79 would be presented in an anion species when dissolving into the intruded groundwater. Being an anionic species, the transport of Se-79 would be regulated by the metal oxides relevant minerals such as goethite and hematite (Jan et al., 2008). This is true that the transport of selenium in the shallow surface environment could be relatively easy to estimate by considering the amount of these metal oxides presenting in the soils and sediments. However, when dealing with deep geological repository, the transport of Se-79 becomes less predictable because of the much less content of metal oxide residing in the host rock such as granite. In order to conduct a reliable performance assessment of repository, it is very important to establish the correlation between selenium adsorption and the properties of potential host rock, in this study, the mineral and chemical compositions of Taiwan local granite. From this point of view, selenium adsorption experiments were conducted with 54 different Taiwan local granite samples collected from the depth ranging from 100 ∝ 400 meters below the surface. These granite samples represent a variety of deep geological environments, including the intact rock, groundwater intruded zones, and some weathered samples. Based upon our preliminary results, several solid conclusions could be made. First, the correlation coefficients between the Kd values and the mineral and chemical compositions are rather low (R-square values are often < 0.2). This points out the complexity of these geological samples and strongly suggests more efforts should be put into to acquire more relevant information. Second, the correlation between the selenium Kd values and the content of iron oxide (R-square 0.110) is much higher than that between the CEC of these granite samples (R-square 0.001). This clearly indicates that the minerals that

  5. REE Comparison Between Muncung Granite Samples and their Weathering Products, Lingga Regency, Riau Islands

    Directory of Open Access Journals (Sweden)

    Ronaldo Irzon

    2016-11-01

    Full Text Available DOI:10.17014/ijog.3.3.149-161The increasing demand for Rare Earth Elements (REE is related to the continous development of technology, and these elements are used in modern equipments. REE can occur in igneous and sedimentary rocks in significant amounts as primary deposits, whereas the secondary REE deposit can be produced by intensive lateritic weathering of bedrocks under the tropical or subtropical climate. Lateritic process can increase REE concentration from sub-economic levels in host rocks to be more valuable. Muncung Granite is located in a tropical area of Lingga Regency, Riau Islands Province. REE occurs in the Muncung Granite and in weathered layers (saprolite, laterite, and soil. ICP-MS was applied to measure the REE content in all samples of this study. The average REE content of the Muncung Granite is 265 ppm with Eu anomaly in REE’s spider diagrams. Lateritization process has increased REE content by more than four times compared to that in the Muncung Granite. Ce and Eu anomalies in weathered layers can be associated with weathering process and initial REE contents in the host rock. Ce anomaly in a laterite layer is found to have a negative correlation to REE total enrichment. The REE level in the Muncung Granite is higher than the content in the soil and saprolite layers, but lower than that in the laterite.

  6. Characterization and application of municipal solid waste incineration (MSWI) bottom ash and waste granite powder in alkali activated slag

    NARCIS (Netherlands)

    Gao, X.; Yuan, B.; Yu, Q. L.; Brouwers, H. J.H.

    2017-01-01

    In this paper, the feasibility of using two solid wastes in alkali activated slag composites as construction and building materials is evaluated. One waste is the municipal solid waste incineration (MSWI) bottom ash, and the other one is fine granite powder from aggregate manufacturing. These two

  7. Determination of low concentrations of uranium in granite samples by X-ray fluorescence

    International Nuclear Information System (INIS)

    Roca, M.; Diaz-Guerra, J.P.

    1981-01-01

    An x-ray fluorescence method for the determination of uranium in granite samples for concentrations ranging from 3 to 100 ppm U 3 O 8 has been developed. To this purpose a sample holder, specially designed, allowing the irradiation of sample surfaces 42.5 mm in diameter and a molybdenum tube operating with a power of 2700 W (90 kV, 30 mA) are used. The background influence and the spectral interferences from rubidium and strontium have been taken into account and specific correction coefficients have been computed. A Basic program facilitates the report of the analytical results. (author)

  8. Use of alpha spectrometry for analysis of U-isotopes in some granite samples

    International Nuclear Information System (INIS)

    El-Galy, M.M.; Desouky, O.A.; Khattab, M.R.; Issa, F.A.

    2011-01-01

    The present study aims to use the α-spectrometry, at NMA. A radiochemical technique for analysis of U-isotopes was carried out for some granite samples from Gabal Gattar and El Missikat localities and also for some reference soil samples of IAEA. Several steps of sample preparation, radiochemical separation, and source preparation were performed before analysis. The concerned sample was leached by HNO 3 , HF and H 2 O 2 acids after ashing. The ashed sample was spiked with uranium tracer ( 232 U) for chemical yield and activity calculation. Then uranium was extracted from the matrix elements with trioctylphosphine oxide (TOPO) and stripped with 1 M NH 4 F/0.1 M HCl solution. The uranium fraction was purified by co-precipitation with LaF 3 to ensure complete removal of thorium and traces of resolution degrading elements. This was followed by a final clean-up step using an anion exchange. The pure uranium fraction was electrodeposited on a stainless steel disc from HCl/oxalate solution. The obtained results from the soil reference samples indicate general similarities between the techniques of α-spectrometers of NMA, EAEA and IAEA for analysis of U-isotopes. The U-isotopes in the granite samples of high radioactivity levels need more attempts after dilution process to be in the limit detection of α-spectrometry. (author)

  9. Correlation between radon exhalation and radium content in granite samples used as construction material in Saudi Arabia

    Energy Technology Data Exchange (ETDEWEB)

    Al-Jarallah, M.I. [Department of Physics, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia)]. E-mail: mibrahim@kfupm.edu.sa; Fazal-ur-Rehman [Department of Physics, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Musazay, M.S. [Department of Physics, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Aksoy, A. [Department of Physics, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia)

    2005-11-15

    Measurements of radon exhalation for a total of 205 selected samples of construction materials used in Saudi Arabia were carried out using an active radon gas analyzer with an emanation container. It was found that granite samples were the main source of radon exhalation. The radon exhalation rates per unit area from these granite samples varied from below the minimum detection limit up to 13.1Bqm{sup -2}h{sup -1} with an average of 1.5 +/-1.9(1{sigma})Bqm{sup -2}h{sup -1}. The radium contents of 27 granite samples were measured using an HPGe-based {gamma} spectroscopy setup. The {sup 226}Ra content of the granites varied from below the minimum detection limit up to 297Bqkg{sup -1}, with an average of 83+/-73(1{sigma})Bqkg{sup -1}. The linear correlation coefficient between exhaled radon and radium content was found to be 0.90.

  10. 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

  11. 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.

  12. Sample damage investigation by laboratory testing and DDM modelling by FRACOD2D of Brazilian tests on Toki granite

    International Nuclear Information System (INIS)

    Lanaro, Flavio; Sato, Toshinori; Funato, Akio

    2008-01-01

    Numerical scooping calculations by means of FRACOD 2D had shown that Brazilian test models present a bend in the relation between the sample deformation perpendicularly to the loading direction and the load itself. The input 'direct' tensile strength of the rock could be re-obtained based on the numerical load at the bend. In this study, a similar technique is applied to specially designed Brazilian tests on Toki granite (Gifu, Japan) which also exhibits such bend for a tensile stress in the centre of the samples of about 2.6 MPa. However, the samples show a wide range of Brazilian tensile strengths that appear to be negatively correlated to the level of in-situ stress at the depth where the samples were taken. The correlation was interpreted as an effect of sample damage due to drilling in a stressed rock mass. Numerical models were designed with various preexist ent crack patterns to simulate the sample damage. The numerical results show Brazilian peak strength results ranging between 6.7 and 13.0 MPa, which are very realistic considering that the laboratory Brazilian tensile strength was observed to vary between 4.1 and 11.3 MPa. These values are all larger than the stress at the bend which is then interpreted as the tensile strength of the weakest grains in the granite. It is also shown that the occurrence of newly initiated cracks at the bend completely changes the stress distribution and failure mechanism of the samples: this explains why the Brazilian tensile strength should be higher than the 'direct' tensile strength of the rock from uniaxial tests. (author)

  13. AMS studies in Portuguese variscan granites

    Science.gov (United States)

    Sant'Ovaia, Helena; Martins, Helena; Noronha, Fernando

    2014-05-01

    A large volume of Variscan granitic rocks outcrop in Central Iberian Zone which are well documented concerning geological mapping, petrography and geochemistry but whose magnetic characteristics and fabric remain unknown. In this study we summarize the available AMS data from approximately 644 sampling stations (5152 samples) on different massifs of Variscan Portuguese granites. Despite their different geological, petrographic and geochemical characteristics, magnetic susceptibility (K) values obtained for the majority of the studied granites range from 15 to 300 × 10-6 SI. The dominant paramagnetic behaviour of the granite bodies reflects the presence of ilmenite as the main iron oxide. This feature indicates the reduced conditions involved in the granite melt formation during the Variscan orogeny. The two-mica granites show K values ranging between 15 to 70 × 10-6 SI which are lower than values displayed by the biotite-rich facies scattered within the interval of 70 and 300 × 10-6 SI. The magnetite-bearing granites are scarce but represented in Lavadores, Gerês and Manteigas. Even so, only the Lavadores body could be considered as a true magnetite-type granite (K >3.0 × 10-3 SI) in face of its K, comprised between 1550 and 19303 × 10-6 SI. Magnetic anisotropy can be used as a "marker" for the deformation experienced by granite mushes during their crustal emplacement and further cooling. Magnetic anisotropy can thus be correlated with the finite deformation of a rock, as record by mineral fabrics. Post-tectonic granites, such as those from Vila Pouca de Aguiar, Pedras Salgadas, Caria, Vila da Ponte, Chaves and Lamas de Olo, have a magnetic anisotropy <2.5% which corresponds to a deformation hardly visible to the naked eye. Nevertheless, at microscopic scale, these granites display almost ubiquitous magmatic to submagmatic microstructures (rare wavy extinction in quartz, erratic subgrain boundaries in quartz and, eventually, folded or kinked biotites). For

  14. 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

  15. 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

  16. 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.)

  17. Distribution of elements among minerals of a single (muscovite-) biotite granite sample – an optimal approach and general implications

    Czech Academy of Sciences Publication Activity Database

    Janoušek, V.; Navrátil, Tomáš; Trubač, J.; Strnad, J.; Laufek, F.; Minařík, Luděk

    2014-01-01

    Roč. 65, č. 4 (2014), s. 257-271 ISSN 1335-0552 Institutional research plan: CEZ:AV0Z30130516 Institutional support: RVO:67985831 Keywords : modal analyses * trace-element residence * ICP -MS * Central Bohemian Plutonic Complex * Říčany granite Subject RIV: DD - Geochemistry Impact factor: 0.761, year: 2014

  18. Failure Characteristics of Granite Influenced by Sample Height-to-Width Ratios and Intermediate Principal Stress Under True-Triaxial Unloading Conditions

    Science.gov (United States)

    Li, Xibing; Feng, Fan; Li, Diyuan; Du, Kun; Ranjith, P. G.; Rostami, Jamal

    2018-05-01

    The failure modes and peak unloading strength of a typical hard rock, Miluo granite, with particular attention to the sample height-to-width ratio (between 2 and 0.5), and the intermediate principal stress was investigated using a true-triaxial test system. The experimental results indicate that both sample height-to-width ratios and intermediate principal stress have an impact on the failure modes, peak strength and severity of rockburst in hard rock under true-triaxial unloading conditions. For longer rectangular specimens, the transition of failure mode from shear to slabbing requires higher intermediate principal stress. With the decrease in sample height-to-width ratios, slabbing failure is more likely to occur under the condition of lower intermediate principal stress. For same intermediate principal stress, the peak unloading strength monotonically increases with the decrease in sample height-to-width. However, the peak unloading strength as functions of intermediate principal stress for different types of rock samples (with sample height-to-width ratio of 2, 1 and 0.5) all present the pattern of initial increase, followed by a subsequent decrease. The curves fitted to octahedral shear stress as a function of mean effective stress also validate the applicability of the Mogi-Coulomb failure criterion for all considered rock sizes under true-triaxial unloading conditions, and the corresponding cohesion C and internal friction angle φ are calculated. The severity of strainburst of granite depends on the sample height-to-width ratios and intermediate principal stress. Therefore, different supporting strategies are recommended in deep tunneling projects and mining activities. Moreover, the comparison of test results of different σ 2/ σ 3 also reveals the little influence of minimum principal stress on failure characteristics of granite during the true-triaxial unloading process.

  19. Leaching of gallium from gaiter granite, eastern desert, Egypt

    International Nuclear Information System (INIS)

    Zahran, M.A.; Mahmoud, KH.F.; Mahdy, M.A.; Abd El-Hamid, A.M.

    2006-01-01

    Preliminary leaching tests of gallium from some Egyptian granite rocks such as those of Gabal Gattar area was investigated by using 8 M HCl acid and sodium perchlorate as oxidant. To achieve the optimum leaching conditions, the factors affecting the leaching efficiency as the acid type and concentration, oxidant type and amount, leaching temperature, agitation time, solid / liquid ratio and the effect of grain size were studied. The complete chemical analysis of the collected samples was firstly carried out to determine the chemical features of the Gattarian granite. More than 97% of gallium content was leached when applying these optimum leaching conditions

  20. 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)

  1. 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

  2. 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.)

  3. 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)

  4. Uranium in granites

    International Nuclear Information System (INIS)

    Maurice, Y.T.

    1982-01-01

    Recent research activities of the Canadian Uranium in Granites Study are presented in 18 papers and 3 abstracts. 'Granites' is used as a generic term for granitoids, granitic rocks, and plutonic rocks

  5. 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...

  6. 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.

  7. 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

  8. 2005 dossier: granite; Dossier 2005: granite

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2005-07-01

    This document makes a status of the researches carried out by the French national agency of radioactive wastes (ANDRA) about the geologic disposal of high-level and long-lived radioactive wastes in granite formations. Content: 1 - advantage of granitic formations for the geologic disposal; 2 - containers; 3 - design study of a disposal facility in granitic environment; 4 - understanding and modelling of granite; 5 - description of disposal concepts in granitic environment; 6 - long-term and safety aspects; 7 - conclusion. (J.S.)

  9. 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.

  10. Calibrated acoustic emission system records M -3.5 to M -8 events generated on a saw-cut granite sample

    Science.gov (United States)

    McLaskey, Gregory C.; Lockner, David A.

    2016-01-01

    Acoustic emission (AE) analyses have been used for decades for rock mechanics testing, but because AE systems are not typically calibrated, the absolute sizes of dynamic microcrack growth and other physical processes responsible for the generation of AEs are poorly constrained. We describe a calibration technique for the AE recording system as a whole (transducers + amplifiers + digitizers + sample + loading frame) that uses the impact of a 4.76-mm free-falling steel ball bearing as a reference source. We demonstrate the technique on a 76-mm diameter cylinder of westerly granite loaded in a triaxial deformation apparatus at 40 MPa confining pressure. The ball bearing is dropped inside a cavity within the sample while inside the pressure vessel. We compare this reference source to conventional AEs generated during loading of a saw-cut fault in a second granite sample. All located AEs occur on the saw-cut surface and have moment magnitudes ranging from M −5.7 down to at least M −8. Dynamic events rupturing the entire simulated fault surface (stick–slip events) have measurable stress drop and macroscopic slip and radiate seismic waves similar to those from a M −3.5 earthquake. The largest AE events that do not rupture the entire fault are M −5.7. For these events, we also estimate the corner frequency (200–300 kHz), and we assume the Brune model to estimate source dimensions of 4–6 mm. These AE sources are larger than the 0.2 mm grain size and smaller than the 76 × 152 mm fault surface.

  11. Natural radionuclide distribution in Brazilian commercial granites

    International Nuclear Information System (INIS)

    Anjos, R.M.; Veiga, R.; Soares, T.; Santos, A.M.A.; Aguiar, J.G.; Frasca, M.H.B.O.; Brage, J.A.P.; Uzeda, D.; Mangia, L.; Facure, A.; Mosquera, B.; Carvalho, C.; Gomes, P.R.S.

    2005-01-01

    The dimension stones sector in Brazil produces several varieties of granites, marbles, slates and basalts. More than half of this production corresponds to around 200 different commercial types of granites with specific names, geographical and geological origins and mineral compositions. The well-known natural radioactivity present in rocks, where high radiation levels are associated with igneous rocks such as granite, can be used to determine their general petrologic features. This subject is important in environmental radiological protection, since granites are widely used as building and ornamental stones. In this paper, it is applied to correlate the petrographic characteristics of commercial granites with their corresponding dose rates for natural radioactivity. Amounts of thorium, uranium and potassium concentrations have been reported in several Brazilian commercial granite samples

  12. 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.

  13. 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.

  14. 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 ...

  15. 2005 dossier: granite

    International Nuclear Information System (INIS)

    2005-01-01

    This document makes a status of the researches carried out by the French national agency of radioactive wastes (ANDRA) about the geologic disposal of high-level and long-lived radioactive wastes in granite formations. Content: 1 - advantage of granitic formations for the geologic disposal; 2 - containers; 3 - design study of a disposal facility in granitic environment; 4 - understanding and modelling of granite; 5 - description of disposal concepts in granitic environment; 6 - long-term and safety aspects; 7 - conclusion. (J.S.)

  16. Application of Solvent-In-Pulp Technique for Uranium Extraction from Mineralization Granite

    International Nuclear Information System (INIS)

    Ali, M.M.; Hussein, A.E.M.; Youseif, W.M.; El Didamony, A.M.

    2017-01-01

    Investigations on uranium extraction from a representative mineralized granite sample (Gattar granite GII) by solvent-in-pulp (SIP) technique were carried out in the present study. For this purpose, the solvent (tri-butyl amine) (TBA) was mixed with the leaching slurry without prior filtration. The influence of various factors affecting the SIP process, such as contact time, solvent concentration, dilution factor, type of surfactant, surfactant/solid ratio were studied. About 91% uranium extraction efficiency was attained by the application of the chosen extraction SIP conditions. Also, about 96% of the loaded uranium could be stripped by using sulfuric acid as an effective stripping agent

  17. The petrology, geochronology and significance of Granite Harbour Intrusive Complex xenoliths and outcrop sampled in western McMurdo Sound, Southern Victoria Land, Antarctica

    International Nuclear Information System (INIS)

    Martin, A.P.; Cooper, A.F.; Price, R.C.; Turnbull, R.E.; Roberts, N.M.W.

    2015-01-01

    Granite Harbour Intrusive Complex xenoliths in McMurdo Volcanic Group rocks and in situ outcrops have been studied from Mount Morning, western McMurdo Sound, Antarctica. Calc-alkalic samples have whole rock signatures and normative compositions similar to the Dry Valleys 1b suite, and zircon grains in one specimen yield a 545.2 ± 4.4 Ma crystallisation age. This supports subduction-related magmatism initiating in Southern Victoria Land by 545 Ma. A second group of xenoliths is alkalic, with titanite grains in one xenolith from this group dated at 538 ± 8 Ma. Whole rock chemistry, normative compositions and geochronology of the alkalic group are comparable to the Koettlitz Glacier Alkaline Suite (KGAS). The position of a proposed lower crustal discontinuity that may form a significant basement suture in the McMurdo Sound region is newly constrained to the east of Mount Morning, perhaps along the trace of the Discovery Glacier. The boundary between East and West Antarctica may also pass along the trace of the Discovery Glacier if, as previously hypothesised, its location is controlled by the basement suture. A significant basement suture may also have provided the necessary egress for the (regionally) early and sustained magmatic activity observed at Mount Morning over the last 24 million years. (author).

  18. Radon exhalation from granitic rocks

    International Nuclear Information System (INIS)

    Del Claro, Flávia; Paschuk, Sergei A.; Corrêa, Janine N.; Mazer, Wellington; Narloch, Danielle Cristine; Martin, Aline Cristina; Denyak, Valeriy

    2017-01-01

    Naturally occurring radionuclides such as radon ( 222 Rn), its decay products and other elements from the radioactive series of uranium ( 238 U and 235 U) and thorium ( 232 Th) are an important source of human exposure to natural radioactivity. The worldwide evaluation of health radiobiological effects and risks from population exposure to natural radionuclides is a growing concern. About 50% of personal radiation annual dose is related to radionuclides such as radon ( 222 Rn), thoron ( 220 Rn), radium ( 226 Ra), thorium ( 232 Th) and potassium ( 40 K), which are present in modern materials commonly used in construction of dwellings and buildings. The radioactivity of marbles and granites is of big concern since under certain conditions the radioactivity levels of these materials can be hazardous to the population and require the implementation of mitigation procedures. Present survey of the 222 Rn and 220 Rn activity concentration liberated in the air was performed using commercialized Brazilian granite rocks at national market as well as exported to other countries. The 222 Rn and 220 Rn measurements were performed using the AlphaGUARD instant monitor and RAD7 detector, respectively. This study was performed at the Applied Nuclear Physics Laboratory of the Federal University of Technology – Paraná (UTFPR). Obtained results of radon concentration activity in air exhaled studied samples of granites varied from 3±1 Bq/m 3 to 2087±19 Bq/m 3 , which shows that some samples of granitic rocks represent rather elevated health risk the population. (author)

  19. 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.

  20. Uranium rich granite and uranium productive granite in south China

    Energy Technology Data Exchange (ETDEWEB)

    Mingyue, Feng; Debao, He [CNNC Key Laboratory of Uranium Resource Exploration and Evaluation Technology, Beijing Research Institute of Uranium Geology (China)

    2012-07-15

    The paper briefly introduces the differences between uranium rich granite and uranium productive granite in the 5 provinces of South China, and discusses their main characteristics in 4 aspects, the uranium productive granite is highly developed in fracture, very strong in alteration, often occurred as two-mica granite and regularly developed with intermediate-basic and acid dikes. The above characteristics distinguish the uranium productive granite from the uranium rich granite. (authors)

  1. Uranium rich granite and uranium productive granite in south China

    International Nuclear Information System (INIS)

    Feng Mingyue; He Debao

    2012-01-01

    The paper briefly introduces the differences between uranium rich granite and uranium productive granite in the 5 provinces of South China, and discusses their main characteristics in 4 aspects, the uranium productive granite is highly developed in fracture, very strong in alteration, often occurred as two-mica granite and regularly developed with intermediate-basic and acid dikes. The above characteristics distinguish the uranium productive granite from the uranium rich granite. (authors)

  2. 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

  3. 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

  4. 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.

  5. EXPLOITATION OF GRANITE BOULDER

    Directory of Open Access Journals (Sweden)

    Ivan Cotman

    1994-12-01

    Full Text Available The processes of forming, petrography, features, properties and exploitation of granite boulders are described. The directional drilling and black powder blasting is the succesful method in exploitation of granite boulders (boulder technology (the paper is published in Croatian.

  6. Effect of Bacillus subtilis on Granite Weathering: A Laboratory Experiment

    Science.gov (United States)

    Song, W.; Ogawa, N.; Oguchi, C. T.; Hatta, T.; Matsukura, Y.

    2006-12-01

    We performed a comparative experiment to investigate how the ubiquitous soil bacterium Bacillus subtilis weathers granite and which granite-forming minerals weather more rapidly via biological processes. Batch type experiments (granite specimen in a 500 ml solution including NaCl, glucose, yeast extract and bacteria Bacillus subtilis at 27°E C) were carried out for 30 days. Granite surfaces were observed by SEM before and after the experiment. Bacillus subtilis had a strong influence on granite weathering by forming pits. There were 2.4 times as many pits and micropores were 2.3 times wider in granite exposed to Bacillus subtilis when compared with bacteria-free samples. Bacillus subtilis appear to preferentially select an optimum place to adhere to the mineral and dissolve essential elements from the mineral to live. Plagioclase was more vulnerable to bacterial weathering than biotite among the granite composing minerals.

  7. 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

  8. Mechanical properties of Stripa granite

    International Nuclear Information System (INIS)

    Stephansson, O.; Swan, G.; Leijon, B.

    1978-01-01

    For the determination of the mechanical properties of Stripa Granite samples were taken from the boreholes in the vicinity of the test site. The granite type taken from these different sources is of variable character. For the purpose of numerical calculations performed in projects related to the waste storage research program the following parameters have been determined: Young's modulus, Poisson's ratio, compressive fracture stress and expansion coefficient as a function of temperature 20< T<200C; Young's modulus and compressive fracture stress as a function of confining pressure; Brazilian tensile fracture stress; residual shear stress as a function of normal stress; anisotropy ratio for Young's modulus and compressive fracture stress; dilatational wave velocity and deduced dynamic Young's modulus. A brief description of the test methods and the results for each test are presented

  9. A study of uranium series disequilibrium in core profiles and mineral separates from the samples of Lac du Bonnet granite from the URL site, Pinawa, Manitoba, Canada

    International Nuclear Information System (INIS)

    Ivanovich, M.; Longworth, G.; Wilkins, M.A.; Hasler, S.E.

    1987-12-01

    Uranium series disequilibrium measurements of actinide activities and activity ratios have been used to study the geochemical history of Lac du Bonnet granite, from the URL site, Pinawa, Canada. Measurements on core profiles between fractured surfaces and the parent rock show that the granite underwent high temperature events several million years ago, followed by more recent low temperature events within the last million years. The main locations for the rock/water interaction and exchange of actinides are the fracture surfaces. The results of similar measurements on separated mineral phases show that the 'soft' minerals such as biotite and feldspar are more vulnerable to weathering than the 'hard' accessory minerals such as zircon. (author)

  10. Radon exhalation from granitic rocks

    Energy Technology Data Exchange (ETDEWEB)

    Del Claro, Flávia; Paschuk, Sergei A.; Corrêa, Janine N.; Mazer, Wellington; Narloch, Danielle Cristine; Martin, Aline Cristina [Universidade Tecnológica Federal do Paraná (UTFPR), Curitiba, PR (Brazil); Denyak, Valeriy, E-mail: flaviadelclaro@gmail.com, E-mail: spaschuk@gmail.com, E-mail: janine_nicolosi@hotmail.com, E-mail: denyak@gmail.com [Instituto de Pesquisa Pelé Pequeno Príncipe (IPPP), Curitiba, PR (Brazil)

    2017-07-01

    Naturally occurring radionuclides such as radon ({sup 222}Rn), its decay products and other elements from the radioactive series of uranium ({sup 238}U and {sup 235}U) and thorium ({sup 232}Th) are an important source of human exposure to natural radioactivity. The worldwide evaluation of health radiobiological effects and risks from population exposure to natural radionuclides is a growing concern. About 50% of personal radiation annual dose is related to radionuclides such as radon ({sup 222}Rn), thoron ({sup 220}Rn), radium ({sup 226}Ra), thorium ({sup 232}Th) and potassium ({sup 40}K), which are present in modern materials commonly used in construction of dwellings and buildings. The radioactivity of marbles and granites is of big concern since under certain conditions the radioactivity levels of these materials can be hazardous to the population and require the implementation of mitigation procedures. Present survey of the {sup 222}Rn and {sup 220}Rn activity concentration liberated in the air was performed using commercialized Brazilian granite rocks at national market as well as exported to other countries. The {sup 222}Rn and {sup 220}Rn measurements were performed using the AlphaGUARD instant monitor and RAD7 detector, respectively. This study was performed at the Applied Nuclear Physics Laboratory of the Federal University of Technology – Paraná (UTFPR). Obtained results of radon concentration activity in air exhaled studied samples of granites varied from 3±1 Bq/m{sup 3} to 2087±19 Bq/m{sup 3}, which shows that some samples of granitic rocks represent rather elevated health risk the population. (author)

  11. The instrumental neutron-activation analysis of granites from the Bushveld Complex

    International Nuclear Information System (INIS)

    Watterson, J.I.W.

    1978-01-01

    Three methods of instrumental neutron-activation analysis, 14MeV, reactor thermal, and reactor epithermal, are compared for the analysis of granites form the Bushveld Complex. A total of 34 elements can be determined in the granites by these methods. Samples from the Zaaiplaats area were analysed by thermal neutron activation, and 22 elements were determined in all of them. These elements were used to distinguish between the mineralized Bobbejaankop and Lease granites and the Main granite by the use of multivariate statistics. The Bobbejaankop granite appears as a more-differentaited rock carrying greater amounts of the incompatible elements than does the Main granite [af

  12. Geology of Muntok area and the potency of menumbang granite as source of Uranium and Thorium

    International Nuclear Information System (INIS)

    Kurniawan Dwi Saksama; Ngadenin

    2013-01-01

    In the West Bangka there are some granites namely Menumbing, Pelangas, Tempilang, and Jebus granite. The granites is granite tin belt that stretches from Thailand-Malaysia-Bangka Belitung. Granite tin belt or granite source of tin (cassiterite) can act as a source of U and Th. Aims of the study is to find out the information on the geology of Muntok area and its surrounding and to determine the potency of Menumbing granite as a source of U and Th. The methods used is surface geological mapping in Muntok areas and its surrounding with scale 1 : 25.000, measurement grade of uranium and thorium in Menumbing granite areas and petrographic and grain size analysis of sample of Menumbing granite. Determination of granites a source of U and Th is based on content of radioactive mineral, anomaly of U and Th, megascopic and microscopic observation of granite. Morphology of Muntok areas and its surrounding is denudasional undulating plains to hills with an elevation ranging from 0 to 455 meters. Stratigraphy of research areas from old to young is meta sandstone units, granite intrusion of Menumbing and alluvial. Evolving fault is a fault trending West-East. Based on the presence of radioactive minerals, grade of U and Th as well as the type of granite, it was concluded that the Menumbing granite is a source of Th and not sources of U. (author)

  13. Granit, Prof. Ragnar Arthur

    Indian Academy of Sciences (India)

    Home; Fellowship. Fellow Profile. Elected: 1964 Honorary. Granit, Prof. Ragnar Arthur Nobel Laureate (Medicine) - 1967. Date of birth: 30 October 1900. Date of death: 11 March 1991. YouTube; Twitter; Facebook; Blog. Academy News. IAS Logo. 29th Mid-year meeting. Posted on 19 January 2018. The 29th Mid-year ...

  14. Inittial survey of natural radioactivity level in granite resource in hami and tuoli of Xinjiang

    International Nuclear Information System (INIS)

    Zhao Qiwen; Liu E; Di Shaobin; Zhang Zhanjiang

    2009-01-01

    This paper reports the measurement methods and results of natural radioactivity level in large-sized granite stone factories in Hami and Tuoli in Xinjiang Autonomous Region, such as mine pit, materials, finished productions and waste pile. Surface gamma exposure rate of materials and products, radon concentration, as well as specific activity of natural radionuclides in solid samples and process wastewater are detected, and for part of building materials, gamma radiation dose rate in buildings is also measured. It is concluded that the results of measurement fall in the range of the local background except for 20%-25% granite samples in excess of the level specified by National Environmental Protection Agency with respect to gamma radiation dose rate. (authors)

  15. PREVALENCE OF METABOLIC SYNDROME IN GRANITE WORKERS

    Directory of Open Access Journals (Sweden)

    Srilakshmi

    2015-10-01

    Full Text Available BACKGROUND: The prevalence of the metabolic syndrome (MS has significantly increased over the last few decades and has become a main health challenge worldwide. Prevalence of MS is quickly rising in developing countries due to changing lifestyle. It was considered worthwhile to study MS and its components in granite workers since granite factories are situated in and around Khammam area. Moreover, no studies of MS in granite workers have been reported in literature. OBJECTIVES: Aim of our study is to assess the prevalence of metabolic syndrome and its components in granite workers. MATERIALS AND METHODS: 210 male workers in the age group of 20 - 50 working in granite industries located in and around the Khammam town of Telangana State are selected for the present study. Blood pressures (BP, waist circumference (WC were measured. Fasting blood samples were collected for the estimation of glucose and lipids. RESULTS: 69 subjects out of 210 were identified as having MS based on updated National cholesterol education programme - Adult Treatment Panel III (NCEP - ATP III guidelines. CONCLUSION: MS should be identified and remedial measures may be suggested, so that the risk of hypertension, cardiovascular risk, diabetes and the resultant morbidity is minimized and can be delayed

  16. Adsorption behavior of Am(III) on granite

    International Nuclear Information System (INIS)

    Zhang Yingjie; Feng Xiaogui; Liang Junfu; Chen Jing; Su Rui; Wang Ju; Liu Chunli

    2009-01-01

    The adsorption behavior of Am(III) on granite (sampled from drilling well BS01 at Beishan (BS) area--a potential candidate site for China's high-level radioactive waste repository, the granite sample's depth about 300 m) was studied in BS03 well groundwater by a batch technique at (25±1) degree C. The influences of pH, sulphate ion, total carbonate ion, humic acid, and concentration of the Am(III) on the adsorption behavior were also studied, and the possible adsorption mechanism was discussed. Experimental results show that the adsorption distribution rate of Am(III) on granite increases with increasing pH of aqueous phase. The chemical composition of the groundwater is the main factor which influences the species of Am(III) and adsorption behavior. The adsorption mechanism of Am(III) on granite is surface complexation. The adsorption isotherm of Am(III) on granite can be described by Freundlich's equation. (authors)

  17. 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

  18. Processing and finishing of granite surfaces

    OpenAIRE

    Klich, J. (Jiří); Hlaváček, P. (Petr); Ščučka, J. (Jiří); Sitek, L. (Libor); Foldyna, J. (Josef); Georgiovská, L. (Lucie); Souček, K. (Kamil); Staš, L. (Lubomír); Bortolussi, A.

    2013-01-01

    The article deals with granite surface processing and finishing by various methods including bush hammering, flaming, polishing, continuous and pulsating water jetting. Both optical and CT X-ray methods are used for analysis of surface and subsurface areas of tested samples. Advantages of pulsating water jetting compared to other techniques are discussed.

  19. 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.)

  20. 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...

  1. A Rb-Sr isotope study of a young granite sheet at Marble Delta, southern Natal

    International Nuclear Information System (INIS)

    Naidoo, D.D.; Eglington, B.M.; Harmer, R.E.

    1989-01-01

    Rb-Sr isotope data are presented for two apophyses of a granite sheet intrusive into marble at Marble Delta, southern Natal. Granite samples collected near the margins of these apophyses contain calcite and are thought to have been contaminated by the marble during intrusion of the granite magma. In contrast, those further away from contacts lack calcite. The 'uncontaminated' granite samples define an isochron date of 899 ± 11 Ma. This data is thought to represent the intrusive age of the granite sheet. 11 refs., 5 figs., 2 tabs

  2. Hydrothermal alteration of Hercynian granites, its significance to the evolution of geothermal systems in granitic rocks

    Energy Technology Data Exchange (ETDEWEB)

    Marques, Jose M.; Matias, Maria J.; Basto, Maria J.; Aires-Barros, Luis A. [Instituto Superior Tecnico, Centro de Petrologia e Geoquimica, Universidade Tecnica de Lisboa, Av. Rovisco Pais, 1049-001 Lisbon (Portugal); Carreira, Paula M. [Instituto Tecnologico e Nuclear, Estrada Nacional n 10, 2686 - 953 Sacavem (Portugal); Goff, Fraser E. [Earth and Planetary Sciences Department, Univ. of New Mexico, Albuquerque, NM 87131 (United States)

    2010-06-15

    We discuss geochemical and isotopic ({sup 18}O/{sup 16}O, {sup 2}H/{sup 1}H and {sup 87}Sr/{sup 86}Sr) data recording the hydrothermal alteration of northern Portuguese Hercynian granites by Na-HCO{sub 3}-CO{sub 2}-rich mineral waters. Whole-rock samples from drill cores of Vilarelho da Raia granite have {delta}{sup 18}O values in the +11.47 to +10.10 permille range. The lower values correspond to highly fractured granite samples displaying vein and pervasive alteration. In the pervasive alteration stage, which probably results from a convective hydrothermal system set up by the intrusion of the granites, the metamorphic waters are in equilibrium with hydrous minerals. In contrast, the vein alteration of these granitic rocks was caused by water of meteoric origin. The oxygen ratios between water (W) and rock (R), the so-called W/R ratios, obtained for the open system (where the heated water is lost from the system by escape to the surface) range between 0.05 and 0.11, suggesting that the recrystallization of the veins was influenced by a small flux of meteoric water. Stable isotope analyses performed on the cores show that the vein alteration stage relates to post-emplacement tectonic stresses acting on the granite, probably of late Hercynian age. Our results are consistent with the existence of two separate alteration events (pervasive and vein) caused by hydrothermal waters of different isotopic characteristics. The studies presented in this paper should be viewed as a natural analogue that uses the alteration features observed in a fossil geothermal system at Vilarelho da Raia to assess possible water-rock reactions presently occurring at depth in granitic rocks of the nearby Chaves area. (author)

  3. 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...

  4. Protocol proposal for radon concentration mensuration from granitic rocks in marble factory

    International Nuclear Information System (INIS)

    Del Claro, Flavia

    2016-01-01

    Naturally occurring radionuclides such as radon ( 222 Rn), its decay products and other elements from the radioactive series of uranium ( 238 U and 235 U) and thorium ( 232 Th) are an important source of human exposure to natural radioactivity. The worldwide evaluation of health radiobiological effects and risks from population exposure to natural radionuclides is a growing concern. Radionuclides such as radon ( 222 Rn), the thoron ( 220 Rn), radio ( 2 '2'6Ra), thorium ( 23 '2Th) and potassium ( 40 K) may occur in materials commonly used in construction of dwellings and buildings. Thus, the radioactivity from marbles and granites is of importance, so that under certain conditions these materials radioactivity levels can be hazardous requiring the implementation of mitigation measurements. This research presents a technical protocol marble factories for the control human exposure to natural radioactivity exhaled from granitic rocks. The protocol was based on measurements of the 222 Rn and 220 Rn concentration in Brazilian granite rocks commonly nationally and exported. The 222 Rn and 220 Rn measurements were done using the AlphaGUARD (Saphymo GmbH) and RAD7 (Durridge Company) apparatus, respectively. The samples of granite were sealed in glass jars for 40 days in to achieve secular equilibrium between 226 Ra and 222 Rn radionuclides. The measurements were performed on Applied Nuclear Physics Laboratory at the Federal Technological University of Parana. Also, solid-state nuclear track detectors CR-39 were installed in a marble factory environments located in Curitiba - Parana for the evaluation of 222 Rn concentrations in workplaces. The CR-39 detectors were exposed for about 90 days and submitted to etching process. The alpha particle tracks were observed using an optical microscope. Some granite samples analyzed presented 222 Rn concentrations of attention, since the average values ranged from 3 ± 1 Bq/m 3 to 2087 ± 19 Bq/m 3 . The results obtained

  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. 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

  7. Determination of uranium concentrations and "2"3"4U/"2"3"8U activity ratio in some granitic rock samples by alpha spectrometry: application of a radiochemical procedure

    International Nuclear Information System (INIS)

    Khattab, Mahmoud R.

    2016-01-01

    The present study is an application of a radiochemical procedure using alpha spectrometry technique for determination of uranium isotopes "2"3"8U, "2"3"4U and "2"3"5U on 13 granitic samples. These samples were collected from Gabal Gattar area, Northeastern Desert, Egypt. The collected samples were digested using microwave technique with aqua regia and spiked with "2"3"2U for chemical yield and activity calculation. Separation of uranium isotopes from the samples was done by Dowex 1 x 4 (50-100 mesh) resin followed by source preparation using microprecipitation technique. The concentrations of "2"3"8U were ranged between 28.9±0.9 and 134.8±1.8 Bq/g, and the "2"3"4U concentrations were between 24±0.6 and 147.7±2.2 Bq/g. For the "2"3"5U, the activity concentrations were between 1.3±0.2 and 6.7±1.2 Bq/g. The activity ratio of "2"3"4U/"2"3"8U was calculated and varied from 0.80 to 1.30. (author)

  8. Mechanical properties of granitic rocks from Gideaa, Sweden

    International Nuclear Information System (INIS)

    Ljunggren, C.; Stephansson, O.; Alm, O.; Hakami, H.; Mattila, U.

    1985-10-01

    The elastic and mechanical properties were determined for two rock types from the Gideaa study area. Gideaa is located approximately 30 km north-east of Oernskoeldsvik, Northern Sweden. The rock types that were tested were migmatitic gneiss and migmatitic granite. The following tests were conducted: - sound velocity measurements; - uniaxial compression tests with acoustic emission recording; - brazilian disc tests; - triaxial tests; - three point bending tests. All together, 12 rock samples were tested with each test method. Six samples of these were migmatic gneiss and six samples were migmatitic granite. The result shows that the migmatitic gneiss has varying strength properties with low compressive strength in comparison with its high tensile strength. The migmatitic granite, on the other hand, is found to have parameter values similar to other granitic rocks. With 15 refs. (Author)

  9. 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.

  10. Automated tone grading of granite

    International Nuclear Information System (INIS)

    Catalina Hernández, J.C.; Fernández Ramón, G.

    2017-01-01

    The production of a natural stone processing plant is subject to the intrinsic variability of the stone blocks that constitute its raw material, which may cause problems of lack of uniformity in the visual appearance of the produced material that often triggers complaints from customers. The best way to tackle this problem is to classify the product according to its visual features, which is traditionally done by hand: an operator observes each and every piece that comes out of the production line and assigns it to the closest match among a number of predefined classes, taking into account visual features of the material such as colour, texture, grain, veins, etc. However, this manual procedure presents significant consistency problems, due to the inherent subjectivity of the classification performed by each operator, and the errors caused by their progressive fatigue. Attempts to employ automated sorting systems like the ones used in the ceramic tile industry have not been successful, as natural stone presents much higher variability than ceramic tiles. Therefore, it has been necessary to develop classification systems specifically designed for the treatment of the visual parameters that distinguish the different types of natural stone. This paper describes the details of a computer vision system developed by AITEMIN for the automatic classification of granite pieces according to their tone, which provides an integral solution to tone grading problems in the granite processing and marketing industry. The system has been designed to be easily trained by the end user, through the learning of the samples established as tone patterns by the user. [es

  11. Heat production in granitic rocks

    DEFF Research Database (Denmark)

    Artemieva, Irina; Thybo, Hans; Jakobsen, Kiki

    2017-01-01

    Granitic rocks play special role in the dynamics and evolution of the Earth and its thermal regime. First, their compositional variability, reflected in the distribution of concentrations of radiogenic elements, provides constraints on global differentiation processes and large scale planetary...... evolution, where emplacement of granites is considered a particularly important process for the formation of continental crust. Second, heat production by radioactive decay is among the main heat sources in the Earth. Therefore knowledge of heat production in granitic rocks is pivotal for thermal modelling...... of the continental lithosphere, given that most radiogenic elements are concentrated in granitic rocks of the upper continental crust whereas heat production in rocks of the lower crust and lithospheric mantle is negligible. We present and analyze a new global database GRANITE2017 (with about 500 entries...

  12. Granitic rocks from the southern Gyeongsang basin, southeastern Korea, (1)

    International Nuclear Information System (INIS)

    Lee, Yoon-Jong

    1980-01-01

    In southern Gyeongsang basin, southeastern Korea, there are many granitic rock masses. They were divided into 7 groups according to their geological evidences. K-Ar age was determined on 36 samples obtained from the respective groups. Group A: pre-Gyeongsang granitic rock (Pre-Cretaceous), A 1 220 m.y., A 2 166 m.y.; group B: outer zone granitic rock (Cretaceous), 115-72 m.y.; group C: ditto (ditto), 97-70 m.y.; group D: ditto (ditto), 89-68 m.y.; group E: ditto (ditto), 82-68 m.y.; group F: inner zone granitic rock (Cretaceous), 75-74 m.y.; group G: Tertiary granitic rock, 63-41 m.y. The large part of the Cretaceous granitic masses show the double elongated ring form. Most of the Tertiary granitic rocks were probably emplaced in close relation with the Eonyang fault line and Ulsan fault line/or their extension line of the area. (J.P.N.)

  13. 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)

  14. Geochemical reanalysis of historical U.S. Geological Survey sediment samples from the Inmachuk, Kugruk, Kiwalik, and Koyuk River drainages, Granite Mountain, and the northern Darby Mountains, Bendeleben, Candle, Kotzebue, and Solomon quadrangles, Alaska

    Science.gov (United States)

    Werdon, Melanie B.; Granitto, Matthew; Azain, Jaime S.

    2015-01-01

    The State of Alaska’s Strategic and Critical Minerals (SCM) Assessment project, a State-funded Capital Improvement Project (CIP), is designed to evaluate Alaska’s statewide potential for SCM resources. The SCM Assessment is being implemented by the Alaska Division of Geological & Geophysical Surveys (DGGS), and involves obtaining new airborne-geophysical, geological, and geochemical data. As part of the SCM Assessment, thousands of historical geochemical samples from DGGS, U.S. Geological Survey (USGS), and U.S. Bureau of Mines archives are being reanalyzed by DGGS using modern, quantitative, geochemical-analytical methods. The objective is to update the statewide geochemical database to more clearly identify areas in Alaska with SCM potential. The USGS is also undertaking SCM-related geologic studies in Alaska through the federally funded Alaska Critical Minerals cooperative project. DGGS and USGS share the goal of evaluating Alaska’s strategic and critical minerals potential and together created a Letter of Agreement (signed December 2012) and a supplementary Technical Assistance Agreement (#14CMTAA143458) to facilitate the two agencies’ cooperative work. Under these agreements, DGGS contracted the USGS in Denver to reanalyze historical USGS sediment samples from Alaska. For this report, DGGS funded reanalysis of 653 historical USGS sediment samples from the statewide Alaska Geochemical Database Version 2.0 (AGDB2; Granitto and others, 2013). Samples were chosen from an area covering portions of the Inmachuk, Kugruk, Kiwalik, and Koyuk river drainages, Granite Mountain, and the northern Darby Mountains, located in the Bendeleben, Candle, Kotzebue, and Solomon quadrangles of eastern Seward Peninsula, Alaska (fig. 1). The USGS was responsible for sample retrieval from the National Geochemical Sample Archive (NGSA) in Denver, Colorado through the final quality assurance/quality control (QA/QC) of the geochemical analyses obtained through the USGS contract

  15. 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)

  16. 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.

  17. Climax granite test results

    Energy Technology Data Exchange (ETDEWEB)

    Ramspott, L.D.

    1980-01-15

    The Lawrence Livermore Laboratory (LLL), as part of the Nevada Nuclear Waste Storage Investigations (NNWSI) program, is carrying out in situ rock mechanics testing in the Climax granitic stock at the Nevada Test Site (NTS). This summary addresses only those field data taken to date that address thermomechanical modeling for a hard-rock repository. The results to be discussed include thermal measurements in a heater test that was conducted from October 1977 through July 1978, and stress and displacement measurements made during and after excavation of the canister storage drift for the Spent Fuel Test (SFT) in the Climax granite. Associated laboratory and field measurements are summarized. The rock temperature for a given applied heat load at a point in time and space can be adequately modeled with simple analytic calculations involving superposition and integration of numerous point source solutions. The input, for locations beyond about a meter from the source, can be a constant thermal conductivity and diffusivity. The value of thermal conductivity required to match the field data is as much as 25% different from laboratory-measured values. Therefore, unless we come to understand the mechanisms for this difference, a simple in situ test will be required to obtain a value for final repository design. Some sensitivity calculations have shown that the temperature field is about ten times more sensitive to conductivity than to diffusivity under the test conditions. The orthogonal array was designed to detect anisotropy. After considering all error sources, anisotropic efforts in the thermal field were less than 5 to 10%.

  18. 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.

  19. Application of specific extraction chromatographic methods to the Rb-Sr, Sm-Nd isotope study of geological samples: The Hombreiro-Santa Eulalia Granite (Lugo, NW Spain)

    OpenAIRE

    Santos Zalduegui, J. F.; Pin, C.; Aranguren, A.; Gil Ibarguchi, José Ignacio

    1996-01-01

    The analytical application to geological samples of three new chromatographic resins, TRU-Spec ®, Sr-Spec ® and LN-Spec ®) has been investigated. Seven samples of the Hombreiro massif (Lugo, NW Spain) have been studied, that yield a Rb-Sr age of 298 ±5 Ma (SrQ = 0.7086, MSWD = 7.64) for the magma crystallization. Sm-Nd data results for the same massif give eNd values dose to -2 at 300 Ma. This suggests that the origin of the magma might be related to the partial melting of immature sediments,...

  20. S-type granite generation and emplacement during a regional switch from extensional to contractional deformation (Central Iberian Zone, Iberian autochthonous domain, Variscan Orogeny)

    Science.gov (United States)

    Pereira, M. F.; Díez Fernández, R.; Gama, C.; Hofmann, M.; Gärtner, A.; Linnemann, U.

    2018-01-01

    Zircon grains extracted from S-type granites of the Mêda-Escalhão-Penedono Massif (Central Iberian Zone, Variscan Orogen) constrain the timing of emplacement and provide information about potential magma sources. Simple and composite zircon grains from three samples of S-type granite were analyzed by LA-ICP-MS. New U-Pb data indicate that granites crystallized in the Bashkirian (318.7 ± 4.8 Ma) overlapping the proposed age range of ca. 321-317 Ma of the nearby S-type granitic rocks of the Carrazeda de Anciães, Lamego and Ucanha-Vilar massifs. The timing of emplacement of such S-type granites seems to coincide with the waning stages of activity of a D2 extensional shear zone (i.e. Pinhel shear zone) developed in metamorphic conditions that reached partial melting and anatexis (ca. 321-317 Ma). Dykes of two-mica granites (resembling diatexite migmatite) are concordant and discordant to the compositional layering and S2 (main) foliation of the high-grade metamorphic rocks of the Pinhel shear zone. Much of the planar fabric in these dykes was formed during magmatic crystallization and subsequent solid-state deformation. Field relationships suggest contemporaneity between the ca. 319-317 Ma old magmatism of the study area and the switch from late D2 extensional deformation to early D3 contractional deformation. Inherited zircon cores are well preserved in these late D2-early D3 S-type granite plutons. U-Pb ages of inherited zircon cores range from ca. 2576 to ca. 421 Ma. The spectra of inherited cores overlap closely the range of detrital and magmatic zircon grains displayed by the Ediacaran to Silurian metasedimentary and metaigneous rocks of the Iberian autochthonous and parautochthonous domains. This is evidence of a genetic relationship between S-type granites and the host metamorphic rocks. There is no substantial evidence for the addition of mantle-derived material in the genesis of these late D2-early D3 S-type granitic rocks. The ɛNd arrays of heterogeneous

  1. 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

  2. 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.

  3. Uranium enriched granites in Sweden

    International Nuclear Information System (INIS)

    Wilson, M.R.; Aakerblom, G.

    1980-01-01

    Granites with uranium contents higher than normal occur in a variety of geological settings in the Swedish Precambrian, and represent a variety of granite types and ages. They may have been generated by (1) the anatexis of continental crust (2) processes occurring at a much greater depth. They commonly show enrichement in F, Sn, W and/or Mo. Only in one case is an important uranium mineralization thought to be directly related to a uranium-enriched granite, while the majority of epigenetic uranium mineralizations with economic potential are related to hydrothermal processes in areas where the bedrock is regionally uranium-enhanced. (Authors)

  4. Granites and granitoids of the southern region - Granite molybdenite system

    International Nuclear Information System (INIS)

    Issler, R.S.

    1987-01-01

    Economic concentrations of molybdenum are genetically closely associated with acidic and moderately acid granitoids-granites, granodiorites, monzonites and diorites, and are located in two geotectonic settings: subduction-related and rift-related. The aim of this paper is twofold, first succinctly approach the geology, tectonic setting and chemical parameters of the 'granite molybdenite system' as defined by Mutschler and/or alcali granite porphyry bodies emplaced in the North American continent for occasion of a Mesozoic-Fanerozoic extensile event; second to relate the computer-assisted evaluation of 422 major element chemical analysis of granites and granitoids of southern region of Brazil, using chemical fingerprints (SiO 2 ≥ 74. Owt%, Na 2 O ≤ 3.6wt%, K 2 O ≥ 4.5wt%), and K 2 O/Na 2 O ratio > 1.5 developed and testified from North American and Finnish occurrences, may locate molybdenite-bearing granite bodies with high exploration potential. These techniques suggest that some late Precambrian to early Paleozoic granite-rhyolite assemblages inserted at domains of the SG. 22/23 Curitiba/Iguape, SH. 21/22 Uruguaiana/Porto Alegre and SI.22 Lagoa Mirim Sheets, have exploration potential for molybdenum. (author) [pt

  5. 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)

  6. Artificial weathering of granite

    Directory of Open Access Journals (Sweden)

    Silva Hermo, B.

    2008-06-01

    Full Text Available This article summarizes a series of artificial weathering tests run on granite designed to: simulate the action of weathering agents on buildings and identify the underlying mechanisms, determine the salt resistance of different types of rock; evaluate consolidation and water-repellent treatment durability; and confirm hypotheses about the origin of salts such as gypsum that are often found in granite buildings. Salt crystallization tests were also conducted, using sodium chloride, sodium sulphate, calcium sulphate and seawater solutions. One of these tests was conducted in a chamber specifically designed to simulate salt spray weathering and another in an SO2 chamber to ascertain whether granite is subject to sulphation. The test results are analyzed and discussed, along with the shortcomings of each type of trial as a method for simulating the decay observed in monuments. The effect of factors such as wet-dry conditions, type of saline solution and the position of the planes of weakness on the type of decay is also addressed.En este trabajo se hace una síntesis de varios ensayos de alteración artificial realizados con rocas graníticas. Estos ensayos tenían distintos objetivos: reproducir las formas de alteración encontradas en los edificios para llegar a conocer los mecanismos que las generan, determinar la resistencia de las diferentes rocas a la acción de las sales, evaluar la durabilidad de tratamientos de consolidación e hidrofugación y constatar hipótesis acerca del origen de algunas sales, como el yeso, que aparecen frecuentemente en edificios graníticos. En los ensayos de cristalización de sales se utilizaron disoluciones de cloruro de sodio, sulfato de sodio, sulfato de calcio y agua de mar. Uno de estos ensayos se llevó a cabo en una cámara especialmente diseñada para reproducir la alteración por aerosol marino y otro se realizó en una cámara de SO2, con el objeto de comprobar si en rocas graníticas se puede producir

  7. 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)

  8. Assessment of natural radioactivity in commercial marble and granite of Espirito Santo state

    International Nuclear Information System (INIS)

    Aquino, Reginaldo Ribeiro de

    2015-01-01

    In this work, the concentrations of natural radionuclides 226 Ra, 232 Th and 40 K in granite and marble samples were determined, considering the main extraction mining of Espirito Santo state, southeastern Brazil. For all study sites, three samples were sealed in 100 ml high density polyethylene bottles. Each sample rested for 4 weeks to reach the secular equilibrium of 238 U and 232 Th series before measured by high resolution gamma spectrometry, and the acquired spectra were analyzed with the software WinnerGamma. The self-absorption correction was considered for all samples, using an expression and method specially developed for this purpose. The concentration of 226 Ra was determined by the weighted arithmetic mean of the concentrations of 214 Pb and 214 Bi, the concentration of 232 Th by the weighted arithmetic mean of the concentrations of 228 Ac, 212 Pb and 212 Bi and the concentration of 40 K by its single 1460 keV transition. The radium equivalent and gamma index were calculated from the activity concentrations of 226 Ra, 232 Th, and 40 K. The emanated radon was measured using an exhalation chamber and the passive detector technique, with a solid state nuclear tracks detectors (SSNTD) being exposed in NRPB/SSI-H dosimeters. During exposure, a commercial detector CR-39® and a national plastic called Durolon® were used, the last was characterized for this purpose using a technique called double exposure and sensitivity intrinsic factor. The characterized plastic was efficient for the application and the calibration factor corresponded to 1.60 ± 0.10 tracks.cm².(kBq.m -3 day) -1 in relation to the CR-39 factor, equivalent to 2.8 ± 0.2 tracks.cm².(kBq.m -3 .day) -1 . The detector showed a higher efficiency at a higher dose. The activities determined by passive detection varyed from 100 ± 10 Bq.m -3 up to 2400 ± 300 Bq.m -3 , highlighting the biggest exhalation rates for granite Ibere Mombasa. Considering the marbles, activity values varyed from 80

  9. 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.

  10. 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

  11. 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

  12. 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

  13. Stability of cubic zirconia in a granitic system under high pressure and temperature

    International Nuclear Information System (INIS)

    Gibb, F. G. F.; Burakov, B. E.; Taylor, K. J.; Domracheva, Y.

    2008-01-01

    Cubic zirconia is a well known, highly durable material with potential uses as an actinide host phase in ceramic waste forms and inert matrix fuels and in containers for very deep borehole disposal of some highly radioactive wastes. To investigate the behaviour of this material under the conditions of possible use, a cube of ∼2.5 mm edge was made from a single crystal of Yttria stabilized cubic zirconia doped with 0.3 wt.% CeO 2 . The cube was enclosed in powdered granite within a gold capsule and a small amount of H 2 O added before sealing. The sealed capsule was held for 4 months in a cold-seal pressure vessel at a temperature of 780 deg. C and a pressure 150 MPa, simulating both the conditions of a deep borehole disposal involving partial melting of the host rock and the conditions under which the actinide waste form might be encapsulated in granite prior to disposal. At the end of the experiment the quenched, largely glassy, sample was cut into thin slices and studied by optical microscopy, EMPA, SEM and cathodoluminescence methods. The results show that no corrosion of the zirconia crystal or reaction with the granite melt occurred and that no detectable diffusion of elements, including Ce, in or out of the zirconia took place on the timescale of the experiment. Consequently, it appears that cubic zirconia could perform most satisfactorily as both an actinide host waste form for encapsulation in solid granite for very deep disposal and as a container material for deep borehole disposal of highly radioactive wastes (HLW), including spent fuel. (authors)

  14. Sorption of actinides in granitic rock

    International Nuclear Information System (INIS)

    Allard, B

    1982-11-01

    The sorption of americium (III), neptunium(V) and plutonium on geologic media under oxic conditions has been measured by a batch technique. The aqueous phase was a synthetic groundwater or 4M NaCl solution. The solid phase was a pure mineral, representative of igneous rocks, or granite. Altogether 40 different minerals and rocks were used. The effects of pH and the ionic strength of the aqueous phase as well as of the cation exchange capacity and the surface/mass ratio of the solid sorbent are discussed. Empirical equations giving the distribution coefficient as a function of pH in the environmental pH-range 7-9 are suggested. Some observations and conclusions concerning sorption mechanisms are given. (author)

  15. 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)

  16. 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.

  17. 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.

  18. Movement of fossil pore fluids in granite basement, Illinois

    International Nuclear Information System (INIS)

    Couture, R.A.; Seitz, M.G.

    1986-01-01

    The compositions of pore fluids in granite cores from the Precambrian basement in northern Illinois were determined. The estimated chloride concentration in the aqueous phase increases from near zero at the upper contact with sandstone to 2.7 M at 624 m below the contact. Traces of aliphatic oil are present in the overlying sandstone and the upper 516 m of granite, and oil occupies most of the pore space in one sample of unaltered granite 176 m below the contact. The oil has a Δ 13 C of -25%, about the same as average petroleum. The high concentrations of salt more than 500 m below the contact imply that little or no fresh water has reached these levels of the granite by flow. Lower concentrations near the contact are consistent with replacement of brine in the sandstone by fresh water at least 11 m.y. ago and subsequent upward diffusion of salt from the granite. Geologic data suggest that the time of replacement was about 130 Ma. The purpose of the investigation is to study the record of movement of intergranular fluids within a granite pluton. The composition and movement of ground waters can determine the extent that hazardous or radioactive wastes disposed in igneous rock will remain isolated

  19. 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....

  20. 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

  1. 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

  2. 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

  3. Uranium deposits in granitic rocks

    International Nuclear Information System (INIS)

    Nishimori, R.K.; Ragland, P.C.; Rogers, J.J.W.; Greenberg, J.K.

    1977-01-01

    This report is a review of published data bearing on the geology and origin of uranium deposits in granitic, pegmatitic and migmatitic rocks with the aim of assisting in the development of predictive criteria for the search for similar deposits in the U.S. Efforts were concentrated on the so-called ''porphyry'' uranium deposits. Two types of uranium deposits are primarily considered: deposits in pegmatites and alaskites in gneiss terrains, and disseminations of uranium in high-level granites. In Chapter 1 of this report, the general data on the distribution of uranium in igneous and metamorphic rocks are reviewed. Chapter 2 contains some comments on the classification of uranium deposits associated with igneous rocks and a summary of the main features of the geology of uranium deposits in granites. General concepts of the behavior of uranium in granites during crustal evolution are reviewed in Chapter 3. Also included is a discussion of the relationship of uranium mineralization in granites to the general evolution of mobile belts, plus the influence of magmatic and post-magmatic processes on the distribution of uranium in igneous rocks and related ore deposits. Chapter 4 relates the results of experimental studies on the crystallization of granites to some of the geologic features of uranium deposits in pegmatites and alaskites in high-grade metamorphic terrains. Potential or favorable areas for igneous uranium deposits in the U.S.A. are delineated in Chapter 5. Data on the geology of specific uranium deposits in granitic rocks are contained in Appendix 1. A compilation of igneous rock formations containing greater than 10 ppM uranium is included in Appendix 2. Appendix 3 is a report on the results of a visit to the Roessing area. Appendix 4 is a report on a field excursion to eastern Canada

  4. 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...

  5. 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

  6. 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

  7. 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.

  8. 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.

  9. 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...

  10. 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.

  11. Geochemistry of mylonitic tourmaline-bearing granite- gneiss pluton in the northeast of June mine

    Directory of Open Access Journals (Sweden)

    Arezoo Moradi

    2017-07-01

    , allanite, apatite, and magnetite. The mylonitic gneiss-granite has a mantled porphyroclast texture that may be characterized by large asymmetrical porphyroclasts of K-feldspar and plagioclase with a mantle which includes white-mica, biotite, quartz and feldspar aggregates. Some of the petrographic evidence show dynamic deformation during the crystallization such as grain boundary migration (GBM or sub-grain rotation (SGR, patchy perthite. Evidence of strain, such as deformation twins, bent or curved twins, undulatory extinction occur characteristically in plagioclase and display dynamic deformation in solid state. The rocks exhibit identical compositional ranges with 71.24–78.35 wt.% SiO2; high levels of alkalies (Na2O ranges from 3.07 to 4.02 %, K2O varies from 4.18 to 5.53 %; low levels of Fe2O3tot (0.80 to 2.60 %. Also, the trace element compositions display significant variations, such as Zr (157.7-330.5 ppm, Eu (0.07-0.28 ppm, Nb (40.9-77.3 ppm, Ga (19.7-25.97 ppm. The studied rocks are strongly enriched in LREE and HFSE and show a strong depletion in Ba, Sr, Eu and Ti and enrichment in Rb and Zr. The element contents are also similar to typical A-type granite (Whalen et al., 1987. The rocks are alkali to alkali-calcic, metaluminous to mildly peraluminous granite and ferroan in new geochemical classification scheme for granitoids (proposed by Frost et al., 2001. Discussion The chondrite-normalized rare-earth element patterns of the mylonitic gneiss- granitic rocks indicate the LREE over HREE fractionation with significant negative Eu anomalies. Primitive-mantle-normalized spidergrams (Sun and McDonough, 1989 normalized trace element patterns with negative Ba and Nb anomalies, and positive Rb, Th and Ce anomalies, simulate the collisional and post-collisional granitoids of Pearce et al (Pearce et al., 1984. All of the samples fall in the A2 group in Eby classification (Eby, 1992. On the tectonic discrimination plots, the granites show a within-plate granite (WPG

  12. Status of LLNL granite projects

    International Nuclear Information System (INIS)

    Ramspott, L.D.

    1980-01-01

    The status of LLNL Projects dealing with nuclear waste disposal in granitic rocks is reviewed. This review covers work done subsequent to the June 1979 Workshop on Thermomechanical Modeling for a Hardrock Waste Repository and is prepared for the July 1980 Workshop on Thermomechanical-Hydrochemical Modeling for a Hardrock Waste Repository. Topics reviewed include laboratory determination of thermal, mechanical, and transport properties of rocks at conditions simulating a deep geologic repository, and field testing at the Climax granitic stock at the USDOE Nevada Test Site

  13. 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

  14. 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).

  15. Contribution to the radioactivity of Um Ara granitic pluton, south-eastern desert, Egypt

    International Nuclear Information System (INIS)

    El Reedy, M.W.; Kamel, A.F.; Mansour, S.E.I.

    1988-01-01

    Um Ara area lies in the southern part of the eastern desert between latitudes 22 0 30' and 22 0 41'N and longitudes 33 0 46' and 33 0 54'E. Several types of granitic varieties ranging from high silica granite (SiO 2 >75%) to low silica granite (SiO 2 68-70%) occur in Um Ara granitic pluton. Surface samples were collected from the high anomalous locations in the pluton together with trenches samples (about 50cm in depth). The U content in the surface samples ranges from 69 to 7 ppm while in trenches samples, it ranges from 38 to 759 ppm. The thorium content on the other hand ranges from 34 to 402 ppm in surface samples and from 158 to 316 ppm in trenches samples. Some samples show no Th contents. The Th/U ratios ranges from 0.065 to 3.137 in surface samples and from 0.386 to 2.590 in trenches samples. An enrichment of U content is the main feature characterising this granitic pluton, it is mainly connected with the fractured zones. Uranium is mostly present as secondary U mineralization accompanied by Fe, Mn and to some extent by carbonate materials. A hydrothermal origin could be considered for this U mineralization in the pluton. Primary U mineralization (pitchblende) together with secondary mineralization was observed in some locations in the area disseminated in the granite, this reflects the syngenetic origin of this granitic type

  16. Granites petrology, structure, geological setting, and metallogeny

    CERN Document Server

    Nédélec, Anne; Bowden, Peter

    2015-01-01

    Granites are emblematic rocks developed from a magma that crystallized in the Earth’s crust. They ultimately outcrop at the surface worldwide. This book, translated and updated from the original French edition Pétrologie des Granites (2011) is a modern presentation of granitic rocks from magma genesis to their crystallization at a higher level into the crust. Segregation from the source, magma ascent and shapes of granitic intrusions are also discussed, as well as the eventual formation of hybrid rocks by mingling/mixing processes and the thermomechanical aspects in country rocks around granite plutons. Modern techniques for structural studies of granites are detailed extensively. Granites are considered in their geological spatial and temporal frame, in relation with plate tectonics and Earth history from the Archaean eon. A chapter on granite metallogeny explains how elements of economic interest are concentrated during magma crystallization, and examples of Sn, Cu, F and U ore deposits are presented. Mi...

  17. 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)

  18. 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.

  19. 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.

  20. 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)

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  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. Distribution of monazite in granite and alluvial of South Bangka

    International Nuclear Information System (INIS)

    Ngadenin

    2011-01-01

    Monazite is one source of thorium (Th), which has significant economic value and potential as an alternative fuel of nuclear power plants. The aims of research is to find out the distribution monazite alternative fuel of nuclear power plants. The aims of research is to find out the distribution monazite and its potential as a resource of radioactive minerals on the Bangka Island, then the data will be used and its potential as a resource of radioactive minerals on the Bangka Island, then the data will be used as a reference in the development of radioactive minerals exploration areas in the coming year. The research location is in the Bencah and Gadung villages, South Bangka Regency. The method used is the geological mapping, sampling of rock for petrographic, mineragraphic and autoradiographic analysis and heavy mineral for grains counting analysis. The results showed that lithologic area of Bencah Village composed of clay stone and alluvial deposits, while the Gadung Village composed by granite and alluvial deposits. Granite Gadung is predicted as the ilmenite series granite and tend to be of S type, while the material of Bencah alluvial is predicted come from the Klabat granite groups. In general, distribution of monazite in the alluvial slightly more potent of monazite than in the granite so that the development of radioactive minerals exploration will be prioritized in the alluvial areas. (author)

  10. Study on microwave digestion technique of granite with high pressure vessel

    International Nuclear Information System (INIS)

    Xiao Chengjian; Luo Yangming; Fu Zhonghua

    2008-06-01

    The digestion relation of heating time, temperature and pressure for acids is discussed in closed container under microwave field. Some granite samples were digested by microwave in 100 ml closed container. The results show that the best acid to digest granite samples is a combination of HNO 3 and HF, 0.5 g sample powder can be digested completely in 21 minutes, and that the maximum sample mass is 2.0 g using 100 ml closed container. (authors)

  11. 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)

  12. Aqueous phase transport through granitic rocks

    International Nuclear Information System (INIS)

    Bradbury, M.H.; Green, A.

    1984-03-01

    Using Scottish granites of UK origin it has been established that : (1) pore connectivity exists over metre distances and does not vary significantly with distance. (2) The formation factor may show an increase by a factor of approx. 2 for thin samples (approx. 1 cm). Since diffusion samples are of this order of thickness, laboratory measurements may be overestimating the diffusion coefficient appropriate for use in migration model calculations by a factor of approx. 2. (3) The effect of confining pressures up to approx. 16 MPa is to reduce diffusion coefficients by 50 to 60%. This implies that diffusion coefficients appropriate to granite at depths of approx. 500 m are approximately a factor of two lower than those obtained in the laboratory. (4) Diffusion rates through weathered fissure surfaces can be significantly greater (up to approx. 200 times) than through 'good' rock and are strongly dependent on the severity of the weathering. No evidence for pore blocking by weathering products was found. (5) Latex colloids having a diameter of 0.312 μm neither cause pore blocking nor do they penetrate the pore structure. (author)

  13. Granite - water interactions at 100 deg C, 50 MPa: an experimental study

    International Nuclear Information System (INIS)

    Savage, D.

    1984-01-01

    A monzogranite was reacted with water in hydrothermal solution equipment at 100 deg C, 50 MPa for 203 days, during which time six fluid samples were extracted at run temperature and pressure for chemical analysis. Fluid samples were analysed using ICP, INAA and standard wet chemical techniques and data are presented for 18 chemical species. Solids were examined using XRD and SEM. The high temperature speciation of the fluid phase chemistry was investigated using the geochemical software package EQ3/6. The evolution of the fluid phase chemistry is discussed in terms of mineral-fluid equilibria and the kinetics of mineral dissolution and precipitation reactions. The implications of these results to the modelling of the near-field geochemical environment of a high-level radioactive waste repository in granitic rock are discussed. (author)

  14. 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

  15. 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

  16. Chemical Variations in a Granitic Pluton and Its Surrounding Rocks.

    Science.gov (United States)

    Baird, A K; McIntyre, D B; Welday, E E; Madlem, K W

    1964-10-09

    New techniques of x-ray fluorescence spectrography have provided, for the first time, abundant data regarding chemical variability of granitic rocks on different scales. The results suggest that current designs of sampling plans for trend surface analysis should be modified; in particular several specimens, preferably drillcores, may be required at each locality.

  17. 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%.

  18. 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.

  19. 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

  20. 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.

  1. 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

  2. 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.

  3. 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).

  4. 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

  5. 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).

  6. 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...

  7. 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...

  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. Thermal expansion behaviour of granites

    Czech Academy of Sciences Publication Activity Database

    Plevová, Eva; Vaculíková, Lenka; Kožušníková, Alena; Ritz, M.; Simha Martynková, G.

    2016-01-01

    Roč. 123, č. 2 (2016), s. 1555-1561 ISSN 1388-6150 R&D Projects: GA MŠk ED2.1.00/03.0082; GA MŠk(CZ) LO1406 Institutional support: RVO:68145535 Keywords : thermomechanical analysis * differential thermal analysis * granites Subject RIV: DB - Geology ; Mineralogy Impact factor: 1.953, year: 2016 http://link.springer.com/article/10.1007/s10973-015-4996-z

  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. Alkaline lixiviation of uranium in granitic pegmatite

    International Nuclear Information System (INIS)

    Jambor, S.

    1980-06-01

    The work described herein concerns the determination of the experimental optimum conditions for the alkaline lixiviation of uranium based on the following parameters: time, pH, temperature, density and grane size. The samples were obtained from the Supamo complex, near the Currupia river in the Piar District of the Bolivar State in Venezuela. They have a granitic composition and graphitic texture. The uranium was found in them as a secondary oxidized mineral of green-yellow colour localized in fractures fissures, intergranular spaces and also in the mica as. Secondary uranitite. The lixiviation process was carried out using Na 2 CO 3 /NaHCO 3 buffer solution and for 100 gr. samples the best values for an efficient process were found by using 170 mesh grane size and 500 ml of pH buffer at 70 0 C for a 24 hour time period. (author)

  19. Distribution of radioactive minerals in a granite

    Energy Technology Data Exchange (ETDEWEB)

    Coppens, R

    1949-04-04

    The study, by means of a photographic plate, of the radioactivity of a Brittany granite, both of a pulverized sample and of a polished sample, has resulted in a complete determination of the radioactivity present. The ratio of the concentration of Th to that of U i.e., C/sub Th/C/sub U/, was determined as approximately 2.8 using the relationship between the concentration of these elements and the number of ..beta.. particles in a particular range which were detected. Using this ratio and measuring the average number of ..cap alpha.. particles emitted/cm/sup 2//sec, the average activities were found to correspond to concentrations of the order of 10/sup -5/ of both metals. The lack of uniformity in the distribution of the radioactivity within the crystal is noted.

  20. Protocol proposal for radon concentration mensuration from granitic rocks in marble factory; Proposta de protocolo para medicao de concentracoes de radonio proveniente de rochas graniticas em marmorarias

    Energy Technology Data Exchange (ETDEWEB)

    Del Claro, Flavia

    2016-11-01

    Naturally occurring radionuclides such as radon ({sup 222}Rn), its decay products and other elements from the radioactive series of uranium ({sup 238}U and {sup 235}U) and thorium ({sup 232}Th) are an important source of human exposure to natural radioactivity. The worldwide evaluation of health radiobiological effects and risks from population exposure to natural radionuclides is a growing concern. Radionuclides such as radon ({sup 222}Rn), the thoron ({sup 220}Rn), radio ({sup 2}'2'6Ra), thorium ({sup 23}'2Th) and potassium ({sup 40}K) may occur in materials commonly used in construction of dwellings and buildings. Thus, the radioactivity from marbles and granites is of importance, so that under certain conditions these materials radioactivity levels can be hazardous requiring the implementation of mitigation measurements. This research presents a technical protocol marble factories for the control human exposure to natural radioactivity exhaled from granitic rocks. The protocol was based on measurements of the {sup 222}Rn and {sup 220}Rn concentration in Brazilian granite rocks commonly nationally and exported. The {sup 222}Rn and {sup 220}Rn measurements were done using the AlphaGUARD (Saphymo GmbH) and RAD7 (Durridge Company) apparatus, respectively. The samples of granite were sealed in glass jars for 40 days in to achieve secular equilibrium between {sup 226}Ra and {sup 222}Rn radionuclides. The measurements were performed on Applied Nuclear Physics Laboratory at the Federal Technological University of Parana. Also, solid-state nuclear track detectors CR-39 were installed in a marble factory environments located in Curitiba - Parana for the evaluation of {sup 222}Rn concentrations in workplaces. The CR-39 detectors were exposed for about 90 days and submitted to etching process. The alpha particle tracks were observed using an optical microscope. Some granite samples analyzed presented {sup 222}Rn concentrations of attention, since the average

  1. Etude de la diagraphie neutron du granite de Beauvoir. Effet neutron des altérations et de la matrice du granite. Calibration granite. Porosité totale à l'eau et porosité neutron Analysis of the Beauvoir Granite Neutron Log. Neutron Effect of Alterations and of the Granite Matrix. Granite Calibration. Total Water Porosity and Neutron Porosity

    Directory of Open Access Journals (Sweden)

    Galle C.

    2006-11-01

    carottes (n. Nous montrons que, pour le granite de Beauvoir, l'effet neutron de la matrice est important (en moyenne proche de 7% et ne peut être négligé lorsque l'on mesure des porosités voisines de 0,5% sur carottes. La calibration de l'outil neutron dans le granite et non pas dans des calcaires est d'autre part capitale quant à la précision quantitative des résultats. This article describes the research done on the Beauvoir granite (Echassières GPF 1 borehole, French Massif Central range. The aim of this project was to obtain representative values of the water saturation (n total free water porosity of the Beauvoir granite from PorosityN neutron porosity (BRGM neutron log. The exact knowledge of the porosity of a crystalline block is effectively fundamental to determine its possibilities for being used as a waste storage site. With this goal, neutron logging provides indispensable information concerning the characterization of a porous medium. Our procedure was experimental, and we tried to go more deeply into various problems linked to the use of neutron logging in a granitic rock. Two main factors governed the neutron response : (i the hydrogen concentration of the formation (free water and combined water of various minerals and (ii the presence of absorber elements with a large capture cross-section such as gadolinium, cadmium, boron as well as lithium for the Beauvoir granite. After measuring the Beauvoir granite n total (free water porosity on core samples, we evaluated the combined water content of each sample tested on the basis of fire loss tests on rock powder at 900°C. From the hydrogen atoms volumic concentration, we determined a hydrogen index that we directly converted into the PorosityN(OH- neutron porosity, (by definition, pure water at 20°C has a hydrogen index of 1 which is equivalent to a 100% porosity. For the Beauvoir granite, the matrix combined water represents an average neutron porosity (Table 1 of about 4%. In the second phase, we used

  2. 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

  3. Assessment of radioactivity in building material(granite) in Sudan

    International Nuclear Information System (INIS)

    Osman, Z. A; Salih, I; Albadwai, K. A; Salih, A. M; Salih, S. A.

    2016-01-01

    In the present work radioactivity in building materials (granite) central Sudan was evaluated. In general the building materials used in Sudan are derived either from rocks or soil. These contain trace amounts of naturally occurring radioactive materials(NORMs), so it contains radionuclides from uranium and thorium series and natural potassium. The levels of these radionuclides vary according to the geology of their site of origin. High levels increase the risk of radiation exposure in homes(especially exposure due to radon). Investigation of radioactivity in granite used of the building materials in Sudan is carried out, a total of 18 major samples of granite have been collected and measured using X- ray fluorescence system (30 mci). The activity concentrations have been determined for uranium ("2"3"8U), thorium ('2"3"2Th) and potassium("4"0K) in each sample. The concentrations of uranium have been found to range from 14.81 Bq/kg to 24.572 Bq/kg, thorium between 10.02 Bq/kg and 10.020-84.79 Bq/kg and the potassium concentration varies between 13.33 Bq/kg to 82.13 Bq/kg. Limits of radioactivity in the granite are based on dose criteria for controls. This study can be used as a reference for more extensive studies of the same subject in future. (Author)

  4. Extraction of Th and U from Swiss granites

    International Nuclear Information System (INIS)

    Bajo, C.

    1980-12-01

    The extraction, at the laboratory level, of U and Th from Swiss granites is discussed. The Mittagfluh, Bergell and Rotondo granites and the Giuv syenite offered a wide range of U and Th concentrations; 7.7 to 20.0 ppm U and 25.5 to 67.0 ppm Th. U and Th were determined in the leach solutions by the fission track method and by spectrophotometry, respectively. Samples containing less than 0.3 μg U and 4 μg Th, could be measured with an accuracy of 10% for U and 5% for Th. Leach tests were performed during which the following parameters were varied: granite-type, grain size, acid-type, acid concentration, temperature and time. There were very great leaching differences between the granites studied. Temperature was the most important parameter. Sharp differences in extraction occurred between 20 0 C, 50 0 C and 80 0 C. At 80 0 C, more than 85% U and Th were extracted. The extraction curve (percent extracted as a function of time) of aliquots sampled after 1, 2, 4, 8, 12 and 24 hours showed a plateau after 8 hours. The half life of the reaction was between one and two hours. As a general rule, Th was better extracted than U. (Auth.)

  5. 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

  6. 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.

  7. Fracture patterns and stresses in granite

    International Nuclear Information System (INIS)

    Price, N.J.

    1979-01-01

    If granite bodies are to be used as receptacles for toxic waste materials, the presence or absence of barren fractures and the virgin stresses in the granite are of fundamental importance. Unfortunately, very little is known regarding the incidence of fractures, or stresses, which exist at depths (of about 1 km) in granite bodies. A simple analysis is presented of a hypothetical intrusion which indicates the magnitudes of stresses and the possible fracture development which may be expected in such bodies. (auth)

  8. Research on isotope geology. Assessment of heat production potential of granitic rocks and development of geothermal exploration techniques using radioactive/stable isotopes and fission track 2

    Energy Technology Data Exchange (ETDEWEB)

    Shin, Seong Cheon; Chi, Se Jung [Korea Inst. of Geology Mining and Materials, Taejon (Korea, Republic of)

    1995-12-01

    Radioelements and heat production rates of granitic rocks and stable isotopes of groundwaters were analyzed to investigate the geothermal potential of Wolchulsan granite complex in the southern Yeongam area. Wolchulsan granite complex is composed mainly by Cretaceous pink alkali-feldspar granite and partly Jurassic biotite granite. The main target for the geothermal exploration is the alkali-feldspar granite that is known in general to be favorable geothermal reservoir(e.g., Shap granite in UK). To develop exploration techniques for geothermal anomalies, all geochemical data were compared to those from the Jeonju granite complex. Heat production rates(HPR) of the alkali-feldspar granite is 1.8 - 10.6 {mu}Wm{sup -3}. High radio-thermal anomalies were revealed from the central western and northern parts of the granite body. These are relatively higher than the Caledonian hot dry granites in the UK. The integrated assessment of Wolchulsan granite complex suggests potential of the Cretaceous alkali-feldspar granite as a geothermal targets. Groundwater geochemistry of the Yeongam area reflects simple evaporation process and higher oxidation environment. Stable isotope data of groundwaters are plotted on or close to the Meteoric Water Line(MWL). These isotopic data indicate a significant meteoric water dominance and do not show oxygen isotope fractionation between groundwater and wall rocks. In despite of high HPR values of the Yeongam alkali-feldspar granite, groundwater samples do not show the same geochemical properties as a thermal water in the Jeonju area. This reason can be well explained by the comparison with geological settings of the Jeonju area. The Yeongam alkali-feldspar granite does not possess any adjacent heat source rocks despite its high radio-thermal HPR. While the Jeonju granite batholith has later heat source intrusive and suitable deep fracture system for water circulation with sedimentary cap rocks. (Abstract Truncated)

  9. Mobility of heavy metals through granitic soils using mini column infiltration test

    Science.gov (United States)

    Zarime, Nur'Aishah; Yaacob, W. Z. W.

    2014-09-01

    This study is about the mobility of cadmium through compacted granitic soils. Two granitic soils namely the Broga (BGR) and Kajang (KGR) granitic soils were collected in Selangor, Malaysia. Physical and chemical tests were applied for both granitic soils to determine the physical and chemical properties of soil materials. Physical test results shows granitic soils (BGR and KGR) have high percentage of sand ranging between 54%-63% and 46%-54% respectively, an intermediate and intermediate to high plasticity index as well as high specific gravity ie; 2.50-2.59 and 2.45-2.66 respectively. For chemical test, granitic soils shows acidic pH values ranged from 5.35-5.85 for BGR and pH 5.32-5.54 for KGR. For organic matter, SSA and CEC test, it shows low values ranged from 0.22%-0.34% and 0.39%- 0.50% respectively for organic matter test, 17.96 m2/g-21.93 m2/g and 25.76 m2/g-26.83 m2/g respectively for SSA test and 0.79 meq/100g-1.35 meq/100g and 1.31 meq/100g-1.35 meq/100g respectively for CEC test. Mini column infiltration test was conducted to determine the retention of cadmium while flowing through granite soils. This test conducted based on the falling head permeability concepts. Different G-force ranging from 231G to 1442G was used in this test. The breakthrough curves show the concentration of Cd becomes higher with the increasing of G-force for both granitic samples (BGR and KGR). The selectivity sorption for both granites ranked in the following decreasing order of; 231G>519G>923G>1442G. Results demonstrated that granitic soils also have low buffering capacity due to low resist of pH changes.

  10. Paleo-redox boundaries in fractured granite

    DEFF Research Database (Denmark)

    Dideriksen, K.; Christiansen, B. C.; Frandsen, Cathrine

    2010-01-01

    dissolved iron to the groundwater. During such cycling, the Fe isotopes fractionate to an extent that is expected to depend on temperature. In this study, we report on the use of Fe-oxides as paleoredox indicators, using their structure, morphology and Fe-composition as a clue for formation conditions....... In samples taken from similar to 120 m drill cores in granite from SE Sweden, X-ray amorphous, superparamagnetic, nanometre-sized Fe-oxides are confined to fractures of the upper,-,50 m, whereas well-crystalline Fe-oxides, with particle sizes typical for soils, occur down to similar to 110 m. We also...... identified hematite with a particle size of 100 nm, similar to hematite of hydrothermal origin. The Fe isotope composition of the fine-grained Fe-oxides (-1 parts per thousand

  11. 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

  12. 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).

  13. 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

  14. 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.

  15. Questioning the Sedimentary Paradigm for Granites

    Science.gov (United States)

    Glazner, A. F.; Bartley, J. M.; Coleman, D. S.; Boudreau, A.; Walker, J. D.

    2007-12-01

    A critical question regarding volcano-pluton links is whether plutons are samples of magma that passed through on its way to eruption, or residues left behind after volcanic rocks were extracted. A persistent theme of recent work on granites sensu lato is that many are sedimentary accumulations of crystals that lost significant volumes of magmatic liquid. This view is based on observations of structures that clearly seem to reflect deposition on a magma chamber floor (e.g., flows of chilled mafic magma into silicic magma) and on the inference that many other structures, such as modal layering, truncated layering, and crystal accumulations, reflect crystal sedimentation on such chamber floors. There are significant physical and geochemical reasons to question this view, based on observations in the Sierra Nevada of California and similar results from other batholiths. First, few granites show the enrichments in Ba, Sr, and relative Eu that feldspar accumulation should produce. Second, sedimentary features such as graded bedding and cross-bedding form in highly turbulent flows, but turbulence is unachievable in viscous silicic liquids, where velocities on the order of 104 m/s would be required to induce turbulence in a liquid with η=104 Pa s. Third, tabular modally layered domains commonly cut surrounding modal layering on both sides, and orientations of modal layering and of the troughs of "ladder dikes" commonly scatter widely within hectare-sized areas; it is difficult to reconcile these features with gravity-driven settling. Fourth, accumulations of K-feldspar megacrysts are typically inferred to be depositional, but this is precluded by crystallization of most K- feldspar after rheologic lock-up occurs. Finally, accumulations of K-feldspar and hornblende are typically packed too tightly to be depositional. With analogy to layered mafic intrusions, many features attributed to crystal sedimentation in granites may be better explained by crystal aging and other in

  16. Oster pluton (Central Karelia) - the ancient massif of two-feldspar granites of Baltic Shield

    International Nuclear Information System (INIS)

    Kovalenko, A.V.; Rizvanova, N.G.

    2000-01-01

    Geochronological study of two-feldspar granites forming the Oster pluton in the Central Karelia was performed using the methods of U-Pb- and Sm-Nd-dating. U-Pb isotope data for zircons from granite of the Oster pluton correspond to the age of 2876±21 mln. years, whereas Sm-Nd isotope data obtained for three samples of the garnet correspond to the age varying from 3.0 to 3.5 bln. years. The ancient age of granites of the Oster pluton is explained by the presence of a sufficiently powerful crust in the region by that moment [ru

  17. 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.

  18. An experimental study on the sorption of U(VI) onto granite

    International Nuclear Information System (INIS)

    Baik, Min Hoon; Hahn, Pil Soo

    2002-01-01

    The sorption of U(VI) on a domestic granite is studied as a function of experimental conditions such as contact time, solution-solid ratio, ionic strength, and pH using a batch procedure. The distribution coefficients, K d 's, of U(VI) are about 1-100mL/g depending on the experimental conditions. The sorption of U(VI) onto granite particles is greatly dependent upon the contact time, solution-solid ratio, and pH, but very little is dependent on the ionic strength. It is noticed that an U(VI)-carbonato ternary surface complex can be formed in the neutral range of pH. In the alkaline range of pH above 7, U(VI) sorption onto granite particles is greatly decreased due to the formation of anionic U(VI)-carbonato aqueous complexes

  19. 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.

  20. 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.

  1. 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.

  2. Petrogenesis of Karamaili alkaline A-type granites from East Junggar, Xinjiang (NW China) and their relationship with tin mineralization

    International Nuclear Information System (INIS)

    Su Yuping; Tang Hongfeng; Liu Congqiang; Hou Guangshun; Cong Feng; Sylvester, Paul J.; Qu Wenjun

    2007-01-01

    Several types of granites including alkaline granites and alkali feldspar granites are distributed in the Karamaili tectonic belt of East Junggar, Xinjiang, China. Some medium-small tin deposits are located within or near the contact zones of the granitic intrusions. The alkaline granites share all the features commonly observed in peralkaline A-type granites. They contain alkalic mafic minerals such as riebeckite and aegirine; have high contents of SiO 2 , alkalis, Rb, Th, Zr, Hf, REE (except Eu), and high ratios of FeO/MgO and Ga/Al; and show strong depletions in Ba, Sr, Eu in the spidergrams. Laser ablation-ICPMS U-Pb zircon geochronology indicates a crystallization age of ca. 305 Ma for the granites; TIMS analyses of the granites found high ε Nd (T) values of +5.9 to +6.5. Considering their geochemical features, alkaline granites most likely formed by fractional crystallization of graodioritic magmas, which were probably produced by partial melting of lower crustal basaltic to andesitic rocks formed from oceanic crustal materials that were deeply buried during late Palezoic subduction and accretion. Six molybdenite samples from the Sareshike tin deposit in East Junggar yielded an isochron age of 307±11 Ma (2σ) and a weighted mean model age of 306.5±3.4 Ma, consistent with zircon U-Pb ages of the alkaline granites. Low Re contents (0.323-0.961 ppm) in the molybdenite suggest that they originated from crustal sources related to the alkaline granites. Considering their identical ages, close spatial distribution, and similar sources, we argue that the A-type granites have a genetic relationship with the tin mineralization, and that the same association may be important elsewhere. (author)

  3. Structural and petrophysical characterisation of granite: intended for radioactive waste stocking

    International Nuclear Information System (INIS)

    Stanek, Martin

    2013-01-01

    Structural and petrophysical analysis have been conducted within the Melechov massif with focus on structures controlling the porosity, permeability and thermal conductivity of the rock. The structure of the massif has been constrained based on extensive dataset including AMS and field structural measurements of ductile and brittle structures. The fracture system of the massif has been described by four sets of fractures. The measured petrophysical data have been used to characterize the effect of fracturing and alteration on pore space geometry and in turn on permeability, thermal conductivity and elastic properties of the studied granite. Distinct petrophysical properties have been identified for pristine granite, for fractured fresh granite as well as for fractured granite altered by Fe-oxide, chlorite and clay minerals. A detailed microstructural study combined with multidirectional P-wave velocity measurements at high confining pressure and with AMS analysis has been conducted on a Schlieren bearing sample of Lipnice granite. The granite VP anisotropy at low confining pressure was controlled by intergranular cracks interconnecting Schlieren-sub parallel cleavage cracks in micas and feldspars and by exfoliation fracture-sub parallel intra- or trans-granular cracks in cleavage-free quartz. Major closing of the crack porosity linked to the Schlieren granite below depth of 500 m has been interpreted in terms of crack compliance reflected by rapid increase in VP with confining pressure. (author)

  4. 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...

  5. Carboniferous granite basement dredged from a site on the southwest margin of the Challenger Plateau, Tasman Sea

    International Nuclear Information System (INIS)

    Tulloch, A.J.; Kimbrough, D.L.; Wood, R.A.

    1991-01-01

    Discordant zircon fractions from a granite sample dredged off a basement horst on the western margin of the Challenger Plateau yield a 335 ± 7 Ma lower intercept date interpreted as the crystallisation age of the granite. This age, and the modal composition of the granite, is similar to that of the Karamea Suite of Westland and Nelson, New Zealand, and some Tasmanian granites. The concordia upper intercept date of 1747 ± 300 Ma implies the presence of Proterozoic continental crustal material in the source region of the granite. The Challenger granite is distinct from older S-type granites of southeastern Australia and I-type granites of northern Victoria Land and Marie Byrd Land, Antarctica. Subsequent to emplacement, the granite was brecciated and hydrothermally altered. A K-Ar age of 95 Ma on hydrothermal sericite indicates that this event overlapped with a major crustal extension event recorded in Westland and Nelson, and predates the oldest known sea floor in the Tasman Basin by at least 11 Ma. (author). 23 refs., 3 figs., 2 tabs

  6. Preliminary report on a glass burial experiment in granite

    International Nuclear Information System (INIS)

    Clark, D.E.; Zhu, B.F.; Robinson, R.S.; Wicks, G.G.

    1983-01-01

    Preliminary results of a two-year burial experiment in granite are discussed. Three compositions of simulated alkali borosilicate waste glasses were placed in boreholes approximately 350 meters deep. The glass sample configurations include mini-cans (stainless steel rings into which glass has been cast) and pineapple slices (thin sections from cylindrical blocks). Assemblies of these glass samples were prepared by stacking them together with granite, compacted bentonite and metal rings to provide several types of interfaces that are expected to occur in the repository. The assemblies were maintained at either ambient mine temperature (8 to 10 0 C) or 90 0 C. The glasses were analyzed before burial and after one month storage at 90 0 C. The most extensive surface degradation occurred on the glasses interfaced with bentonite. In general, very little attack was observed on glass surfaces in contact with the other materials. The limited field and laboratory data are compared

  7. 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...

  8. A compilation of radioelement concentrations in granitic rocks of the contiguous United States

    International Nuclear Information System (INIS)

    Stuckless, J.S.; VanTrump, G. Jr.

    1982-01-01

    Concentration data for uranium, thorium, and potassium have been compiled for approximately 2,500 granitic samples from the contiguous United States. Uranium and thorium concentrations and ratios involving these elements exhibit a log-normal distribution with statistical parameters. In order to check for a bias in the results due to high concentrations of data in anomalous or heavily sampled areas, the data were reevaluated by averaging all analyses within a 0.5 0 latitude by 0.5 0 longitude grid. The resulting data set contains 330 entries for which radioelements are log-normally distributed. Mean values are not significantly different from those of the ungridded data, but standard deviations are lower by as much as nearly 50 percent. The areal distribution of anomalously high values (more than one standard deviation greater than the geometric mean) does not delineate large uranium districts by either treatment of the data. There is sufficient information for approximately 1,500 samples to permit subdivision of the granites by degree of alumina saturation. Relative to the six variables listed above, peraluminous samples have slightly lower mean values, but the differences are not statistically significant. Standard deviations are also largest for the peraluminous granites with α for Th/U nearly 3 times larger for peraluminous granite than for metaluminous granite. Examination of the variations in Th/U ratios for a few specific granites for which isotopic data are available suggests that variability is caused by late-stage magmatic or secondary processes that may be associated with ore-forming processes. Therefore, although anomalous radioelement concentrations in granitic rocks do not seem to be useful in delineating large uranium provinces with sediment-hosted deposits, highly variable uranium concentrations or Th/U ratios in granitic rocks may be helpful in the search for uranium deposits

  9. 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...

  10. The research frontier and beyond: granitic terrains

    Science.gov (United States)

    Twidale, C. R.

    1993-07-01

    Investigations of granite forms and landscapes over the past two centuries suggest that many features, major and minor, are shaped by fracture-controlled subsurface weathering, and particularly moisture-driven alteration: in other words etch forms are especially well represented in granitic terrains. Commonly referred to as two stage forms, many are in reality multistage in origin, for the structural contrasts exploited by weathering and erosion that are essential to the mechanism originated as magmatic, thermal or tectonic events in the distant geological past. Fracture patterns are critical to landform and landscape development in granitic terrains, but other structural factors also come into play. Location with respect to water table and moisture contact are also important. Once exposed and comparatively dry, granite forms tend to stability; they are developed and diversified, and many are gradually destroyed as new, epigene, forms evolve, but many granite forms persist over long ages. Reinforcement effects frequently play a part in landform development. Several granite forms are convergent, i.e. features of similar morphology evolve under the influence of different processes, frequently in contrasted environments. On the other hand many landforms considered to be typical of granitic terrains are also developed in bedrock that is petrologically different but physically similar to granite; and in particular is subdivided by fractures of similar pattern and density. To date, most of the general statements concerning the evolution of granitic terrains have been based in work in the tropics but other climatic settings, and notably those of cold land, are now yielding significant results. Future research will extend and develop these avenues, but biotic factors, and particularly the role of bacteria, in such areas as weathering, will take on a new importance. Structural variations inherited from the magnetic, thermal and tectonic events to which granite bodies have

  11. The spatial variation of initial 87Sr/86Sr ratios in the Toki granite, Central Japan. Implications for the intrusion and cooling processes of a granitic pluton

    International Nuclear Information System (INIS)

    Yuguchi, Takashi; Tsuruta, Tadahiko; Hama, Katsuhiro; Nishiyama, Tadao

    2013-01-01

    The spatial variation in initial 87 Sr/ 86 Sr ratios (SrI) in the Toki granite, Central Japan, shows heterogeneity ranging from 0.708942 to 0.710069, which provides information on the intrusion and cooling processes of plutons. The Toki granite has three mineralogy-based rock facies: muscovite-biotite granite (MBG), hornblende-biotite granite (HBG) and biotite granite (BG). Large SrI values were found to be distributed at the western margin (west MBG) and the lithologically central region (central BG), while small SrI values were found at the northeast margin (northeast MBG). Regions with high and low Sr concentrations were also found in the Toki granite. In the Sr-rich samples, SrI (0.708942-0.709789) increases with 100/Sr (0.7-1.5). This geochemical trend extends towards the country sedimentary rocks of the Mino Terrane, which can be interpreted to result from assimilation and fractional crystallization (AFC) between the original granitic magma and the Mino sedimentary rocks. The SrI values in the Sr-rich regions show a correlation with the Alumina Saturation Index (ASI). In particular, the west MBG, with large SrI values, is classified as a peraluminous granitoid with large ASI, suggesting that the western margin of the pluton was strongly affected by assimilation during the intrusion process. The Sr-poor samples are present both in the central BG, with large SrI values, and in the northeast MBG, with small SrI values. The Sr-poor samples have small ASI and large differentiation indices, indicating that the central BG and the northeast MBG were generated either by different AFC process with different amounts of contaminants or by the intrusion and fractionation of different source magma with different SrI values. Overall, the geochemical spatial variations found in the Toki granite can be explained by various degrees of assimilation and fractional crystallization in the magma chamber and/or multi-stage intrusions with different degrees of crystallization of

  12. Thermal expansion of granite rocks

    International Nuclear Information System (INIS)

    Stephansson, O.

    1978-04-01

    The thermal expansion of rocks is strongly controlled by the thermal expansion of the minerals. The theoretical thermal expansion of the Stripa Granite is gound to be 21 . 10 -6 [deg C] -1 at 25 deg C and 38 . 10 -6 [deg C] -1 at 400 deg C. The difference in expansion for the rock forming minerals causes micro cracking at heating. The expansion due to micro cracks is found to be of the same order as the mineral expansion. Most of the micro cracks will close at pressures of the order of 10 - 20 MPa. The thermal expansion of a rock mass including the effect of joints is determined in the pilot heater test in the Stripa Mine

  13. Geochemistry of biotite granites from the Lamas de Olo Pluton, northern Portugal

    Science.gov (United States)

    Fernandes, Susana; Gomes, Maria; Teixeira, Rui; Corfu, Fernando

    2013-04-01

    .21, and display isotopic signatures of (87Sr/86Sr)i = 0.7044-0.7077 and Nd = -2.2 to -1.1. Six samples of LO define a whole rock isochron age of 285±15 Ma with (87Sr/86Sr)i = 0.7051±0.001 (MSWD = 0.11). Two monazite analyses for the LO granite yield an weighted average 207Pb/235U age of 297.19±0.73 Ma, consistent with the preliminary ID-TIMS U-Pb analyses of two transparent and euhedral prisms of zircon that define a concordia age of 296.37 ±0.52 Ma (MSWD = 0.66). The linear trends of major and trace elements variation diagrams of LO and AC granites and their similar mean values of (87Sr/86Sr)i point, at this stage, to an involvement of mid-crustal sources, probably mixed with asthenospheric material. Therefore, LOP consists of post-D3 biotite granites installed in higher structural crustal levels, testifying the occurrence of a crustal growth episode after the major recycling processes that occurred during the deformation phase D3. We thank Prof. J.F. Santos and Dr. S. Ribeiro and Petrochron project (PTDC/CTE-GIX/112561/2009) for the Rb-Sr isotopic data obtained at LGI of University of Aveiro, Portugal. Dias, G. et al. 1998. Lithos, 45, 349-369. Pereira, E., 1989. Serviços Geológicos de Portugal.

  14. Two-mica granites of northeastern Nevada.

    Science.gov (United States)

    Lee, D.E.; Kistler, R.W.; Friedman, I.; Van Loenen, R. E.

    1981-01-01

    The field settings are described and analytical data are presented for six two-mica granites from NE Nevada. High delta 18O and 87Sr/86Sr values indicate that all are S-type granite, derived from continental crust. The major element chemistry and accessory mineral contents of these rocks also are characteristic of S-type granites. Chemical, X ray, and other data are presented for the micas recovered from these granites. The muscovites are notably high in Fe2O3, FeO, and MgO. Except for one hydrobiotite, each of the biotites has an MgO content near 6.0 wt%. Two different types of two-mica granites are recognized in the area of this study. One type is distinguished by the presence of many biotite euhedra within muscovite phenocrysts and by an unusual suite of accessory minerals completely devoid of opaque oxides. This type probably resulted from anatexis of late Precambrian argillites under conditions of relatively low oxygen fugacity, along a line that roughly coincides with the westward disappearance of continental basement. In the other textural type of two-mica granite the micas are equigranular and there is a greater variety of accessory minerals. The magmatic evolution of this type also appears to reflect the influence of late Precambrian argillites; there may be age differences between the two types of two-mica granites.-Author

  15. Uranium-enriched granites in Sweden

    International Nuclear Information System (INIS)

    Wilson, M.R.; Aakerblom, G.

    1980-01-01

    Granites with uranium contents higher than normal occur in a variety of geological settings in the Swedish Precambrian, and represent a variety of granite types and ages. They may have been generated by the anatexis of continental crust or processes occurring at a much greater depth. They commonly show enrichment in F, Sn, W and/or Mo. Only in one case is an important uranium mineralization thought to be directly related to a uranium-enriched granite, while the majority of epigenetic uranium mineralizations with economic potential are related to hydrothermal processes in areas where the bedrock is regionally uranium-enhanced. (author)

  16. Lower Granite dam smolt monitoring program: annual report, 2000; ANNUAL

    International Nuclear Information System (INIS)

    Morrill, Charles

    2000-01-01

    The 2000 fish collection season at Lower Granite was characterized by lower than average spring flows and spill, low levels of debris, cool water temperatures, increased unclipped yearling and subyearling chinook smolts, and 8,300,546 smolts collected and transported compared to 5,882,872 in 1999. With the continued release of unclipped supplementation chinook and steelhead above Lower Granite Dam, we can no longer accurately distinguish wild chinook, steelhead, and sockeye/kokanee in the sample. Although some table titles in this report still show ''wild'' column headings, the numbers in these columns for 1999 and 2000 include wild and unclipped hatchery origin smolts. The increases over previous years reflect the increased supplementation. A total of 8,300,546 juvenile salmonids were collected at Lower Granite Dam. Of these, 187,862 fish were bypassed back to the river and 7,950,648 were transported to release sites below Bonneville Dam, 7,778,853 by barge and 171,795 by truck. A total of 151,344 salmonids were examined in daily samples. Nine research projects conducted by four agencies impacted a total of 1,361,006 smolts (16.4% of the total collection)

  17. Hydrothermally-induced changes in mineralogy and magnetic properties of oxidized A-type granites

    Science.gov (United States)

    Nédélec, Anne; Trindade, Ricardo; Peschler, Anne; Archanjo, Carlos; Macouin, Mélina; Poitrasson, Franck; Bouchez, Jean-Luc

    2015-01-01

    The changes in magnetic mineralogy due to the hydrothermal alteration of A-type granitic rocks have been thoroughly investigated in samples from the granite of Tana (Corsica, France), and compared with other A-type granites: Meruoca (NE Brazil), Bushveld (South Africa), Mount Scott (Wichita Mountains, Oklahoma, USA) and the stratoid hypersolvus granites of Madagascar. The altered red-colored samples and their non-altered equivalents were magnetically characterized by means of magnetic susceptibility measurements, hysteresis loops, remanent coercivity spectra, and Lowrie test. It is shown that hydrothermalization in magnetite-bearing granites is related to the formation of fine-grained magnetite and hematite, and to coeval depletion in the content of primary low-coercive coarse-grained magnetite. These mineralogical changes give typical rock magnetic signatures, namely lower susceptibility magnitudes and anisotropy degrees, prolate AMS (anisotropy of magnetic susceptibility) fabrics and increased coercivities. Optical microscopy and SEM (scanning electronic microscopy) images suggest that the orientation of the secondary magnetic minerals is related to fluid-pathways and micro-fractures formed during the hydrothermal event and therefore may be unrelated to magma emplacement and crystallization fabrics. Changes in magnetic mineralogy and grain-size distribution have also to be considered for any paleomagnetic and iron isotope studies in granites.

  18. 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.

  19. 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 -

  20. 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

  1. 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.

  2. Study on radon and thoron levels in different types of granitic work industries around Tumkur city

    International Nuclear Information System (INIS)

    Nagabhushan, S.R.; Ujjinappa; Srilatha; Sannappa, J.

    2013-01-01

    Radon, Thoron and its progeny monitoring has become a global phenomenon due to its health hazards on human being. The concentration of radon, thoron and their progeny levels have been measured in different types of Granite and brick work industries around Tumkur city by using LR-115 type II Solid State Nuclear Track Detectors (SSNTDs) have been used for the measurement of these gases. The higher concentration of radon, thoron and their progeny were observed in the dwellings near brick industries compared to Granite cutting and polishing industries. The inhalation dose due to Radon, Thoron and their progeny to the workers and public living near these industries have been estimated. (author)

  3. 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

  4. Determination of dispersity of crushed granite

    International Nuclear Information System (INIS)

    Liu Dejun; Fan Xianhua; Zhang Yingjie; Yao Jun; Zhou Duo; Wang Yong

    2004-01-01

    The experimental crushed granite column breakthrough curves, using 99 Tc as spike tracer and 3 H as invariant tracer, are analyzed by different linear regression techniques. Dispersity of crushed granite and retardation factor of 99 TcO 4 - on the crushed granite are determined simultaneously by one linear regression technique. Dispersity of crushed granite is also obtained with 3 H as invariant tracer by the other linear regression technique. The dispersities found by spike source and invariant source methods are compared. The experimental results show that the dispersity found by spike source method is close to that found by invariant source method. It indicates that dispersity is only the characteristic of dispersion medium

  5. Determination of dispersity of crushed granite

    International Nuclear Information System (INIS)

    Liu, D.J.; Fan, X.H.

    2005-01-01

    Experimental crushed granite column breakthrough curves, using 99 Tc as spike tracer and 3 H as invariant tracer, were analyzed by different linear regression techniques. Dispersity of crushed granite and the retardation factor of 99 TcO 4 - on the crushed granite were determined simultaneously by one linear regression. Dispersity of crushed granite was also obtained with 3 H as invariant tracer by the other linear regression. The dispersities found by spike source and invariant source methods are compared. Experimental results show that the dispersity found by the spike source method is close to that found by the invariant source method. This indicates that dispersity is only a characteristic of the dispersion medium. (author)

  6. 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.

  7. 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.

  8. 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.

  9. 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...

  10. Petrogenesis of Malaysian tin granites: geochemistry, fractional crystallization, U-Pb zircon geochronology and tectonic setting

    Science.gov (United States)

    Wai-Pan Ng, Samuel; Searle, Mike; Whitehouse, Martin; Chung, Sun-Lin; Ghani, Azman; Robb, Laurence; Sone, Masatoshi; Oliver, Grahame; Gardiner, Nick; Roselee, Mohammad

    2014-05-01

    The Malaysian tin granites forming the backbone of the Thai-Malay Peninsula has been long recognized with two distinct granitic provinces:- 1. Early Permian to Late Triassic Eastern Province with mainly "I-type" (Hbl)-Bt granites with associated Cu-Au deposits, with subordinate Bt granites hosting limited Sn-W deposits, and 2. Late Triassic Main Range Province with mainly "S-type" Bt granites with associated Sn-W deposits, and subordinate (Hbl)-Bt granites. New geochemical data show that Chappell and White's (1974) I-S granite classification adopted in the existing model does not adequately distinguish the granites from one another as previously implied. Trace element geochemistry and Sr-Nd isotopic compositions show that the Malaysian tin granites in both provinces have transitional I-S characteristics. In addition, they inherited within-plate signature from Cambro-Ordovician Gondwana-related source rocks. Previous ages were obtained by whole rock Rb-Sr and biotite K-Ar geochronology in the 70s and 80s, dating methods that may not accurately represent the crystallization age of granites. We re-sampled the entire Malaysian Peninsula and 40 samples were collected for high-precision U-Pb SIMS dating on extracted zircon grains in order to better constrain the magmatic and tectonic evolution of Southeast Asia. The crystallization ages of the Eastern Province granitoids have been constrained ranging from 220 to 290 Ma, while the Main Range (Western) Province granitoids have ages ranging from 200 to 230 Ma. A progressive westward younging trend is apparent across the Eastern Province, but becomes less obvious in the Main Range Province. Our model suggests two east dipping subduction zones. We suggest that subduction roll-back along the Bentong-Raub suture might account for the westward younging trend, in the Eastern province. A second Late Triassic east-dipping subduction zone beneath western Malaysia is proposed in order to explain the "I-type" components to the Main

  11. Limit of the radionuclides in granite

    International Nuclear Information System (INIS)

    Wang Shaling; Jiang Rangrong

    2003-01-01

    Granite is an important sort of building materials. Their radionuclide contents are limited by the national standard GB6566-2001 just as other building materials. This standard divides them into main materials and decorative materials, and relaxes the limit of the latter obviously. Owing to the consideration of public dose limit and environment protection, this method needs discussion. Otherwise, red granite contains high radionuclide contents relatively, especially the sort of Indian Red, and need be paid more attention

  12. Granite Exfoliation, Cosumnes River Watershed, Somerset, California

    Science.gov (United States)

    Crockett, I. Q.; Neiss-Cortez, M.

    2015-12-01

    In the Sierra Nevada foothills of California there are many exposed granite plutons within the greater Sierra Nevada batholith. As with most exposed parts of the batholith, these granite slabs exfoliate. It is important to understand exfoliation for issues of public safety as it can cause rock slides near homes, roads, and recreation areas. Through observation, measuring, and mapping we characterize exfoliation in our Cosumnes River watershed community.

  13. 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)

  14. Preliminary analysis of rare earth in knowledge of uranium metallogeny in the granite from San Ramon-La Merced, Junin

    International Nuclear Information System (INIS)

    Valencia, Jacinto

    2014-01-01

    The study shows the petrogenesis of San Ramon granite by the interpretation of Rare Earth Elements (REE) analyzed from the metallogenic understanding of the presence of uranium. The preliminary results indicate that the intrusive has originated from a very distinct crustal magma source of per-aluminous alkaline composition; constituting the negative anomaly of Europium (Eu) element confirming the cortical origin of granite; accordingly, uranium mineralization represented by torbernite, from a source of per-aluminous alkaline composition. The REE help to establish a genetic relationship with granite, which was placed in the late stages of magmatism, while uranium has originated from the same granite by hydrothermal incipient process. SR-1.1 sample presents the largest partition of REE in the diagram and is related to the Th and U amounts in facie red granite. (author).

  15. 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

  16. Magnetic susceptibility of Variscan granite-types of the Spanish Central System and the redox state of magma

    Energy Technology Data Exchange (ETDEWEB)

    Villaseca, C.; Ruiz-Martínez, V.C.; Pérez-Soba, C.

    2017-07-01

    Magnetic susceptibility (MS) has been measured in Variscan granites from central Spain. They yield values in the order of 15 to 180μSI units for S- and I-type granites, indicating that both types belong to the ilmenite series. Only samples from magnetite-bearing leucogranites from the I-type La Pedriza massif show high MS values, in the order of 500-1400μSI, reflecting the presence of this ferromagnetic mineral. Mineral chemistry of magmatic Fe-rich minerals (mainly biotite) suggests similar oxidation values for both granite types. MS values change in highly fractionated granites accordingly either with the presence of rare new Fe-oxide phases (some I-type leucogranites) or with the marked modal amount decrease of Fe-rich minerals (I- and S-type leucogranites). The redox state in highly fractionated granite melts is mostly controlled by magmatic processes that modify redox conditions inherited from the source region. Thus, the occurrence of magnetite or ilmenite in granites is primarily controlled by the oxidation state of the source material but also by the differentiation degree of the granite melt. The presence of magnetite in some Variscan I-type leucogranites might be a consequence of crystal fractionation processes in a more limited mafic mineral assemblage than in S-type granite melts.

  17. 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...

  18. 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)

  19. 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.

  20. 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

  1. 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.

  2. Electrical conductivity of sandstone, limestone, and granite

    Energy Technology Data Exchange (ETDEWEB)

    Duba, A.; Piwinskii, A.J.; Santor, M.; Weed, H.C.

    1978-01-01

    The electrical conductivity of cylindrical cores of Westerly granite, Indiana limestone and Nugget, St Peter and Kayenta sandstones was measured at about 25/sup 0/C in vacuo, in air, and after saturation in distilled water, tap water, and 0.1 M NaCl solution. The three-electrode technique with a guard ring and the two-electrode technique without a guard ring were used. Core aspect ratio over the range of 2.00 to 0.25, as well as frequency over the range of 50 Hz to 10 kHz, influences the conductivity of all rocks, especially those measured in vacuo. Measurements from water-saturated samples using a guard ring are not appreciably different from those obtained without a guard ring. The conductivity of rocks saturated in 0.1 M NaCl solution changes least with a change in aspect ratio; for these rocks a linear relationship, known as Archie's Law, exists between log porosity and log conductivity. No simple correlation was found between those factors in rocks saturated with tap or distilled water. Thus, it appears Archie's Law is of questionable value for correlating laboratory data from rocks saturated with low-conductivity fluids.

  3. Emplacement and deformation of the A-type Madeira granite (Amazonian Craton, Brazil)

    Science.gov (United States)

    Siachoque, Astrid; Salazar, Carlos Alejandro; Trindade, Ricardo

    2017-04-01

    The Madeira granite is one of the Paleoproterozoic (1.82 Ga) A-type granite intrusions in the Amazonian Craton. It is elongated in the NE-SW direction and is composed of four facies. Classical structural techniques and the anisotropy of magnetic susceptibility (AMS) method were applied to the study of its internal fabric. Magnetic susceptibility measurements, thermomagnetic curves, remanent coercivity spectra, optical microscopy and SEM (scanning electron microscopy) analyses were carried out on the earlier and later facies of the Madeira granite: the rapakivi granite (RG) and the albite granite (AG) respectively. The last one is subdivided into the border albite granite (BAG) and the core albite granite (CAG) subfacies. AMS fabric pattern is controlled by pure magnetite in all facies, despite significant amounts of hematite in the BAG subfacies. Microstructural observations show that in almost all sites, magnetic fabric correlates to magmatic state fabrics that are defined by a weak NE-SW orientation of mafic and felsic silicates. However, strain mechanisms in both subfacies of AG also exhibit evidence for solid-state deformation at high to moderate temperatures. Pegmatite dyke, strike slip fault (SFA-B-C), hydrothermal vein, normal fault (F1-2) and joint (J) structures were observed and their orientation and kinematics is consistent with the magmatic and solid-state structures. Dykes, SFA-C and F1, are usually orientated along the N70°E/40°N plane, which is nearly parallel to the strike of AMS and magmatic foliations. In contrast, veins, SFB, F2 and some J are oriented perpendicular to the N70°E trend. Kinematic analysis in these structures shows evidence for a dextral sense of movement in the system in the brittle regime. The coherent structural pattern for the three facies of Madeira granite suggests that the different facies form a nested pluton. The coherence in orientation and kinematics from magmatic to high-temperature solid-state, and into the brittle

  4. Rn-222 release to the environment: comparison between different granite sources

    International Nuclear Information System (INIS)

    Mamoon, M.; Kamal, S.M.

    2005-01-01

    In this work three different types of granites were studied, namely: pure granite, alkali granite and altered (hydrated) alkali granite. General radioactivity of the granites was studied along with the potential for 222 Rn emanation. The study indicated that altered alkali granite releases, relatively, the highest 222 Rn emanation to the surrounding air while alkali granite emits the more intense gamma radiation of the three granites. Hence, altered alkali granite can be used as a laboratory source for 222 Rn.

  5. 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

  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

    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.

  7. Geochemical characteristics and origin of the Lebowa Granite Suite, Bushveld Complex

    Science.gov (United States)

    Hill, M.; Barker, F.; Hunter, D.; Knight, R.

    1996-01-01

    The ??? 2052-Ma Lebowa Granite Suite (LGS) represents the culminating phase of an Early Proterozoic magmatic cycle in the Central Transvaal area of the Kaapvaal Province. Following extrusion of at least 200,000 km3 of intermediate to acid volcanics (Rooiberg Felsite), mafic and ultramafic magmas intruded at 2065 Ma to form the Rustenburg Layered Suite (RLS). The LGS includes the Nebo, Makhutso, Bobbejaankop, Lease, and Klipkloof granites. The Nebo Granite intruded the Rooiberg Felsite as sheets up to 4 km thick above the RLS. Smaller stocks of the other granites crosscut the Nebo. We determined major- and trace-element compositions and oxygen, Rb-Sr, and Sm-Nd isotope ratios for samples of: Nebo Granite; Rooiberg Felsite; granophyre and granophyric granite; Makhutso, Bobbejaankop, and Lease granites; and feldspar porphyry from areas throughout the exposed area of the LGS (Dennilton, Verena Balmoral, Enkeldoorn, Sekhukhune Plateau, Zaaiplaats-Potgeitersrus, and Western Transvaal). Coherent floor-to-roof geochemical trends exist in some areas, although it is not possible to model them convincingly. Regional variations in geochemistry exist and likely are related to source variations in the estimated 200,000 km3 of the Nebo Granite sheets. ??18O for the LGS range from +5.9??? to +9.5???; if these are approximate primary magmatic values, pelitic sediments cannot have been an important source for the LGS. The Rb-Sr isotope system has been altered, a finding consistent with previous studies. A mineral isochron for Nebo Granite near Dennilton yields a York regression age of 1995 ?? 99 Ma, with initial 143Nd/144Nd = 0.50978??8 and ???CHUR=-5.12. Samples from the Sekhukhune Plateau have higher 143Nd/144Nd ratios than do Dennilton-area samples, suggesting that the former originated from older or less LREE-enriched sources. We suggest that intrusion of mafic to ultramafic magmas at depth in the continental crust triggered melting of Archean quartzofeldspathic crystalline

  8. Retardation of radionuclide transport by fracture flow in granite and argillaceous rocks

    International Nuclear Information System (INIS)

    Bradbury, M.H.; Green, A.

    1985-11-01

    Laboratory techniques have been developed for the measurement of diffusion rates and permeabilities through highly consolidated rock samples. The work has predominantly concentrated on the generation of diffusion data for slates and granites in particular. Rock properties fundamental to mass transfer processes have been obtained. Diffusion rates have been measured through weathered granite fissure surfaces and as a function of distance from such surfaces on core samples obtained from Troon, Cornwall. Pore connectivity over metre distances in granite cores has been shown to exist and diffusion coefficients were measured as a function of confining pressure in a specially designed rig. The Dsub(i) (intrinsic diffusion coefficient) values determined at ambient pressure were approximately a factor of 2 greater than those measured at pressures equivalent to 500 m of rock overburden. Some initial experiments on the accessibility of the pore space in granites to colloids based on a permeability technique indicated that such particles neither blocked pores nor penetrated through 15 mm thick samples over times of the order 2 to 3 thousand hours. Diffusion rates through samples of Canadian granites, some of which contained weathered fissure surfaces, were measured. (author)

  9. 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)

  10. 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

  11. Age of Pedra Branca granite (Goias) and possible geotectonic implications

    International Nuclear Information System (INIS)

    Marini, O.J.; Botelho, N.F.; Macambira, M.J.B.; Provost, A.

    1986-01-01

    Rb-Sr geochronologic dating of granites from the Pedra Branca Granite Massif (Nova Roma, Goias) shown an age of 1405 ± 21My. and a questionable initial Sr 87 /Sr 86 ratio of 0,7004 ± 0,006. Rhyolite from the base of the Arai Group is probably of the same age as the granitic intrusion. The 475 ± 19 My. age for the granitic intrusion is evidence of the Brasiliano Cycle imprint in Pedra Branca region. The age attributed to the Pedra Branca Granite is lower than known ages of the Goias tin granites giving rise to new geotectonic interpretations. It is possible that the Pedra Branca Granite represents a low-level intrusion emplaced at the beginning of structuration and deposition of the Arai basin. It may be correlated with granitic intrusions related to a rift stage above mantle hot spots, like the Nigerian tin younger granites. (author)

  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. Rare metal granites and related rocks of the Ukrainian shield

    Directory of Open Access Journals (Sweden)

    Esipchuk, K.Ye.

    1993-12-01

    Full Text Available Two rare metal leucocratic granites, Perga and Kamennaya complexes, can be distinquished on the Ukrainian shield. The Perga complex consists of medium- and coarse grained, mainly porphyric, biotite, riebeckite and aegirine granites, granite porphyries, microclinites and albitites with rare metal mineralization (genthelvite, phenacite, tantalite, cassiterite and wolframite etc.. Granites from several stocks (up to 30 km2 in the northwestern part of the shield, situated along the fracture zone, restricted the large Korosten pluton of rapakivi granites to the northwest. The age of these granites (Pb-Pb and U-Pb methods on zircon and monazite practically coincide with the age of rapakivi granites being 1750 Ma. Within the Korosten complex of rapakivi granites we consider that zinnwaldite granites, which are characterized by fluorite and topazine mineralization, represent the final phase of pluton. These granites differ from the Perga ones by their low content of rare metals. The Kamennaya Mogila complex lies in the southeastern part of the Ukrainian shield. It consists of biotite and muscovite-biotite, medium- and coarse-grained (also porphyric, and occasionally greisining granites with rare metal mineralization (cassiterite, columbite, molybdenite, wolframite and beryl. Granites form several stocks (5-30 km2 situated 10-30 km to the west-northwest of the South-Kalchik gabbro-syenite-granite pluton. Granitoids in both of these complexes have similar isotopic ages (1800 Ma. Leucocratic subalkaline granites (the Novoyanisol type are known within the pluton itself, occupying an intermediate position between the above mentioned in terms of mineral and geochemical composition. The gabbro-syenite-granite formation of the Nearazov region has a substantial similarity to the anorthosite-rapakivi-granite formation. In this respect the relation of each of them to rare metal granites is rather remarkable. This relation is, most probably, not only spatial, but

  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. Permeability of Granite Including Macro-Fracture Naturally Filled with Fine-Grained Minerals

    Science.gov (United States)

    Nara, Yoshitaka; Kato, Masaji; Niri, Ryuhei; Kohno, Masanori; Sato, Toshinori; Fukuda, Daisuke; Sato, Tsutomu; Takahashi, Manabu

    2018-03-01

    Information on the permeability of rock is essential for various geoengineering projects, such as geological disposal of radioactive wastes, hydrocarbon extraction, and natural hazard risk mitigation. It is especially important to investigate how fractures and pores influence the physical and transport properties of rock. Infiltration of groundwater through the damage zone fills fractures in granite with fine-grained minerals. However, the permeability of rock possessing a fracture naturally filled with fine-grained mineral grains has yet to be investigated. In this study, the permeabilities of granite samples, including a macro-fracture filled with clay and a mineral vein, are investigated. The permeability of granite with a fine-grained mineral vein agrees well with that of the intact sample, whereas the permeability of granite possessing a macro-fracture filled with clay is lower than that of the macro-fractured sample. The decrease in the permeability is due to the filling of fine-grained minerals and clay in the macro-fracture. It is concluded that the permeability of granite increases due to the existence of the fractures, but decreases upon filling them with fine-grained minerals.

  19. [Spectral characteristics and implication of granite from pozaiying molybdenite deposits in west of Guangdong].

    Science.gov (United States)

    An, Yan-Fei; Zhong, Li-li; Zhou, Yang-Zhang; Chen, Qing; Li, Xing-yuan

    2014-06-01

    Some granite samples from Pozaiying molybdenite deposits in the west of Guangdong were retrieved to characterize the spectral signature of XRD, FT-NIR and Raman. The results show that compared to the Porphyry granite and granite in the far zone, the signal of XRD and Raman of granite in near zone is weaker while the signal of FT-NIR is stronger. The authors' analyses indicate that the FWHM of quartz (101) peak in XRD, Sericite peak (4 529 cm(-1)) in FT-NIR and quartz peak in Raman shift from the latter are higher than those of former two. Those spectral characteristics indicate that compared with other samples, the content of petrogenetic mineral in samples from near zone is lower while the content of alteration mineral is higher, and its crystallinity and crystallization temperatures are both lower. The authors' studies suggest that there may be an alteration zone, embracing the granite-porphyry, which comprised low temperature mineral, and the quartz-porphyry which related to molybdenite mineralization belongs to the zone near Guanshanzhang mass.

  20. 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.

  1. Radiometric analysis of Chinese commercial granites

    International Nuclear Information System (INIS)

    Xinwei, L.; Lingqing, W.; Xiaodan, J.

    2006-01-01

    Due to the widespread use of granites as building and ornamental materials, measurements of 226 Ra, 232 Th and 40 K activities in commercial granites have been carried out using a NaI(Tl) γ-ray spectrometer with a matrix-inversion-based spectral stripping technique. The concentrations of 226 Ra, 232 Th and 40 K in Chinese commercial granite range from 14.5 to 204.7 Bq x kg -1 , 16.7 to 186.7 Bq x kg -1 and 185.7 to 1745.6 Bq x kg -1 , respectively. The mean values of the activity concentrations of 226 Ra, 232 Th and 40 K in red and pink commercial granites are all higher than those in black and gray commercial ones. The radium equivalent activity (Ra eq ), the external hazard index (H ex ), the internal hazard index (H in ) and the annual gonadal dose equivalent (AGDE) were also calculated and compared to the international recommended values. Six types of red commercial granites (CBR, MLR, QXR, PBR, JXR, LQR, YDR and TSR) of China do not satisfy the universal standards. (author)

  2. 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).

  3. 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.

  4. 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)

  5. 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)

  6. 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.

  7. Biofouling of granite-rapakivi in St. Petersburg monuments and in the quarry in Russia and Finland

    Science.gov (United States)

    Vlasov, Dmitry; Panova, Elena; Alampieva, Elena; Olhovaya, Elena; Popova, Tatyana; Vlasov, Alexey; Zelenskaya, Marina

    2013-04-01

    Granite-rapakivi was widely used in the architecture of St. Petersburg: the facades of buildings, embankments of rivers and canals, bridges, sculptural monuments, pedestals, facing the metro stations. This stone is rapidly destroyed due to the peculiarities of its structure. Biofouling of granite is insufficiently studied. Cause the destruction of granite can be bacteria, microscopic algae, fungi, mosses, lichens, higher plants, invertebrates and vertebrates. They often form specific lithobiotic communities that contribute to the destruction of granite-rapakivi. The objects of research were monuments of St. Petersburg (granite sculpture, facades, facing embankments) as well as granite-rapakivi quarries in Russia and Finland, where the stone was quarried for use in St. Petersburg. Sampling was carried out from the most typical biofouling sites. Different methods were applied for the study of damaged granite: petrographic analysis, light and scanning electron microscopy, methods for detection and identification of microorganisms, X-ray microprobe analysis. As result the main forms of granite destruction were described: fractures, ovoid weathering, granular disintegration, surface films, crusts and layers, pitting and fouling. Lichens, mosses, herbaceous and micromycetes were dominated on the granite-rapakivi in quarries. For example, in a Monferran quarry (Virolahti region) the complicated lithobiotic community was revealed. It included 30 species of micromycetes, 31 species of lichens, 10 species of moss. Bacteriological analysis showed the dominance of bacteria Bacillus, and actinomycetes in microbial biofilms. More than 100 species of plants were found on the granite embankments in St. Petersburg. They were confined to the cracks, seams of granite blocks. Plants and mosses were common to the granite embankments of rivers and canals in the central (historical) part of the city. Dimensions of mosses depend on the area of the deepening which they occupy. The most

  8. Charnockites and granites of the western Adirondacks, New York, USA: a differentiated A-type suite

    Science.gov (United States)

    Whitney, P.R.

    1992-01-01

    Granitic rocks in the west-central Adirondack Highlands of New York State include both relatively homogeneous charnockitic and hornblende granitic gneisses (CG), that occur in thick stratiform bodies and elliptical domes, and heterogeneous leucogneisses (LG), that commonly are interlayered with metasedimentary rocks. Major- and trace-element geochemical analyses were obtained for 115 samples, including both types of granitoids. Data for CG fail to show the presence of more than one distinct group based on composition. Most of the variance within the CG sample population is consistent with magmatic differentiation combined with incomplete separation of early crystals of alkali feldspar, plagioclase, and pyroxenes or amphibole from the residual liquid. Ti, Fe, Mg, Ca, P, Sr, Ba, and Zr decrease with increasing silica, while Rb and K increase. Within CG, the distinction between charnockitic (orthopyroxene-bearing) and granitic gneisses is correlated with bulk chemistry. The charnockites are consistently more mafic than the hornblende granitic gneisses, although forming a continuum with them. The leucogneisses, while generally more felsic than the charnockites and granitic gneisses, are otherwise geochemically similar to them. The data are consistent with the LG suite being an evolved extrusive equivalent of the intrusive CG suite. Both CG and LG suites are metaluminous to mildly peraluminous and display an A-type geochemical signature, enriched in Fe, K, Ce, Y, Nb, Zr, and Ga and depleted in Ca, Mg, and Sr relative to I- and S-type granites. Rare earth element patterns show moderate LREE enrichment and a negative Eu anomaly throughout the suite. The geochemical data suggest an origin by partial melting of biotite- and plagioclase-rich crustal rocks. Emplacement occurred in an anorogenic or post-collisional tectonic setting, probably at relatively shallow depths. Deformation and granulite-facies metamorphism with some partial melting followed during the Ottawan phase

  9. 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.

  10. The study of long-term stability in liquid-solid phases for HLW disposal

    International Nuclear Information System (INIS)

    Wei, Y.Y.; Tseng, C.L.; Yang, J.Y.; Ke, C.H.; Wang, T.H.; Jan, Y.L.; Lee, C.B.; Lan, P.L.; Hsu, C.N.; Tsai, S.C.; Li, M.H.; Teng, S.P.

    2005-01-01

    Full text of publication follows: This study is conducted to observe changes in both chemical properties of buffer materials and liquid phases over an experimental period of 2 years. In our experiments, bentonite powder and crushed granite are separately mixed with synthetic groundwater, synthetic seawater and de-ionised water at a fixed liquid-solid ratio of 30. A mixed set with both bentonite and granite together as solid phase is also investigated. During this study, aliquots of the liquid phases are sampled every two months and pH and Eh values are measured immediately. Concentrations of Na, Mg, K, Al, Ca, Ti, Mn, Ba, Fe, Sr, Li and Th are analyzed in the liquid phase directly by ICP-AES. After separation by centrifugation followed by freeze drying and digestion, the solid phases are analyzed as well for elemental composition. Alteration of solid phases during the experimental period is discussed. The preliminary results show that the pH values of the three solutions vary considerably in the individual experimental systems containing bentonite, granite or the mixed system. In general, higher pH values are found in DI-water for all solid phases. Eh values fluctuate a lot in the range 100 to 300 mV in all experiment sets. Different to the experiments with granite for which similar Eh values are found in all solutions, a significantly different Eh-value is found in the experiment with bentonite in DI-water as compared to the other solutions. The results from element analysis indicate that equilibrium is achieved after only two months and element concentrations change only slightly thereafter. We conclude from our experiments that both bentonite and granite keep their characteristics as radionuclide sorbents in the vicinity of a nuclear waste repository. Reaction equilibria appear to be attained rapidly. Because there are just a few alterations in this study, it would be a huge error source in analyzing from the inhomogeneous solid phase such as granite and losses

  11. 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.

  12. 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

  13. 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.

  14. 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

  15. 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

  16. Influence of the properties of granite and sandstone in the desalination process by electrokinetic technique

    DEFF Research Database (Denmark)

    Feijoo, J.; Ottosen, Lisbeth M.; Pozo-Antonio, J.S.

    2015-01-01

    ) achieved in both stones.From the results obtained, it was possible to find those inherent factors to each stone which could have an influence on the efficacy of the treatment. With this technique it was possible to reduce the salt concentration in the granite almost to 100%. However, in the sandstone...... samples the decreases were not equally high, mainly at the intermediate levels where slight enrichments were observed. The results indicate that although the used technique is efficient for salt removal regardless of the porosimetric distribution of the rock, the better interconnection between the pores...... in the granite samples (favored a faster desalination process)....

  17. 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.

  18. 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.

  19. Mobility of heavy metals through granitic soils using mini column infiltration test

    International Nuclear Information System (INIS)

    Zarime, Nur 'Aishah; Yaacob, W. Z.W.

    2014-01-01

    This study is about the mobility of cadmium through compacted granitic soils. Two granitic soils namely the Broga (BGR) and Kajang (KGR) granitic soils were collected in Selangor, Malaysia. Physical and chemical tests were applied for both granitic soils to determine the physical and chemical properties of soil materials. Physical test results shows granitic soils (BGR and KGR) have high percentage of sand ranging between 54%–63% and 46%–54% respectively, an intermediate and intermediate to high plasticity index as well as high specific gravity ie; 2.50–2.59 and 2.45–2.66 respectively. For chemical test, granitic soils shows acidic pH values ranged from 5.35–5.85 for BGR and pH 5.32–5.54 for KGR. For organic matter, SSA and CEC test, it shows low values ranged from 0.22%–0.34% and 0.39%– 0.50% respectively for organic matter test, 17.96 m 2 /g–21.93 m 2 /g and 25.76 m 2 /g–26.83 m 2 /g respectively for SSA test and 0.79 meq/100g–1.35 meq/100g and 1.31 meq/100g–1.35 meq/100g respectively for CEC test. Mini column infiltration test was conducted to determine the retention of cadmium while flowing through granite soils. This test conducted based on the falling head permeability concepts. Different G-force ranging from 231G to 1442G was used in this test. The breakthrough curves show the concentration of Cd becomes higher with the increasing of G-force for both granitic samples (BGR and KGR). The selectivity sorption for both granites ranked in the following decreasing order of; 231G>519G>923G>1442G. Results demonstrated that granitic soils also have low buffering capacity due to low resist of pH changes

  20. 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.

  1. 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.

  2. 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)

  3. 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.

  4. 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...

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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)

  10. 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

  11. Geochemistry and petrogenesis of Proterozoic granitic rocks from ...

    Indian Academy of Sciences (India)

    Geochemistry and petrogenesis of Proterozoic granitic ... This study presents the geochemical characteristics of granitic rocks located on the northern ... Frost and Frost 2013). ...... King P L, White A J R, Chappell B W and Allen C M 1997.

  12. 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...

  13. 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.

  14. 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

  15. 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

  16. Formation of A-type granites in the Lower Yangtze River Belt: A perspective from apatite geochemistry

    Science.gov (United States)

    Jiang, Xiao-Yan; Li, He; Ding, Xing; Wu, Kai; Guo, Jia; Liu, Ji-Qiang; Sun, Wei-Dong

    2018-04-01

    Apatite is ubiquitous in A-type granites, and can be used to elucidate the volatile contents of the silicate melt, which reflect its source characteristics. A-type granites have been recognized as a distinct group of granites. A1- and A2-type subgroups are produced under different extensional settings. However, the details of the mechanisms behind the distinctive geochemical characteristics of A1- and A2-type granites remain obscure. Belts of Cretaceous A1- and A2-type granites occur along the Lower Yangtze River Belt in eastern China. Here we investigated the major and trace element compositions of apatites from contemporary A1- and A2-type granites at different localities along the Lower Yangtze River Belt, in order to decipher their discrepant source processes. Apatites from A1- and A2-type granites show similar major and trace elements, but differ in their F and Cl concentrations. Apatites from A1-type granites in the eastern part of the Lower Yangtze River Belt have much lower F and higher Cl concentrations compared to A2-type granites in the western part. Moreover, from the east to the west, the F concentrations of apatites from A1-type granites increase, while the Cl concentrations decline. In a subducted plate, F is retained by amphibole, chlorite, serpentine and mica minerals through the amphibolite stage, and finally by phengite and lawsonite during the eclogite stage, whereas, Cl is controlled by amphibole, chlorite and serpentine. The high and varied Cl concentrations in A1 subgroup apatites, therefore, may be attributed to the breakdown of amphibole, chlorite and/or serpentine decomposition during partial melting of subducted oceanic crust releasing a large amount of Cl at shallower depth. In contrast, F is transported to deeper depths in the subducted oceanic crust, and released through breakdown of phengite and lawsonite, making an important contribution to the formation of A2-type granites. Apatites from A1- and A2-type granite samples show regular

  17. 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.

  18. Determining heterogeneous deformation for granitic rocks in the northern thrust in Wadi Mubarak belt, Eastern Desert, Egypt

    Science.gov (United States)

    Kassem, Osama M. K.

    2011-05-01

    Finite-strain was studied in the mylonitic granitic and metasedimentary rocks in the northern thrust in Wadi Mubarak belt to show a relationship to nappe contacts between the old granitic and metavolcano-sedimentary rocks and to shed light on the heterogeneous deformation for the northern thrust in Wadi Mubarak belt. We used the Rf/ϕ and Fry methods on feldspar porphyroclasts, quartz and mafic grains from 7 old granitic and 7 metasedimentary samples in the northern thrust in Wadi Mubarak belt. The finite-strain data shows that old granitic rocks were moderate to highly deformed and axial ratios in the XZ section range from 3.05 to 7.10 for granitic and metasedimentary rocks. The long axes (X) of the finite-strain ellipsoids trend W/WNW and E/ENE in the northern thrust in Wadi Mubarak belt. Furthermore, the short axes (Z) are subvertical associated with a subhorizontal foliation. The value of strain magnitudes mainly constants towards the tectonic contacts between the mylonitic granite and metavolcano-sedimentary rocks. The data indicate oblate strain symmetry (flattening strain) in the mylonitic granite rocks. It is suggested that the accumulation of finite strain was formed before or/and during nappe contacts. The penetrative subhorizontal foliation is subparallel to the tectonic contacts with the overlying nappes and foliation was formed during nappe thrusting.

  19. Re-Os molybdenite dating of granite-related Sn-W-Mo mineralization at Hnilec, Gemeric Superunit, Slovakia

    International Nuclear Information System (INIS)

    Kohut, M.; Stein, H.

    2005-01-01

    Re-Os molybdenite ages from the exocontact of the Hnilec granite-greisen body provide temporal constraints for tin, tungsten and molybdenite mineralization in the Gemeric Superunit, Slovakia. Two molybdenite separates were taken from a representative sample of the Sn-W-Mo mineralization at Hnilec and their Re-Os ages of 262.2 ± 0.9 and 263.8 ± 0.8 Ma (2-sigma) are in excellent agreement. The obtained Re-Os molybdenite ages are similar to recent but less precise electron microprobe monazite (276 ± 13 Ma) and U-Pb single zircon (250 ± 18 Ma) ages from the Hnilec granite intrusion, supporting a granite-related greisen origin for the Sn-W-Mo mineralization. Our precise Re-Os molybdenite ages resolve the long time controversy over the timing of high-temperature mineralization in the Gemeric Superunit. These Permian ages eliminate suggestions of an Alpine age. The sulphur isotope composition of the studied molybdenite is δ 34 S (CDT) = 1.71 ± 0.2 %o and is consistent with a magmatic sulphur source. Field observations indicate the lack of a broad contact aureole in the vicinity of the Hnilec granite body. Shallow level granite emplacement in schistose host rocks was accompanied by alteration and formation of tin-tungsten greisen in the upper part of the granite and exocontact molybdenite mineralization, both commonly lacking in other granite bodies within the Gemeric Superunit. (author)

  20. 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).

  1. Chemical and isotopic studies of granitic Archean rocks, Owl Creek Mountains, Wyoming: Geochronology of an Archean granite, Owl Creek Mountains, Wyoming

    International Nuclear Information System (INIS)

    Hedge, C.E.; Simmons, K.R.; Stuckless, J.S.

    1986-01-01

    Rubidium-strontium analyses of whole-rock samples of an Archean granite from the Owl Creek Mountains, Wyo., indicate an intrusive age of 2640 ± 125 Ma. Muscovite-bearing samples give results suggesting that these samples were altered about 2300 Ma. This event may have caused extensive strontium loss from the rocks as potassium feldspar was altered to muscovite. Alteration was highly localized in nature as evidence by unaffected rubidium-strontium mineral ages in the Owl Creek Mountains area. Furthermore, the event probably involved a small volume of fluid relative to the volume of rock because whole-rock δ 18 O values of altered rocks are not distinct from those of unaltered rocks. In contrast to the rubidium-strontium whole-rock system, zircons from the granite have been so severely affected by the alteration event, and possibly by a late-Precambrian uplift event, that the zircon system yields little usable age information. The average initial 87 Sr/ 86 Sr (0.7033 ± 0.0042) calculated from the isochron intercept varies significantly. Calculated initial 87 Sr/ 86 Sr ratios for nine apparently unaltered samples yield a range of 0.7025 to 0.7047. These calculated initial ratios correlate positively with whole-rock δ 18 O values; and, therefore, the granite was probably derived from an isotopically heterogeneous source. The highest initial 87 Sr/ 86 Sr ratio is lower than the lowest reported for the metamorphic rocks intruded by the granite as it would have existed at 2640 Ma. Thus, the metamorphic sequence, at its current level of exposure, can represent no more than a part of the protolith for the granite

  2. Tasmanian tin and tungsten granites - their radiometric characteristics

    International Nuclear Information System (INIS)

    Yeates, A.N.

    1982-01-01

    A radiometric survey of Tasmanian granites has shown, with one exception, that tin and tungsten-bearing granites have high radioactivity, largely owing to increased uranium. Many have a high uranium/thorium ratio as well. Radiometric measurements can also delineate different granite types within composite bodies

  3. Modeling the fate transport of cesium in crushed granite

    International Nuclear Information System (INIS)

    Lee, C.B.; Kuo, Y.M.; Hsu, C.N.; Li, M.H.; Cheng, H.P.; Teng, S.P.

    2005-01-01

    Full text of publication follows: In order to assess the safety of a underground radwaste repository, reactive transport models suitable for evaluating the fate and transport of radionuclides need to be established based on experimental observation and analysis. The goal of this study is to construct adequate models simulating the reactive transport of cesium (Cs) in crushed granite through a systematic analysis, where synthetic groundwater (SGW) and synthetic seawater (SSW) were employed as the liquid phase. To build such models, this study applied N 2 -BET, x-ray diffraction (XRD), polar-microscopy/ auto-radiography, and solid-phase digestion for the analysis of granite, kinetic batch tests for the characterization of sorption/desorption of Cs, and multi-stage advection-dispersion column tests for the determination of major transport processes and the calibration/validation of hypothesized reactive transport models. Based on the results of solid phase analysis and batch tests, a two-site Langmuir kinetic model has been determined capable of appropriately describing Cs sorption/desorption under test conditions. From the results of non-reactive HTO column tests, a mobile/immobile transport model was proposed to capture the major transport processes in our column system. However, the combination of the two-site Langmuir model and the mobile/immobile transport model failed to provide numerical breakthrough curves matching the Cs experimental breakthroughs. It implied that our model needs to be further refined. To achieve this, the setup of our column test needs to be modified first to reduce the volume of column connecting space, so that the effect of extra diffusion/dispersion on breakthroughs would be minimized and major transport characteristics can be clearly revealed. Moreover, more investigations on the reaction mechanisms and transport processes of the reactive transport system must be conducted. (authors)

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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)

  12. U-Pb ages in zircon of some classic granites from the Borborema province

    International Nuclear Information System (INIS)

    Neves, Benjamin Bley de Brito; Basei, Miguel Angelo Stipp; Passarelli, Claudia Regina; Santos, Edilton Jose dos

    2003-01-01

    The Neoproterozoic evolution of the Borborema Province in the east-northeast part of the South American platform exhibits remarkable, much studied granitic plutonism. In 1967 F. F. Almeida and co-workers discriminated a series of granitic typologies as 'Conceicao type', 'Itaporanga type' etc, mostly based upon general geological features and petrographic grounds. This preliminary classification has somehow been maintained in all subsequent papers up to now, despite all the newly observed plutons and the newly generated tectonic, geochemical and isotopic data since then. Samples of these classical types of granites from their type-localities were analyzed geo chronologically using the U-Pb method in zircons in response to the felt needs of the geological community, because previous age-determinations involved less accurate methods. The new data have been added to all other preexisting U-Pb data (from other granitic bodies) obtained over the last decade, making it possible to recognize three main stages of granitic magmatism for the Borborema Province: 650-625 Ma, 580-570 Ma and 545-520 Ma. The last group of dates is closely association with the escape tectonics of the Brasiliano-Pan African collage, which preceded the assembly of the super continental landmass of Western Gondwana. (author)

  13. 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

  14. 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

  15. 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.

  16. Factors affecting neutron measurements and calculations. Part E. Hydrogen content in granite

    International Nuclear Information System (INIS)

    Komatsubara, Tetsuro; Sasa, Kimikazu; Ohshima, Hiroyuki

    2005-01-01

    For evaluation of radiation doses from the atomic bomb at Hiroshima, many systematic measurements have been made of the residual activities of activation products in rocks and concrete. For the Motoyasu Bridge, which is located close to the bomb hypocenter, the depth profile of 152 Eu was measured in a granite core (Hasai et al. 1987; Shizuma et al. 1997). In order to reproduce the depth profile of the activities, it is important to calculate the neutron scattering and absorption (Endo et al. 1999). In this section, the first result of hydrogen analysis by proton-proton elastic recoil coincidence spectrometry for the granite samples is described. (author)

  17. Identification of granite varieties from colour spectrum data.

    Science.gov (United States)

    Araújo, María; Martínez, Javier; Ordóñez, Celestino; Vilán, José Antonio

    2010-01-01

    The granite processing sector of the northwest of Spain handles many varieties of granite with specific technical and aesthetic properties that command different prices in the natural stone market. Hence, correct granite identification and classification from the outset of processing to the end-product stage optimizes the management and control of stocks of granite slabs and tiles and facilitates the operation of traceability systems. We describe a methodology for automatically identifying granite varieties by processing spectral information captured by a spectrophotometer at various stages of processing using functional machine learning techniques.

  18. Portuguese granites associated with Sn-W and Au mineralizations

    OpenAIRE

    Ana M.R. Neiva

    2002-01-01

    In northern and central Portugal, there are different tin-bearing granites. Most of them are of S-type, others have mixed characteristics of I-type and S-type granites and a few are of I-type. Tin-tungsten deposits are commonly associated with Hercynian tin-bearing S-type granites. Some quartz veins with wolframite are associated with an I-type granite, which has a low Sn content. In suites of tin-bearing S-type granitic rocks, Sn content increases as a function of the degree of fractional cr...

  19. 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).

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. On the interaction of granite with Tc(IV) and Tc(VII) in aqueous solution

    International Nuclear Information System (INIS)

    Eriksen, T.E.; Cui, Daquing

    1991-10-01

    The behaviour of technetium in granite-groundwater systems under reducing conditions was investigated. The anion TcO 4 - was reduced to Tc(IV) and simultaneously precipitated as TcO 2 xnH 2 O on the granite surfaces. The electron sources are assumed to be iron oxides and/or iron containing minerals in the granite. The technetium concentration in ground water under repository conditions may be predicted assuming TcO 2 xnH 2 O as the solid phase and TcO(OH) 2 0 and TcO 4 - as the predominant aqueous complexes using a formation constant for TcO(OH) 2 0 of log K = -8.16 and a standard reduction potential E 0 for the reaction TcO 4 - + 3e - + 4H + = TcO 2 xnH 2 O of 0.738 V. The surface related distribution ratio K a for TcO(OH) 2 0 between Stripa granite and ground water is approximately 1 cm based on geometrical surface area. (au)

  6. 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

  7. Study of isotopic desequilibrium of natural radioactive series in granitic environment: Pluton of El Berrocal (Toledo)

    International Nuclear Information System (INIS)

    Hernandez Benitez, A.

    1994-01-01

    This report summarizes the work funded by European Communities with contract '' The Berrocal project: characterization and validation of natural radionuclide migration processes under real conditions in a fissured granitic environment''. The author takes into account the following aspects in his study: isotope of natural radionuclides, sampling methods, analytic methodology and geological characteristics of the area

  8. 2005 dossier: granite. Tome: phenomenological evolution of the geologic disposal

    International Nuclear Information System (INIS)

    2005-01-01

    This document makes a status of the researches carried out by the French national agency of radioactive wastes (ANDRA) about the phenomenological aspects of the geologic disposal of high-level and long-lived radioactive wastes (HLLL) in granite formations. Content: 1 - introduction: ANDRA's research program on disposal in granitic formation; 2 - the granitic environment: geologic history, French granites; 3 - HLLL wastes and disposal design concepts; 4 - identification, characterization and modeling of a granitic site: approach, geologic modeling, hydrologic and hydro-geochemical modeling, geomechanical and thermal modeling, long-term geologic evolution of a site; 5 - phenomenological evolution of a disposal: main aspects of the evolution of a repository with time, disposal infrastructures, B-type wastes disposal area, C-type wastes disposal area; spent fuels disposal area, radionuclides transfer and retention in the granitic environment; 6 - conclusions: available knowledge, methods and tools for the understanding and modeling of the phenomenological evolution of a granitic disposal site. (J.S.)

  9. U-Pb and K-Ar isotopic dating of Sinec (Rimavica) granites (Kohut zone of veporides)

    International Nuclear Information System (INIS)

    Bibikova, E.V.; Grachema, T.V.; Makarov, V.A.

    1988-01-01

    New results of radiometric dating of Sinec (Rimavica) granites by U-Pb and K-Ar method are presented. The K-Ar method (muscovite and biotite) gives the age of 94 m.y., which can be interpreted by tectonics. The U-Pb dating of zircons gave a concordant age of 350±5 m.y., which is a more reliable age than the one obtained from the same samples by Rb-Sr isochrone. The increased age of the Sinec (Rimavica) granites determined by the Sb-Sr method could be caused by the supply of radiogenic Sr from the surrounding older metamorphic rocks to the granites during retrograde metamorphism synchronous with granite autometasomatism. (author). 3 figs., 2 tabs., 15 refs

  10. Study on the behavior of naturally occurring radioactivity originated from heavy minerals in weathering process of granite

    International Nuclear Information System (INIS)

    Nakano, M.; Nakashima, Y.

    1993-01-01

    Mass fraction of biotite and of heavy minerals originally in granite rocks at Naegi granite area are 3% and 1 x 10 -4 %, respectively. Though their values are very small, specific activities of 238 U is 1.3 Bq/g and 80 Bq/g, respectively. Their values are much higher than that of gross granite (0.1 Bq/g). Therefore, they play important roles in the weathering process. Authors separated biotite and heavy minerals from less-weathered and weathered (outcrop, plastic materials) granite samples by using heavy liquid, and determined each specific activities and activity ratios. Furthermore, the surface of heavy minerals were washed in 6 N HCl for 20 minutes. And lost fraction of activity in the heavy minerals was determined. The result suggested that activity around heavy mineral's surface was removed into surroundings or external environment through weathering process. (5 figs.)

  11. Differential rates of feldspar weathering in granitic regoliths

    Science.gov (United States)

    White, A.F.; Bullen, T.D.; Schulz, M.S.; Blum, A.E.; Huntington, T.G.; Peters, N.E.

    2001-01-01

    time. Differential feldspar weathering in the low-permeability Panola bedrock environment is more dependent on relative feldspar solubilities than on differences in kinetic reaction rates. Such weathering is very sensitive to primary and secondary hydraulic conductivities (qp and qs), which control both the fluid volumes passing through the regolith and the thermodynamic saturation of the feldspars. Bedrock permeability is primarily intragranular and is created by internal weathering of networks of interconnected plagioclase phenocrysts. Saprolite permeability is principally intergranular and is the result of dissolution of silicate phases during isovolumetric weathering. A secondary to primary hydraulic conductivity ratio of qs/qp = 150 in the Panola bedrock results in kinetically controlled plagioclase dissolution but thermodynamically inhibited K-feldspar reaction. This result is in accord with calculated chemical saturation states for groundwater sampled in the Panola Granite. In contrast, greater secondary conductivities in the Davis Run saprolite, qs/qp = 800, produces both kinetically controlled plagioclase and K-feldspar dissolution. Faster plagioclase reaction, leading to bedrock weathering in the Panola Granite but not at Davis Run, is attributed to a higher anorthite component of the plagioclase and a wetter and warmer climate. In addition, the Panola Granite has an abnormally high content of disseminated calcite, the dissolution of which precedes the plagioclase weathering front, thus creating additional secondary permeability. Copyright ?? 2001 Elsevier Science Ltd.

  12. 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.

  13. 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

  14. 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

  15. 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

  16. 2005 dossier: granite. Tome: phenomenological evolution of the geologic disposal; Dossier 2005: Granite. Tome evolution phenomenologique du stockage geologique

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2005-07-01

    This document makes a status of the researches carried out by the French national agency of radioactive wastes (ANDRA) about the phenomenological aspects of the geologic disposal of high-level and long-lived radioactive wastes (HLLL) in granite formations. Content: 1 - introduction: ANDRA's research program on disposal in granitic formation; 2 - the granitic environment: geologic history, French granites; 3 - HLLL wastes and disposal design concepts; 4 - identification, characterization and modeling of a granitic site: approach, geologic modeling, hydrologic and hydro-geochemical modeling, geomechanical and thermal modeling, long-term geologic evolution of a site; 5 - phenomenological evolution of a disposal: main aspects of the evolution of a repository with time, disposal infrastructures, B-type wastes disposal area, C-type wastes disposal area; spent fuels disposal area, radionuclides transfer and retention in the granitic environment; 6 - conclusions: available knowledge, methods and tools for the understanding and modeling of the phenomenological evolution of a granitic disposal site. (J.S.)

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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)

  4. 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

  5. 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.

  6. 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.

  7. 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.

  8. Measurement of natural radioactivity in commercial granites and glazing stones from Aswan area, Egypt

    International Nuclear Information System (INIS)

    Ahmad, F.; Shousha, H.A.

    2005-01-01

    Ornamental stones are considered as an important source of the mineral wealth in Egypt. These rocks have characteristics that enable them to be used in decoration as being hard, able to be polished and have low water absorption. A knowledge of radioactivity present in these natural rock samples helps to assess the possible radiological hazards to human health and hence take safety precautions if necessary. For the first time, the natural radioactivity of glazing stones used in granite possessing was measured. The concentration of natural radionuclides U-238, Th-232 and K-40 for eighteen ore and three processed granite samples from Aswan area have been determined using a shielded high purity germanium detector coupled to a computerized multichannel analyzer. Also, the gamma activities of 13 glazing stones, which are used in processing of granite, were measured. The average values of the measured activities for granite were 66.15 ± 4.48, 86.12 ± 5.43 and 1902.03 ± 50.64 Bq/kg and for glazing stones were 44.05 ± 3.54, 51.58 ± 4.44 and 87.55 ± 5.46 Bq/kg for U-238, Th-232 and K-40, respectively. The main absorbed dose rates were 167.04 ± 7.52 and 56.72 ± 7.00 n Gy/h at one meter above the ground level for granite and glazing stones, respectively. The average estimated radium equivalent was 335.75 ± 16.48 and 124.55 ± 11.36 Bq/kg for granite and glazing stones, respectively. This value is comparable with the reported values for many countries (370 Bq/kg). The external hazard index varied from 0.5 ± 0.02 to 1.79 ± 0.09 mGy/y for granite and from 0.042 ± 0.011 to 0.852 ± 0.080 mGy/y for glazing stones. Cs-137 concentration ranged from 0.15 ± 0.07 to 3.31 ± 0.29 Bq/kg for granite and from 0.29 ± 0.02 to 1.49 ± 0.010 Bq/kg for glazing stones. For glazing stones, the measured samples are acceptable for use and safe to the workers in granite processing. The radon exhalation rate for granite samples was calculated using nuclear track detector (CR-39). It was

  9. Petrochemical characteristics of Serra do Meio alkaline granite (Campo Alegre de Lourdes - Bahia State)

    International Nuclear Information System (INIS)

    Matos Maia Leite, C. de; Froes, R.J.B.

    1989-01-01

    The Serra do Meio granite outcrops near the town of Campo Alegre de Lourdes, north-northeast of Bahia State. The granite is intrusive into micachists, which are correlatives of the Salgueiro-Cachoeirinha Group (Early Proterozoic), during early to the syn-tectonic shear phase. The geological setting also comprises a phosphatic rock-bearing carbonatitic complex and gabbroid complexes with one of the main world resources of Fe-Ti-V. The granite mineralogical composition grades from Aegerine-augite alkali-feldspar granite/syenites to Leuco alcali-feldspar granite. The geochemical analysis shows SiO 2 -enrichment (67 to 76%), in alkalis (Na 2 +K 2 O, 7,5 to 12,5%), Nb (up to 680ppm), Zr (up to 2,390ppm), Y (up to 250ppm) e REE (up to 796ppm). The geochemical behaviour is peculiar to alkaline series, denoting a silica-oversaturated, potassium-rich, magma. The chondrite-normalized REE patterns display a first group with smooth slopes from the La to Lu, and a second one with negative slopes. Negative Eu anomalies are displayed in all the patterns. The first group is HREE-enriched, with low fractionation ratios. Samples with milonytic fabrics and higher fractionation ratios are related to the second group, suggesting the interaction of metassomatic fluids and the alkaline magma. Discriminant diagrams for Nb, Y and Rb, coupled with geophysical data, point to an intrusive granite in an extensional within a plate tectonic setting of attenuated continental crust. (author) [pt

  10. 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

  11. 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

  12. A study of selenium and tin sorption on granite and geothite

    International Nuclear Information System (INIS)

    Ticknor, K.V.; McMurry, J.

    1996-01-01

    Sensitivity analyses based on an illustrative performance assessment case study of a disposal concept for nuclear fuel waste have shown that radioisotopes of Se and Sn could have a significant effect on cumulative radioactive dose if they were to be transported through the geosphere without retardation. Static batch sorption methods, coupled with 2 n factorial experimental designs, were used to determine the extent to which Se and Sn can be sorbed by granite and goethite as a function of total dissolved solids concentration, [TDS], natural fulvic acid concentration as dissolved organic carbon, [DOC], pH and, for the studies with Se, the Se concentration, [Se]. Aqueous speciation and the saturation indices of solubility-controlling solid phases were estimated using the speciation code HARPHRQ with the HATCHES thermodynamic database. The experimental results indicated that Se sorption on granite was, low and not affected by changes in [DOC] or [TDS]. Increased [Se] and increased pH decreased sorption. For Se sorption on goethite, the pH range was narrow but indicated that sorption decreased as pH increased. Increased [TDS] and [Se] lowered sorption on goethite, but changes in [DOC] had no effect on sorption. For Sn, increased pH, [TDS] and [DOC] decreased sorption on granite. For Sn sorption on goethite, increased [DOC] resulted in decreased sorption, but differences in [TDS] and pH had little consistent effect on sorption. (orig.)

  13. A study of selenium and tin sorption on granite and goethite

    International Nuclear Information System (INIS)

    Ticknor, K.V.; McMurry, J.

    1996-01-01

    Sensitivity analyses based on an illustrative performance assessment case study of a disposal concept for nuclear fuel waste have shown that radioisotopes of Se and Sn could have a significant effect on cumulative radioactive dose if they were to be transported through the geosphere without retardation. Static batch sorption methods, coupled with 2 n factorial experimental designs, were used to determine the extent to which Se and Sn can be sorbed by granite and goethite as a function of total dissolved solids concentration, (TDS), natural fulvic acid concentration as dissolved organic carbon, [DOC], pH and, for the studies with Se, the Se concentration, [Se]. Aqueous speciation and the saturation indices of solubility-controlling solid phases were estimated using the speciation code HARPHRQ with the HATCHES thermodynamic database. The experimental results indicated that Se sorption on granite was low and not affected by changes in [DOC] or [TDS]. Increased [Se] and increased pH decreased sorption. For Se sorption on goethite, the pH range was narrow but indicated that sorption decreased as pH increased. Increased [TDS] and [Se] lowered sorption on goethite, but changes in (DOC] had no effect on sorption. For Sn, increased pH, [TDS] and [DOC] decreased sorption on granite. For Sn sorption on goethite, increased [DOC] resulted in decreased sorption, but differences in [TDS] and pH had little consistent effect on sorption. (author)

  14. Petrogenesis of the Bosworgey granitic cusp in the SW England tin province and its implications for ore mineral genesis

    Science.gov (United States)

    Ball, T. K.; Basham, I. R.

    1984-01-01

    The Bosworgey granite cusp forms an apical portion of the concealed northern extension of the Tregonning-Godolphin granite ridge. It is characterised by unusually high values of B, P, Mn, Fe, As, Cu, Nb, Ta, Bi, Sn, W, U and S which are present largely as tourmaline, apatite, pyrite, arsenopyrite, chalcopyrite, bismuth, columbite, cassiterite, wolframite and uraninite; and low levels of Zr, Hf, Ti and REE present in zircon, ilmenite and monazite. The granite is classified as Sn and W “specialised” (Tischendorf, 1974) and it belongs to the ilmenite series of Japanese workers. The classification of Chappell and White (1974) (“S” and “I” type granites) is shown to be inapplicable to Cornubian rocks although the Bosworgey samples show characteristics of “S” type granites. The accessory mineral assemblages are typical of high temperature lodes (cassiterite, wolframite, arsenopyrite, chalcopyrite) and the assamblage is concluded to be the cusp analogue of hypothermal lodes produced by extreme differentiation and concentration of volatiles. It is speculated that such granites could provide the parent material for the mesothermal crosscourse mineralisation (pitchblende, bismuth, pyrite, galena, sphalerite).

  15. 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.

  16. Zircon U-Pb geochronology and geochemistry of granites in the Zhuguangshan complex, South China: Implications for uranium mineralization

    Science.gov (United States)

    Zhang, Long; Chen, Zhenyu; Li, Xiaofeng; Li, Shengrong; Santosh, M.; Huang, Guolong

    2018-05-01

    The Zhuguangshan complex, composed of Caledonian, Indosinian, and Yanshanian granites, and Cretaceous mafic dykes, is one of the most important granite-hosted uranium producers in South China. Here we present LA-ICP-MS zircon U-Pb and hornblende 40Ar/39Ar geochronology and whole-rock and biotite geochemistry for the granites in this complex to evaluate the magmatism and its constraints on uranium mineralization. Samples collected from the Fuxi, Youdong, Longhuashan, Chikeng, Qiling, and Sanjiangkou intrusions yield zircon weighted 206Pb/238U ages of 426.7 ± 5.4 Ma, 226.4 ± 3.5 Ma, 225.0 ± 2.7 Ma, 152.2 ± 3.0 Ma, 153.9 ± 2.1 Ma, and 155.2 ± 2.1 Ma, respectively. A new Ar-Ar dating of the hornblende of the diabase from the Changjiang uranium ore field yields a plateau age of 145.1 ± 1.5 Ma. These results coupled with published geochronological data indicate that six major magmatic events occurred in the study area at 420-435 Ma, 225-240 Ma, 150-165 Ma, 140 Ma, 105 Ma, and 90 Ma. Both U-bearing and barren granites occur in this complex, and they display differences in whole-rock and biotite geochemistry. The barren granites show higher Al2O3, CaO, TFMM, Rb, Zr, Ba, SI, Mg#, (La/Yb)N, and Eu/Eu*, but lower SiO2, ALK, Rb, DI, Rb/Sr, and TiO2/MgO than those of the U-bearing granites. Biotites in the U-bearing granites are close to the Fe-rich siderophyllite-annite end member with Fe/(Fe + Mg) ratios higher than 0.66, whereas those in the barren granites are relatively close to the Mg-rich eastonite-phlogopite end member with Fe/(Fe + Mg) ratios uranium ore potential of the granites in the Zhuguangshan complex. The geochemical variations of U-bearing and barren granites can serve as a potential detector for granite-hosted uranium deposits.

  17. Preliminary study on influences of radioactivity of residential granite building materials upon parent mice and their offspring

    International Nuclear Information System (INIS)

    Liang Minyi; Zhang Jinghong; Zhu Weiyun; Li Yinyan; Liang Yongqing; Zhang Songshuan; Zhu Daming; Li Jinlin; Lu Qingpu

    2006-01-01

    Objective: To observe the effects of radioactivity of the residential granite building materials on the survival and fertility of mice. Methods: The radioactivities of A, B, C, and D granite building materials were measured and screened by gamma-ray spectrometer, and then these materials were placed into the mice cages. The residential radon was measured with solid state nuclear track detector's and 24-hour continuous measurement. Ninety-six healthy and ablactated mice were randomly selected and put into the four animal cages with different levels of radioactivity, and fed for 120 days. Mice mated and bred naturally. The fertilities and survivals of P, F 1 , and F 2 generation were observed and analyzed. Results: External exposures in the four mice cages were higher than those from the internal exposure. The differences of rates of pregnancy, abortion, and infertility between the P and F 1 generations had no statistical significance among all the groups after being fed for 120 days (P>0.05). There was significant difference among each group in the fertility of F 1 generation (P< 0.001), and the survival rates of the offspring were decreased with increase of radioactivity in granite building materials (P<0.001). Conclusion: Compared with the residential radon, the gamma rays released from the granite building materials had a greater influence on animals. The study suggested that different granite building materials had different influences on the survival and fertility of mice. (authors)

  18. Study on the environmental movements and distributions of natural radioactive nuclides on the granite area (II)

    International Nuclear Information System (INIS)

    Morishima, Hiroshige; Koga, Taeko

    1999-03-01

    The natural radionuclides as K-40, uranium decay series and thorium decay series etc. are widely distributed on environment, but are not uniformly. These have various forms as the sources of terrestrial environmental γ radiation and of radon and make wide fluctuation seasonal and spatially on the environment. We have selected Ikeda mineral spring district, Shimane pref., Misasa spa district, Tottori pref., Muro district, Hachibuse district, Nara pref. and Arima spa district, Hyogo-pref. for HBRA, and Kawanishi-shi, Hyogo pref. and Higashi-osaka-shi, Osaka pref. as CA. We have carried out the study on the environmental movement and distribution of natural radioactive nuclides containing radon and decay nuclides. Radon measurements have been carried using cup typed radon and thoron monitors, pico-rad method by active charcoal sampling and Pilon scintillation-cell by grub sampling. Accumulated radon monitors have been used with cellulose nitrate as solid state track detector. Rn-222 concentrations in air at Misasa spa ranged 2 - 150 Bq/m 3 outdoor and 8 - 194 Bq/m 3 indoor. Rn-222 concentrations on Misasa district, Asahi district and Takeda district geologically formed from granite strata are high, and those on Osika district and Mitoku district formed from volcanic rocks (Andesite and Basalt) are low level. Rn-222 concentration variations in well water used as drinking water were 2 - 138 Bq/l (mean value 31 Bq/l) and those in ground waters varied from non detectable to 4620 Bq/l (mean 875 Bq/l) on sampling time and places. Mean Rn-222 concentration in the spring water at Arima spa area, Hyogo prefecture is 26 Bq/l at Tansan spring source and the other spring sources are comparatively low level. (J.P.N.)

  19. 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.

  20. 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.

  1. 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.

  2. Sorption of Np (Ⅴ) on Beishan granite fracture filling materials

    International Nuclear Information System (INIS)

    Jiang Tao; Wang Bo; Bao Liangjin; Zhou Duo; Long Haoqi; Song Zhixin; Chen Xi

    2012-01-01

    The sorption behaviors of Np (Ⅴ) on the granite fracture filling materials were studied by batch experiments under anaerobic in Beishan groundwater. The impact of pH of groundwater, CO 3 2- , humic acid and different components of granite fracture filling materials on sorption of Np (Ⅴ) was investigated. The results show that the granite fracture filling materials have strong capacity of Np (Ⅴ) adsorption. The value of K d , for Np (Ⅴ) sorption on the granite fracture filling materials is 843 mL/g. With the increase of pH, the value of K d increases at first and then decreases. K d of Np sorption on granite fracture filling materials in the presence of CO 3 2- and humic acid decreases. The chlorite and feldspar are major contributors to the sorption of Np (Ⅴ) on Beishan granite fracture filling materials. (authors)

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Elemental analysis of granite by instrumental neutron activation analysis (INAA) and X-ray fluorescence analysis (XRF)

    International Nuclear Information System (INIS)

    El-Taher, A.

    2012-01-01

    The instrumental neutron activation analysis technique (INAA) was used for qualitative and quantitative analysis of granite samples collected from four locations in the Aswan area in South Egypt. The samples were prepared together with their standards and simultaneously irradiated in a neutron flux of 7×10 11 n/cm 2 s in the TRIGA Mainz research reactor. Gamma-ray spectra from an hyper-pure germanium detector were analyzed. The present study provides the basic data of elemental concentrations of granite rocks. The following elements have been determined Na, Mg, K, Fe, Mn, Sc, Cr, Ti, Co, Zn, Ga, Rb, Zr, Nb, Sn, Ba, Cs, La, Ce, Nd, Sm, Eu, Yb, Lu, Hf, Ta, Th and U. The X-ray fluorescence (XRF) was used for comparison and to detect elements, which can be detected only by XRF such as F, S, Cl, Co, Cu, Mo, Ni, Pb, Se and V. The data presented here are our contribution to understanding the elemental composition of the granite rocks. Because there are no existing databases for the elemental analysis of granite, our results are a start to establishing a database for the Egyptian granite. It is hoped that the data presented here will be useful to those dealing with geochemistry, granite chemistry and related fields. - Highlights: ► Instrumental neutron activation analysis technique (INAA) was used for qualitative and quantitative analysis of granite. ► The samples were prepared together with their standards and simultaneously irradiated in a neutron flux of 7×10 11 n/cm 2 s in the TRIGA Mainz research reactor. ► Following elements have been determined Na, Mg, K, Fe, Mn, Sc, Cr, Ti, Co, Zn, Ga, Rb, Zr, Nb, Sn, Ba, Cs, La, Ce, Nd, Sm, Eu, Yb, Lu, Hf, Ta, Th and U.

  9. Rare-earth elements in granites: concentration and distribution pattern

    International Nuclear Information System (INIS)

    Galindo, A.C.

    1983-01-01

    The geochemistry of rare earth elements in granites is studied. The rare earth element (REE) distribution pattern in granites is characterized by a smooth curve with decreasing concentrations from La to Lu, and frequently a marked Eu negative anomaly. It seems to exist relationship between granite genesis and its REE pattern, in that bodies of primary (magmatic differentiation) origin always show this negative Eu anomaly, while those bodies generated by crustal anatexis do not show this anomaly. (E.G.) [pt

  10. 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.

  11. Mineralogical Control on Microbial Diversity in a Weathered Granite?

    Science.gov (United States)

    Gleeson, D.; Clipson, N.; McDermott, F.

    2003-12-01

    Mineral transformation reactions and the behaviour of metals in rock and soils are affected not only by physicochemical parameters but also by biological factors, particularly by microbial activity. Microbes inhabit a wide range of niches in surface and subsurface environments, with mineral-microbe interactions being generally poorly understood. The focus of this study is to elucidate the role of microbial activity in the weathering of common silicate minerals in granitic rocks. A site in the Wicklow Mountains (Ireland) has been identified that consists of an outcrop surface of Caledonian (ca. 400 million years old) pegmatitic granite from which large intact crystals of variably weathered muscovite, plagioclase, K-feldspar and quartz were sampled, together with whole-rock granite. Culture-based microbial approaches have been widely used to profile microbial communities, particularly from copiotrophic environments, but it is now well established that for oligotrophic environments such as those that would be expected on weathering faces, perhaps less than 1% of microbial diversity can be profiled by cultural means. A number of culture-independent molecular based approaches have been developed to profile microbial diversity and community structure. These rely on successfully isolating environmental DNA from a given environment, followed by the use of the polymerase chain reaction (PCR) to amplify the typically small quantities of extracted DNA. Amplified DNA can then be analysed using cloning based approaches as well as community fingerprinting systems such as denaturing gradient gel electrophoresis (DGGE), terminal restriction fragment length polymorphism (TRFLP) and ribosomal intergenic spacer analysis (RISA). Community DNA was extracted and the intergenic spacer region (ITS) between small (16S) and large (23S) bacterial subunit rRNA genes was amplified. RISA fragments were then electrophoresed on a non-denaturing polyacrylamide gel. Banding patterns suggest that

  12. Portuguese granites associated with Sn-W and Au mineralizations

    Directory of Open Access Journals (Sweden)

    Ana M.R. Neiva

    2002-01-01

    Full Text Available In northern and central Portugal, there are different tin-bearing granites. Most of them are of S-type, others have mixed characteristics of I-type and S-type granites and a few are of I-type. Tin-tungsten deposits are commonly associated with Hercynian tin-bearing S-type granites. Some quartz veins with wolframite are associated with an I-type granite, which has a low Sn content. In suites of tin-bearing S-type granitic rocks, Sn content increases as a function of the degree of fractional crystallization. Greisenizations of two-mica S-type granites associated with tin-tungsten mineralizations are accompanied by an increase in SiO2, H2O+, Sn, W, Nb, Ta, Rb, Zn, and Pb and decrease in MgO, Na2O, V, Sc,Zr, and Sr. The granite associated with the Jales gold deposit is of S-type and strongly differentiated like the tin-bearing S-type granites, but it has a very low Sn content. During fractional crystallization, Si, Rb, Sn, Pb, Au, As, Sb, and S increase. During increasing degree of hydrothermal alteration of this granite at the gold-quartz vein walls, there are progressive increases in K2O, H2O+, Sn, Cs, Cu, Pb, Au, Sb, As, and S.

  13. Assessment of radioactivity level in granite stones sold to ornamental and building purposes in Brazilian Amazon region (Belem, PA, Brazil): a cross sectional study

    International Nuclear Information System (INIS)

    Queiroz, Y.M.; Santos, R.J.C.; Teixeira, C.E.C.

    2015-01-01

    The aim of this work was evaluate the level of radioactivity in granite sold in the region of Belem (Para, Brazil) using a Geiger-Mueller detector. The results showed that only 5 from 57 samples of 35 types of granite evaluated had count rates above that measured in the background. However, the counting statistics suggests that the measured radiation values in these 5 samples are not due random fluctuations inherent in such measures. (author)

  14. Assessment of radioactivity level in granite stones sold to ornamental and building purposes in Brazilian Amazon region (Belem, PA, Brazil): a cross sectional study

    Energy Technology Data Exchange (ETDEWEB)

    Queiroz, Y.M.; Santos, R.J.C.; Teixeira, C.E.C., E-mail: cecteixeira@pq.cnpq.br [Universidade da Amazonia (UNAMA), Belem, PA (Brazil). Centro de Ciencias Biologicas e da Saude. Lab. de Radiologia

    2015-07-01

    The aim of this work was evaluate the level of radioactivity in granite sold in the region of Belem (Para, Brazil) using a Geiger-Mueller detector. The results showed that only 5 from 57 samples of 35 types of granite evaluated had count rates above that measured in the background. However, the counting statistics suggests that the measured radiation values in these 5 samples are not due random fluctuations inherent in such measures. (author)

  15. Simulation of bentonite colloid migration through granite

    International Nuclear Information System (INIS)

    Rosicka, Dana; Hokr, Milan

    2012-01-01

    Document available in extended abstract form only. Full text of publication follows: Colloidal bentonite particles generate at the interface of buffer and host rock in spent nuclear fuel repository due to an erosion process and migrate through granite by the water flow. Stability of these colloids and their migration possibilities have been studied on account of radionuclide transport possibility as colloid could carry adsorbed radionuclides in groundwater through granite. That is why a simulation of bentonite colloid migration in the surrounding of a repository might be requested. According to chemical condition as ionic strength and pH, the colloidal particles coagulate into clusters and that influence the migration of particles. The coagulation kinetics of natural bentonite colloids were experimentally studied in many articles, for example by light scattering techniques. We created a model of coagulation of bentonite colloids and simulation of a chosen experiment with use of the multicomponent reactive transport equation. The coagulation model describes clustering of particles due to attractive van der Waals forces as result of collision of particles due to heat fluctuation and different velocity of particles during sedimentation and velocity gradient of water flow. Next, the model includes influence of repulsive electrostatic forces among colloidal particles leading to stability of particles provided high surface charge of colloids. In the model, each group of clusters is transported as one solution component and the kinetics of coagulation are implemented as reactions between the components: a shift of particles among groups of particles with similar migration properties, according to size of the clusters of colloids. The simulation of migration of bentonite colloid through granite using the coagulation model was calibrated according to experiment results. On the basis of the simulation, one can estimate the basic processes that occur during bentonite colloid

  16. Contribution to uranium geochemistry in intrusive granites

    International Nuclear Information System (INIS)

    Coulomb, R.

    1959-01-01

    This work aims to define the position of a certain number of French granitic deposits within the field of the geochemistry of granites in general, and of the geochemistry of uranium in particular. The regions concerned are: - 3 French Hercynian ranges, in the Vendee, in Brittany and in the Morvan, - 1 African range, probably precambrian, of the Hoggar. For each range, the petrochemical framework is first of all determined and then the degree of chemical homogeneity of the rocks is evaluated. In the petrochemical groups thus obtained the geochemical behaviour of the uranium is studied. From a point of view of the geochemistry of the granites under investigation, a comparison of the laws of distribution of the major elements in the 4 ranges shows up a convergence of average composition which was not anticipated by geological and petrographic considerations alone. The statistical and geochemical distribution laws of the total uranium as a function of the petrochemical variations are established. A study of the chemical forms of uranium in the rocks has drawn an attention to the qualitative and quantitative importance of the fraction of this uranium soluble in dilute acids. We have therefore reconsidered on the one hand, the laws of distribution of the insoluble uranium, which represents essentially the uranium fixed in crystalline structures (zircon, allanite...), and we have justified on the other hand the interest presented by the soluble uranium: this, although more complex in character, presents a geochemical unity in post magmatic phenomena which makes possible to find a genetic connection between the uraniferous deposits and the intrusive massifs. Finally we have given a plan of the geochemical cycle of uranium, in which we hope to have provided some more accurate data on the igneous phase. (author) [fr

  17. 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.

  18. Effect made by the colloids to the sorption behavior of strontium on granite fracture-fillings

    Science.gov (United States)

    Wang, L.; Zuo, R.

    2017-12-01

    The objective of this study was to investigate the effects made by the colloid to the sorption capacity of colloids in granite fracture-fillings in aqueous solutions. The granite fracture-fillings were collected from three different depth of the research mine in Gansu province. According to the composition of the local soil and groundwater, two colloids were chosen to investigate this sorption process. Batch tests had been investigated at 27° under the air atmosphere as a function of pH(3 11), initial uranium concentration(5 400 mg/L) and water-rock ratio on the sorption of Sr on granite fracture-fillings. The batch experimental results showed that the sorption capacity presented a positive relationship with pH value, which may be caused by the hydrolytic adsorption raised by the reaction between Sr(OH)+ and OH- groups on the surface on the adsorbent. Initial strontium concentration also showed a positive relationship with sorption capacity when the concentration was lower than 200mg/mL, when the concentration was higher than 200mg/ml sorption reached the equilibrium. Sorption percentage showed a positive relationship with water/solid ratios, when the ratio was lower than 1:100 the system got equilibrium. When other experiment parameters were fixed and only the solid-liquid ratio changed, the adsorption capacity increased with the increasing solid-water ratio. The reason was that the total amount of Sr in the adsorption system remained unchanged, the adsorption sites increased with the solid-liquid ratio, and the adsorption capacity increased gradually with the increasing adsorption sites. The experiments data were interpreted in terms of Freundlich and Langmuir isotherms and the data fitted the former better. Equilibrium isotherm studies were used to evaluate the maximum sorption capacity of colloid.

  19. Natural radioactivity in granite stones used as building materials in Iran.

    Science.gov (United States)

    Asgharizadeh, F; Abbasi, A; Hochaghani, O; Gooya, E S

    2012-04-01

    Due to increasing concern about environmental radiological protection, specific radioactivity concentrations of (226)Ra, (232)Th and (40)K in different types of commonly used granite stone samples collected from the Tehran city of Iran have been determined by means of a high-resolution HPGe gamma-spectroscopy system. The activity concentrations of (232)Th, (226)Ra and (40)K in the selected granite samples ranged from 18 to 178, 6 to 160 and 556 to 1539 Bq kg(-1), respectively. The radium equivalent activities (Ra(eq)) are lower than the limit of 370 Bq kg(-1) set by NEA-OECD [Nuclear Energy Agency. Exposure to radiation from natural radioactivity in building materials. Report by NEA Group of Experts. OECD (1979)], except in two samples. The internal hazard indexes have been found well below the acceptable limit in most of the samples. Five samples of investigated commercial granite stones do not satisfy the safety criterion illustrated by UNSCEAR (United Nations Scientific Committee on the Effects of Atomic Radiation. Exposure from natural sources of radiation. Report to the General Assembly (1993). Applying dose criteria recently recommended by the EC [European Commission Report on Radiological Protection Principles Concerning the Natural Radioactivity of Building Materials. Radiation Protection 112 (1999)] for superficial materials, all investigated samples meet the exemption dose limit of 0.3 mSv y(-1).

  20. Microstructural modeling of Vienne granite damage

    International Nuclear Information System (INIS)

    Homand, F.; Hoxha, D.

    2002-01-01

    The microstructural approach in damage modeling, which is presented in this paper describes the evolution of micro-crack geometry as a function of history loading. If the crack geometry is known, the effective properties could then be calculated foe any cracked rock by the mean of a micro-mechanical model. The P L evolution law which is necessary in the describing of crack geometry evolution is hardly based on the crack microscope observation as well as on the theory of fabric tensors. This approach is applied in the modeling of mechanical behaviour of Vienne granite. The result of model simulations are compared with laboratory tests. (author)

  1. Deep fracturation of granitic rock mass

    International Nuclear Information System (INIS)

    Bles, J.L.; Blanchin, R.; Bonijoly, D.; Dutartre, P.; Feybesse, J.L.; Gros, Y.; Landry, J.; Martin, P.

    1986-01-01

    This documentary study realized with the financial support of the European Communities and the CEA aims at the utilization of available data for the understanding of the evolution of natural fractures in granitic rocks from the surface to deep underground, in various feasibility studies dealing with radioactive wastes disposal. The Mont Blanc road tunnel, the EDF Arc-Isere gallerie, the Auriat deep borehole and the Pyrenean rock mass of Bassies are studied. In this study are more particularly analyzed the relationship between small fractures and large faults, evolution with depth of fracture density and direction, consequences of rock decompression and relationship between fracturation and groundwater [fr

  2. GRANITE- A steroscopic imaging Chernkov telescope system

    International Nuclear Information System (INIS)

    Shubnell, M.; Akerlof, C.W.; Cawley, M.F.; Chantell, M.; Fegan, D.J.; Fennell, S.; O'Flaherty, K.S.; Freeman, S.; Frishman, D.; Gaidos, J.A.; Hagan, J.; Harris, K.; Hillas, A.M.; Kerrick, A.D.; Lamb, R.C.; Lappin, T.; Lawrence, M.A.; Levy, H.; Lewis, D.A.; Meyer, D.I.; Mohanty, G.; Punch, M.; Reynolds, P.T.; Rovero, A.C.; Sembroski, G.; Weaverdyck, C.; Weekes, T.C.; Whitaker, T.; Wilson, C.

    1993-01-01

    A second 10 meter class imaging telescope was constructed on Mt. Hopkins, Arizona, the site of the original 10 meter Whipple Cherenkov telescope. The twin telescope system with a 140 meter base line will allow both a reduction in the energy threshold and an improvement in the rejection of the hardonic background. The new telescope started operation in December 1991. With the final completion of the first installation stage (GRANITE I) during spring 92, it is now operating simultaneously with the orginal reflector. We describe in this paper design and construction of the new instrument and demonstrate the capability of the experiment to record coincident events

  3. Uranium-lead age determinations on granitic rocks from the eastern Bushveld Complex

    International Nuclear Information System (INIS)

    Faurie, J.N.

    1978-08-01

    Uranium-lead age determinations were carried out on four types of granitic rocks from the eastern Bushveld Complex. The oldest rocks in the area are gneisses and felsites - 2604 plus minus 100 m.y. old - which form the centre of the Dennilton dome. The Rooiberg felsites could not be dated directly because of the absence of zircon, however a porphyritic granite sill, which shows intrusive relations with the Rooiberg felsites, was dated at 2090 plus minus 40 m.y., an age which can also be regarded as a minimum age for the Rooiberg felsites. No reliable age could be determined for the granophyres because of the large amount of lead-loss reflected in the zircon. The majority of zircons from these granophyres showed a peculiar hieroglyphic texture, a phenomena which has not yet been recorded in literature. The samples collected from the granites gave an age of 1950 plus minus 80 m.y. and thus form part of the Nebo Granite. Attempts have been made to obtain more concordant zircon ages throughout the present study. Although some success was achieved by analysing different size fractions of a zircon population, the non-magnetic fractions gave the most promising results [af

  4. Evaluation of natural radioactivity in some granitic rocks in the state of Parana, Brazil and its use in civil construction

    International Nuclear Information System (INIS)

    Ferreira, Ademar de Oliveira

    2013-01-01

    with the Solid State Nuclear Track Detectors (CR-39) and the sealed can technique, assuming a ventilation rate of 0.5 h -1 and an annual exposure time of 7000 h. The results for this studies show that the annual effective dose ranged from (62 ± 3) μSv.y 1 to (138 ± 1) μSv.y -1 and the internal annual effective dose ranged from (0,39 ± 0,04) μSv.y -1 to (70 ± 4) μSv.y -1 . These values are below the maximum limit of 1 mSv.y -1 suggested by the European Commission of Radiological Protection, meaning that the granitic rocks evaluated can be used without radiological implications since the considered scenario is obeyed. The values obtained for the contribution due to the internal dose ranged from 1 % to 78 % of the values obtained for the respective external dose showing the radon contribution varies strongly with the rock type. The results of the correlations between 222 Rn superficial exhalation rate, 226 Ra activity concentration, density, porosity and major oxides of the samples, showed that, in terms of influence in the emanation fraction of radon, the most important parameter is the density, due to low porosity and similarity in terms of chemical composition amid the studied samples. (author)

  5. The Influence of Temperature on Time-Dependent Deformation and Failure in Granite: A Mesoscale Modeling Approach

    Science.gov (United States)

    Xu, T.; Zhou, G. L.; Heap, Michael J.; Zhu, W. C.; Chen, C. F.; Baud, Patrick

    2017-09-01

    An understanding of the influence of temperature on brittle creep in granite is important for the management and optimization of granitic nuclear waste repositories and geothermal resources. We propose here a two-dimensional, thermo-mechanical numerical model that describes the time-dependent brittle deformation (brittle creep) of low-porosity granite under different constant temperatures and confining pressures. The mesoscale model accounts for material heterogeneity through a stochastic local failure stress field, and local material degradation using an exponential material softening law. Importantly, the model introduces the concept of a mesoscopic renormalization to capture the co-operative interaction between microcracks in the transition from distributed to localized damage. The mesoscale physico-mechanical parameters for the model were first determined using a trial-and-error method (until the modeled output accurately captured mechanical data from constant strain rate experiments on low-porosity granite at three different confining pressures). The thermo-physical parameters required for the model, such as specific heat capacity, coefficient of linear thermal expansion, and thermal conductivity, were then determined from brittle creep experiments performed on the same low-porosity granite at temperatures of 23, 50, and 90 °C. The good agreement between the modeled output and the experimental data, using a unique set of thermo-physico-mechanical parameters, lends confidence to our numerical approach. Using these parameters, we then explore the influence of temperature, differential stress, confining pressure, and sample homogeneity on brittle creep in low-porosity granite. Our simulations show that increases in temperature and differential stress increase the creep strain rate and therefore reduce time-to-failure, while increases in confining pressure and sample homogeneity decrease creep strain rate and increase time-to-failure. We anticipate that the

  6. 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

  7. 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

  8. 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.

  9. 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...

  10. 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...

  11. 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.

  12. Determination of low concentrations of thorium in granites using X-ray fluorescence technique

    International Nuclear Information System (INIS)

    Shigematsu, H.M.; Sato, I.M.; Iyer, S.S.

    1981-03-01

    An analytical method for the accurate determination of low concentrations of thorium in rocks using X-ray fluorescence technique, was developed. A tungsten tube was utilized for the production of X-rays. The samples were prepared in the form of double layer pressed pellets using boric acid as a binding agent. The concentration of thorium was determined by measuring the intensity of the characteristic first order Th L α line. The calibration was carried out with USGS rock standards AGV-1, GSP-1 and G-2. Seven granite rocks samples from Granite Mountains of Wyoming, USA, supplied by Dr. Stuckless. Also were analysed. The results obtained were compared with values obtained in others laboratories using different analytical methods. The analyses show that the thorium is concentrated in accessory minerals and presented a non-uniform distribution, making sampling an important factor in the analysis of thorium. A discussion of the precision and accuracy of the method is presented. (Author) [pt

  13. 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

  14. Gypsum-induced decay in granite monuments in Northwestern Spain

    Directory of Open Access Journals (Sweden)

    Silva Hermo, B.

    2010-03-01

    Full Text Available One of the most common forms of decay in granite monuments is the detachment of the superficial layer of the stone (plaques, plaquettes and scales. Previous studies of granite monuments in the northwest Iberian Peninsula revealed a direct relation between this type of weathering and the presence of calcium sulphate, and a mechanism whereby the salt causes this type of decay was suggested. In the present study, various hypotheses as regards the origin of the gypsum found in granite monuments are proposed. The study involved analysis of the contents of ions soluble in water, the results of X-ray diffraction analyses and the ratios of CaO/SO3 in samples of stone, mortar and deposits collected from different monuments. It was concluded that in most cases the gypsum originated from old paintworks or/and from the joint mortars, although inputs from other sources cannot be discounted, as discussed

    Una de las formas de deterioro más frecuente en los monumentos graníticos es la separación de la capa superficial de la piedra (placas, plaquetas y escamas. En trabajos anteriores centrados en monumentos del noroeste de la Península Ibérica, se constató la relación directa entre esta forma de alteración y la presencia de sulfato de calcio y se propuso el mecanismo a través del cual esta sal provoca este tipo de deterioro. En este trabajo se plantean varias hipótesis acerca del origen del yeso encontrado en monumentos graníticos. Para ello se comparan los contenidos de iones solubilizados en agua, los resultados de difracción de rayos X y las relaciones OCa/SO3 de muestras de piedra, morteros y depósitos recogidas en diferentes monumentos. Se llega a la conclusión de que en la mayor parte de los casos el yeso procede de antiguas pinturas o de revestimientos superficiales y de los morteros de juntas entre sillares, pero no se puede descartar la contribución de otros aportes, los cuales se discuten también en este artículo.

  15. The 'Granite' collegial mission of dialogue. Report

    International Nuclear Information System (INIS)

    Boisson, P.; Huet, Ph.; Mingasson, J.

    2000-06-01

    The aim of the 'Granite' collegial mission of dialogue is to inform the French authorities, associations and population about the project of construction of an underground laboratory for the study of the disposal of high level and long-life radioactive wastes in a granitic environment. The aim of the dialogue was not to select a site but to collect the public reactions and advices about such a project. However, such a dialogue has partially failed because of a misunderstanding of the population about the aims of the mission. However, the mission has collected many point of views and questions which are developed in this report. The first and second chapters recall the process of the mission and its progress, while a third chapter stresses on the questions asked by the public and which concern the fear of nuclear wastes and the incompatibility between the disposal of wastes and the socio-economical development of the region concerned. Thanks to the lessons drawn from this experience, the mission has formulated some recommendations (chapter 4) concerning the need for a better information of the population about any topic in relation with the radioactive wastes. Some complementary information is provided in appendixes. (J.S.)

  16. Warren Hunt to test granite well

    International Nuclear Information System (INIS)

    Harvie, W.

    1996-01-01

    Various theories which purport to explain the existence of the Alberta oil sands, were discussed briefly. One theory, held among others by Warren Hunt, speculates that oil is formed deep in the Precambrian basement and not in the higher sedimentary rock. According to this theory, methane in the crust is the abiogenic product that results from hydrogen reacting with silicon carbide in the lower mantle. As it rises through the fractures, it encounters the microbiota, and hydrogen is stripped away making larger molecules until only bitumen remains. Hunt and other adherents of this theory believe that hydrocarbon reservoirs are replenished as oil is produced, hence there is no end to the world's oil supply. This theory is about to be tested by retesting a granite well near Fort McMurray, which was suspended in September 1994, when funding dried up. Kaleeda Enterprises, owners of the well, believe that the well bottom is currently in a granite pool, and oil will be found by deepening the well to 2,150 metres from the current 1,650 metres. While this is not universally accepted, if true, the abiogenic theory would go a long way towards explaining the origin of the oil sands

  17. Study on the environmental movements and distributions of natural radioactive nuclides on the granite area (III)

    International Nuclear Information System (INIS)

    Morishima, Hiroshige; Koga, Taeko

    2000-03-01

    The natural radionuclides as K-40, uranium decay series and thorium decay series etc. are widely distributed on environment, but are not uniformly. These have influences various forms as the sources of terrecial environmental γ radiation and of radon in to the human life environment and make wide fluctuation seasonal and spatially on the environment. The environmental radiation is higher than that of the other on the west Japan where generally consist rich of granite strata. We deeply appreciate in regard to natural radiation and would carry the studies on the movement and distribution of natural radioactive nuclides on high background radiation area consisted rich granite strata. We have selected and observed on Ikeda mineral spring district Ota-shi Shimane pref., Misasa spa district, Tohaku-gun, Tottori pref. on Chugoku area, Muro district Uda-gun, Hachibuse district, Nafa-shi Nara pref., and Arima spa district, Hyogo-pref., Kawanishi-shi, Hyogo pref. on Kinki area and Masutomi spa, Koma-gun, Yamanashi pref., for HBRA, and Higashi-osaka-shi, Osaka pref., for CA. We have carried out the study on the environmental movement and distribution of natural radioactive nuclides containing radon and decay nuclides, and reported these results on following; (1) Radon measurements have been carried using cup typed radon and thoron monitors which are easy handling in spite of need of long sampling period, pico-rad method by active charcoal sampling and Pilon scintillation-cell with 300 ml volume by grub sampling. Accumulated radon monitors have been used cellulose nitrate (LR-115 type II, Kodak Co.) as solid state track detector. Among these characteristics of radon monitors, though minimum detectable limit of cup method for 3 months sampling is higher than those by the other method, it is able to measure mean Rn-222 concentration for 3 months. Rn-222 concentration by pico-rad method is able to get briefly mean concentration for 24 hours, is small detector and many sample are

  18. The Serra do Carambei Granite - PR and the uraniferous anomalism

    International Nuclear Information System (INIS)

    Pinto-Coelho, C.V.

    1986-01-01

    The Serra do Carambei Granite forms a pluton relatively homogeneous, covering about 33 km 2 , cropping out as an elongate retangular body trending NE-SW, being emplaced in the Cunhaporanga Granitoid Complex. Its characteristics indicates a kind of hololeucocratic granite, equigranular, medium to coarse-grained, consisting predominantly of microperthitic alkali-feldspar, quartz and a small amount of biotite (less than 1%), thus being classified as an alaskite. Chemical data allows a classification in the group of granite with high contents of silica (74-76% Wt. SiO 2 ), dominantly alkaline chemism and hypersolvus character, derived from a parental magma under saturated in water with distinguished features of granitoids from the magnetite series and types I and A granites. The pluton shows important chemical variations due to weathering processes. However detailed chemical studies reveal the presence of anomalous concentrations of trace elements such as U, Sn, Nb, Y, Zr, the Serra do Carambei Granite lacks economically important mineralizations because of the absence of well-developed tardi/pos-magmatic processes that could concentrate them. The SW side of the granite is cut by leucocratic rhyolite dykes that show some radiometric anomalies. These rocks, which are highly diferentiated, were emplaced contemporaneously to the Serra do Carambei Granite. Although petrographic and chronological similarities are found between the uraniferous alaskite of Roessing (Namibia) and the Serra do Carambei Granite anyhow it was not possible to establish any lateral continuity with the uranifeous Pan-African Province. (Author) [pt

  19. Soil Radon In The Nigerian Younger Granites | Dewu | Nigerian ...

    African Journals Online (AJOL)

    ... not had enough time to attain equilibrium with its daughters. In general, the results suggest that with proper control, soil radon measurements over the Younger Granite can be used for uranium exploration in the region. Keywords: Radon, younger granite, soil uranium, half-lifeand thorium. Nigerian Journal of Physics Vol.

  20. Durability of two water repelents applied to granite

    Directory of Open Access Journals (Sweden)

    Rivas, T.

    1998-06-01

    Full Text Available The durability of two water-repellents for granitic stonework was determined. Weathered and sound samples of granites widely used in building construction and restoration in Galicia (NW Spain were treated with water repellents of known efficacy, and then subjected to two artificial weathering tests: prolonged exposure to UV light, and sodium sulphate crystallization cycles. In both tests, but especially in the salt crystallization cycles, both treatments rapidly lost their water-repellency. Furthermore, the hydrophobic layer of water repellent impeded salt mobility, favouring fissuration parallel to the treated surface, which was eventually shed in the form of a plaque.

    Se presentan los resultados de la durabilidad de dos tratamientos de hidrofugación aplicados a rocas graníticas ampliamente utilizados en la construcción de edificios en Galicia (Noroeste de España. Tras la evaluación de la eficacia de dichos tratamientos, cuyos resultados se presentaron en un trabajo anterior, se someten las muestras tratadas a dos ensayos diferentes de envejecimiento acelerado: ciclos de exposición a la luz ultravioleta y ciclos de cristalización de sulfato de sodio. Los productos hidrofugantes muestran una escasa resistencia a ambos ensayos, sobre todo a los ciclos de cristalización de sulfato de sodio; esta débil durabilidad se manifiesta en una rápida pérdida de sus propiedades hidrofugantes. Así mismo, se observa que la presencia de la capa hidrófoba en la piedra funciona como una barrera frente a la movilidad de sales, lo que ocasiona el total desprendimiento de aquella y un fuerte deterioro del material rocoso.

  1. Long-term solute diffusion in a granite block immersed in sea water

    International Nuclear Information System (INIS)

    Jefferies, N.L.

    1988-01-01

    Solute diffusion profiles for Cl - , Br - , F - and SO 4 -- have been measured in a granite block which was immersed in the sea at Falmouth, Cornwall, for 30 years. Leachable concentrations of Cl - and Br - were found to be higher in the block than in quarry samples of granite, which demonstrates that solutes from the sea water have diffused into the block. The Cl - and Br - profiles within the block were flat, implying that equilibrium has been reached between the seawater and granite porewater. The apparent diffusion coefficient and the solute accessible porosity have been estimated from these profiles, and these were used to calculate the intrinsic diffusion coefficient which was then compared with previously obtained laboratory data. Concentration profiles for F - and S0 4 -- indicate that these elements have high concentrations at the margins of the block (to depths of up to 15 cm) and are in the process of diffusing outwards into the surrounding seawater. The initially high porewater concentrations of F - and SO 4 -- in the block are believed to result from weathering of the granite prior to its immersion in the sea, due to the breakdown of primary minerals such as pyrite and the micas. F - and SO 4 -- sorptivity has been estimated from an analysis of the porewater concentration profiles. This preliminary experiment has demonstrated the potential for the measurement of solute migration in granite, as a result of the rock having been immersed in seawater. This work is part of the CEC project MIRAGE (radionuclide migration in the geosphere)- Second phase (1985-89) Research area 'Natural analogues'

  2. 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.

  3. Effects of temperature and sliding rate on frictional strength of granite

    Science.gov (United States)

    Lockner, D.A.; Summers, R.; Byerlee, J.D.

    1986-01-01

    Layers of artificial granite gouge have been deformed on saw-cut granite surfaces inclined 30?? to the sample axes. Samples were deformed at a constant confining pressure of 250 MPa and temperatures of 22 to 845??C. The velocity dependence of the steady-state coefficient of friction (??ss) was determined by comparing sliding strengths at different sliding rates. The results of these measurements are consistent with those reported by Solberg and Byerlee (1984) at room temperature and Stesky (1975) between 300 and 400??C. Stesky found that the slip-rate dependence of (??ss) increased above 400??C. In the present study, however, the velocity dependence of (??ss) was nearly independent of temperature. ?? 1986 Birkha??user Verlag.

  4. 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.

  5. 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.

  6. Chemical characteristics of zircon from A-type granites and comparison to zircon of S-type granites

    Czech Academy of Sciences Publication Activity Database

    Breiter, Karel; Lamarão, C. N.; Krás Borges, R. M.; Dall'Agnol, R.

    1192/195, April (2014), s. 208-225 ISSN 0024-4937 Institutional support: RVO:67985831 Keywords : zircon * A-type granites * S-type granites * Wiborg batholith * Brazil * Krušné hory/Erzgebirge Subject RIV: DD - Geochemistry Impact factor: 4.482, year: 2014

  7. Three-dimensional cooling pattern of a granitic pluton 2. The study of deuteric sub-solidus reactions in the Toki granite, Central Japan

    International Nuclear Information System (INIS)

    Yuguchi, Takashi; Tsuruta, Tadahiko; Nishiyama, Tadao

    2011-01-01

    Petrographical studies examining the development and variations of sub-solidus reactions recorded in the Toki granite represent the three-dimensional cooling pattern of this zoned pluton in Central Japan. Samples collected from 19 boreholes in the Toki granite show characteristics indicative of spatial variations in the extent of the sub-solidus reactions. Exsolution coarsening has produced microperthite, including albite-rich lamellae, in this pluton, while deuteric coarsening has resulted in the formation of patchperthite, myrmekite, and the reaction rim. The extent of the deuteric coarsening reactions can be evaluated from the width and spacing of the albite-rich patch in patchperthite and from the thickness of myrmekite and the reaction rim. The width, spacing, and thickness of these textural features increase systematically with elevation; they also increase gradually in the horizontal inward direction in the western part of the pluton but not in the eastern part of the pluton. The systematic variations in textural development indicate that the Toki granite cooled effectively from the roof and from the western margin during the deuteric coarsening stage. The deuteric coarsening may have occurred at temperatures below 500°C, as indicated by ternary feldspar thermometry. (author)

  8. Total exploitation of an ornamental granite quarry

    Directory of Open Access Journals (Sweden)

    Taboada, J.

    2005-09-01

    Full Text Available In this paper we propose a methodology to estimate the recovery percentage for each of the products which can be obtained from the exploitation of an ornamental granite quarry: block, semiblock, masonry-transverse stone, and the smaller materials that can be used to obtain construction aggregates. This methodology ensures that quarry exploitation is exhaustive, thereby minimising the production of spoils and the consequent negative impact on the environment. The analysis is based on a detailed and exhaustive compilation of discontinuity data from the research fronts, which are then interpreted statistically and projected over the three weakness planes that are a particular feature of ornamental granite deposits. Using this information, and bearing in mind the minimum commercially viable sizes for each kind of granite, the corresponding recovery rates are calculated for each material in each plane. The results are then integrated using spatial techniques, and the result is an evaluation of quarry contents with a view to total exploitation. This methodology was applied to a quarry in the opening phase in order to carry out an a priori assessment of the economic feasibility of the quarry.

    En este trabajo se propone una metodología para estimar el porcentaje de recuperación de cada uno de los productos que se pueden obtener en la explotación de una cantera de granito ornamental: bloque, semibloque, manpostería y per piaños, y material restante destinado a la obtención de áridos. De esta manera se logra un aprovechamiento integral de la cantera, evitándose la generación de estériles y el subsiguiente impacto ambiental producido por éstos. La metodología de análisis se basa en la recopilación detallada y exhaustiva de datos de discontinuidades en los frentes de investigación, que se interpretan estadísticamente y se proyectan sobre los tres planos de debilidad propios del granito ornamental. Con esta información, y las

  9. 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

  10. 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.

  11. The effects of confining pressure and stress difference on static fatigue of granite

    Science.gov (United States)

    Kranz, R. L.

    1980-01-01

    Samples of Barre granite have been creep tested at room temperature at confining pressures up to 2 kbar. Experimental procedures are described and the results of observations and analysis are presented. It is noted that the effect of pressure is to increase the amount of inelastic deformation the rock can sustain before becoming unstable. It is also shown that this increased deformation is due to longer and more numerous microcracks.

  12. The water retention of a granite rock fragments in High Tatras stony soils

    OpenAIRE

    Novák, Viliam; Šurda, Peter

    2010-01-01

    The water retention capacity of coarse rock fragments is usually considered negligible. But the presence of rock fragments in a soil can play an important role in both water holding capacity and in hydraulic conductivity as well. This paper presents results of maximum water holding capacity measured in coarse rock fragments in the soil classified as cobbly sandy loam sampled at High Tatra mountains. It is shown, that those coarse rock (granite) fragments have the maximum retention capacity up...

  13. The Oldest Granites of Russia: Paleoarchean (3343 Ma) Subalkali Granites of the Okhotsk Massif

    Science.gov (United States)

    Kuzmin, V. K.; Bogomolov, E. S.; Glebovitskii, V. A.; Rodionov, N. V.

    2018-02-01

    The Paleoarchean age (3.34 Ga) of subalkali granite magmatism first established for the Kukhtui uplift of the Okhotsk Massif suggests a formation time of the mature continental K-rich crust in this region as early as the Paleoarchean. According to the geological structural, mineralogical-geochemical, geochronological, and isotopic-geochemical data, the Kukhtui uplift can be considered as the most ancient Paleoarchean province in Russia: the ancient consolidation core of the sialic protocrust of the Okhotsk-Omolon Craton.

  14. Example of fracture characterization in granitic rock

    International Nuclear Information System (INIS)

    Thorpe, R.K.

    1981-03-01

    A detailed study of geologic discontinuities for an underground heater test in highly fractured granitic rock is reported. Several prominent shear fractures were delineated within a 6 x 30 x 15 m rock mass by correlating surface mapping and borehole fracture logs. Oblique-reverse faulting is suspected on at least one of the surfaces, and its inferred borehole intercepts appear to be collinear in the direction of slickensiding observed in the field. Four distinct joint sets were identified, one of which coincides with the shear fractures. Another lies nearly horizontal, and two others are steeply inclined and orthogonal. Fracture lengths and spacings for the four joint sets are represented by lognormal probability distributions

  15. Radionuclide sorption on granitic drill core material

    International Nuclear Information System (INIS)

    Eriksen, T.E.; Locklund, B.

    1987-11-01

    Distribution ratios were determined for Sr-85, Cs-134 and Eu-152 on crushed granite and fissure coating/filling material from Stripa mines. Measurements were also carried out on intact fissure surfaces. The experimental data for Sr-85, Cs-134 on crushed material can be accomodated by a sorption model based on the assumption that the crushed material consists of porous spheres with outer and inner surfaces available for sorption. In the case of Eu-152 only sorption on the outer surfaces of the crushed material was observed. The absence of sorption on inner surfaces is most probably due to high depletion of the more strongly sorbed Eu-152 in the water phase and very low diffusivity of Eu-152 in the sorbed state. (orig./HP)

  16. Uranium in granites from the Southwestern United States: actinide parent-daughter systems, sites and mobilization. First year report

    Energy Technology Data Exchange (ETDEWEB)

    Silver, L T; Williams, I S; Woodhead, J A

    1980-10-01

    Some of the principal findings of the study on the Lawler Peak Granite are: the granite is dated precisely by this work at 1411 +- 3 m.y., confirming its synchroneity with a great regional terrane of granites. Uranium is presently 8-10 times crustal abundance and thorium 2-3 times in this granite. Uranium is found to be enriched in at least eight, possibly ten, primary igneous mineral species over the whole-rock values. Individual mineral species show distinct levels in, and characteristics ranges of, uranium concentration. It appears that in a uraniferous granite such as this, conventional accuracy mineral suites probably cannot account for most of the uranium in the rock, and more rare, high U-concentration phases also are present and are significant uranium hosts. It appears that at least two different geological episodes have contributed to the disturbance of the U-Th-Pb isotope systems. Studies of various sites for transient dispersal of uranium, thorium, and radiogenic lead isotopes indicate a non-uniform dispersal of these components. It appears that the bulk rock has lost at least 24 percent of its original uranium endowment, accepting limited or no radiogenic lead or thorium migration from the sample.

  17. Uranium in granites from the Southwestern United States: actinide parent-daughter systems, sites and mobilization. First year report

    International Nuclear Information System (INIS)

    Silver, L.T.; Williams, I.S.; Woodhead, J.A.

    1980-10-01

    Some of the principal findings of the study on the Lawler Peak Granite are: the granite is dated precisely by this work at 1411 +- 3 m.y., confirming its synchroneity with a great regional terrane of granites. Uranium is presently 8-10 times crustal abundance and thorium 2-3 times in this granite. Uranium is found to be enriched in at least eight, possibly ten, primary igneous mineral species over the whole-rock values. Individual mineral species show distinct levels in, and characteristics ranges of, uranium concentration. It appears that in a uraniferous granite such as this, conventional accuracy mineral suites probably cannot account for most of the uranium in the rock, and more rare, high U-concentration phases also are present and are significant uranium hosts. It appears that at least two different geological episodes have contributed to the disturbance of the U-Th-Pb isotope systems. Studies of various sites for transient dispersal of uranium, thorium, and radiogenic lead isotopes indicate a non-uniform dispersal of these components. It appears that the bulk rock has lost at least 24 percent of its original uranium endowment, accepting limited or no radiogenic lead or thorium migration from the sample

  18. 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...

  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. Investigating the effect of using granite and marble as a building material on the radiation exposure of humans

    International Nuclear Information System (INIS)

    Ebaid, Y. Y.; Bakr, W. F.

    2012-01-01

    The aim of this study was to comprehensively study the radiological hazards of granite and marble used as a building material in Egypt. The activity concentrations of 226 Ra, 232 Th and 40 K were determined using high-resolution hyper-pure germanium detectors in 25 samples of different types of commercially available granite and marble. The measured activity concentrations for these natural radionuclides were compared with the reported data for Egypt and other countries. In order to assess the radiological impact, the radiation hazard parameters such as radium equivalent activity (Ra eq ) and hazard level index (γ) were calculated. The internal and external dose rates due to natural radionuclides in granite and marble were also calculated. The data obtained were considered as helpful in regulating the use of building materials in Egypt. (authors)

  2. Study of the incorporation of marble and granite wastes in the raw material to produce glass wool

    International Nuclear Information System (INIS)

    Rodrigues, Girley Ferreira; Junca, Eduardo; Telles, Victor Bridi; Espinosa, Denise Crocce Romano; Tenorio, Jorge Alberto Soares; Alves, Joner Oliveira

    2010-01-01

    The study aimed to characterize materials obtained from the melted mixture containing marble and granite wastes, and also chemical reagents. Using the characterization results was defined the feasibility of reuse of the marble and granite wastes, through the incorporation in the raw material to produce glass wool (a material with great consumer market as thermo-acoustic insulator). The batch was poured in a water-filled recipient and also in a Herty viscometer at temperatures of 1400, 1450 and 1500 °C. Samples of produced materials were characterized by morphology using Scanning Electron Microscopy, by atomic structure using X-ray Diffraction, and by thermal behavior using Differential Thermal Analysis. The total amount of marble and granite wastes can reach about 79% replacement in relation to the total weight of the raw material used in the glass wool production. (author)

  3. Sm-Nd isotope system of the Ukrainian shield (Korosten'sky massif) anorthosite-granite formation

    Energy Technology Data Exchange (ETDEWEB)

    Bogatikov, O A; Karpenko, S F; Sukhanov, M K; Spiridonov, V G

    1988-01-01

    The results of Sm-Nd isotope investigation of rocks of the Ukrainian shield anorthosite-granite association are described; this association, according to the geologic data, is the latest association in a seriesof self-contained anorthosited. The latters are connected with considerable masses of rapakiwi-granited. Isotope analysis is carried out by mass spectrometry. Isotope ratios /sup 147/Sm//sup 144/Nd and /sup 143/Nd//sup 144/Nd for five samples investigated are presented. Isotope data obtained are marked to be important information about the origin of rocks studied. Evident age difference of granite and basic components of the association is established, that idnores the possibility of the rock formation during crystallization differentiation. The basic value of the radiometric 1.89-1.74 milliared years age of the Ukrainian shield anorthosites lied in the fact that these data confirm once more the specific nature of the earth's crust evolution especially at early stages of its formation.

  4. 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.)

  5. The source rock characters of U-rich granite

    Energy Technology Data Exchange (ETDEWEB)

    Mingyue, Feng; Debao, He [CNNC Key Laboratory of Uranium Resources Exploration and Evaluation Technology, Beijing Research Institute of Uranium Geology (China)

    2012-03-15

    This paper discusses the stratum composition, lithological association, uranium content of crust and the activation, migration, concentration of uranium at each tectonic cycle in South China. The authors point out that the source rock of U-rich granite is U-rich continental crust which is rich in Si, Al and K. The lithological association is mainly composed of terrestrial clastic rocks formation of mudstone and sandstone, mingled with intermediate-acidic, mafic pyroclastic rocks and carbonate rocks formation. During tectonic movements, the rocks had undergone regional metamorphism, migmatitization, granitization, and formed U-rich granites finally. (authors)

  6. The source rock characters of U-rich granite

    International Nuclear Information System (INIS)

    Feng Mingyue; He Debao

    2012-01-01

    This paper discusses the stratum composition, lithological association, uranium content of crust and the activation, migration, concentration of uranium at each tectonic cycle in South China. The authors point out that the source rock of U-rich granite is U-rich continental crust which is rich in Si, Al and K. The lithological association is mainly composed of terrestrial clastic rocks formation of mudstone and sandstone, mingled with intermediate-acidic, mafic pyroclastic rocks and carbonate rocks formation. During tectonic movements, the rocks had undergone regional metamorphism, migmatitization, granitization, and formed U-rich granites finally. (authors)

  7. Design of a dosimetric evaluation protocol workers granite quarries

    International Nuclear Information System (INIS)

    Guillen, J.; Tejado, J. J.; Baeza, A.

    2011-01-01

    The Autonomous Community of Extremadura is one of the major regions of Spain as far as the extraction of granite and further processing of products derived from it are concerned. One of the most industrialized areas of the sector presents a serious problem for non-radiological occupational health of workers, particularly silicosis. Since in this area of activity levels of granites can be classified as medium-high within the precipitates ranges, the question is whether in addition to this occupational disease, there is a radiological impact associated with the activity NORM extraction and manufacturing of granite.

  8. 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.

  9. 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).

  10. 2005 dossier: granite. Tome: phenomenological evolution of the geologic disposal; Dossier 2005: Granite. Tome evolution phenomenologique du stockage geologique

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2005-07-01

    This document makes a status of the researches carried out by the French national agency of radioactive wastes (ANDRA) about the phenomenological aspects of the geologic disposal of high-level and long-lived radioactive wastes (HLLL) in granite formations. Content: 1 - introduction: ANDRA's research program on disposal in granitic formation; 2 - the granitic environment: geologic history, French granites; 3 - HLLL wastes and disposal design concepts; 4 - identification, characterization and modeling of a granitic site: approach, geologic modeling, hydrologic and hydro-geochemical modeling, geomechanical and thermal modeling, long-term geologic evolution of a site; 5 - phenomenological evolution of a disposal: main aspects of the evolution of a repository with time, disposal infrastructures, B-type wastes disposal area, C-type wastes disposal area; spent fuels disposal area, radionuclides transfer and retention in the granitic environment; 6 - conclusions: available knowledge, methods and tools for the understanding and modeling of the phenomenological evolution of a granitic disposal site. (J.S.)

  11. Optically stimulated luminescence (OSL) and some other luminescence images from granite slices exposed with radiations

    International Nuclear Information System (INIS)

    Hashimoto, T.; Notoya, S.; Ojima, T.; Hoteida, M.

    1995-01-01

    Optically stimulated luminescence (OSL) images of some X- and γ-irradiated granite slices were obtained using photon detection through a 570 nm bandpass filter with diode-laser excitation of 910 nm. Alternative photo-induced phosphorescence (PIP) images, which were colour photographed immediately after the sunlight exposure of slice samples, were also found to be helpful in the observation of the luminescence properties and to filter selection for OSL measurements. These OSL and PIP images were compared with some other colour luminescence images, including thermoluminescence images (TLCI) and after-glow images (AGCI). It was obvious that there exists a variety of coloured emissions derived mainly from feldspar constituents and these were found to be dependent on the geological history or metamorphism of the granites. (Author)

  12. Study of the mineralogical transformations of granite by underground nuclear explosions

    International Nuclear Information System (INIS)

    Faure, Jean

    1970-01-01

    The object of the following communication is to prove new data about the petrographic effects of the underground nuclear explosions. It is founded on the results of trench tests in granite rock. The samples are collected by drilling and the temperature of the rock was measured in the hole. Four types of melted rocks can be sorted, grey-green glass and pumices, beige to red-brown pumices, dark lavas, dark veinlets and crushed granite. The distribution of these rocks is studied. Optical microscopy, X-rays and chemical analysis, study by electron probe, are made. The results complete previously published data. They are interesting as far as the use of nuclear explosions for industrial applications is concerned. (author)

  13. The origin of groundwater salinity in granitic rocks: identification and characterisation of chloride sources

    International Nuclear Information System (INIS)

    Savoye, Sebastien

    1998-01-01

    This research thesis aims at clearly identifying the possible origins of chlorine in solution in underground waters in a granitic environment, and is thus a first step in the prediction of concentration of dissolved compounds in waters in crystalline environment, with respect to the geological context. In a first part, the author proposes a synthetic and critical overview of knowledge and previous studies: definition of the term 'salinity', presentation of geochemical tracers, presentation of available data on potential chlorine sources in granitic rocks. The author then describes the experimental protocols and studied sites, reports results of the characterisation of different chlorine tanks performed on samples from each studied site. Based on mass assessment calculations and on the use of tracers, the author finally discusses the contribution of each of the chlorine tanks to the salinity of underground waters [fr

  14. Determination of rare-earth elements content in granitic rocks by argon plasma emission spectrometry

    International Nuclear Information System (INIS)

    Merodio, J.C.; Martinez, J.M.

    1990-01-01

    A method has been developed that enables the rare-earth elements in granitic rocks to be measured sequentially, using an inductively coupled plasma (ICP) source spectrometer with medium spectral resolution (0,02nm). The rocks were dissolved in an open system with a mixture of nitric-hydrofluoric-perchloric acids. Any residues remaining at this stage were removed by filtration and digested using a mini-fusion method with lithium tetraborate. Prior to the excitation in the spectrometer the rare-earth group was separated from other constituents using cation-exchange chromatography. A detailed study of spectral interferences and the evaluation of the detection limits have been performed. Five geochemical reference sample (granitic rocks) were analyzed and the obtained results agree favourably with recommended values and with reported determinations, using high spectral resolution ICP spectrometry. (Author) [es

  15. Study of the mineralogical transformations of granite by underground nuclear explosions

    Energy Technology Data Exchange (ETDEWEB)

    Faure, Jean [Commissariat a I' Energie Atomique, Centre d' Etudes de Bruyeres-le-Chatel (France)

    1970-05-15

    The object of the following communication is to prove new data about the petrographic effects of the underground nuclear explosions. It is founded on the results of trench tests in granite rock. The samples are collected by drilling and the temperature of the rock was measured in the hole. Four types of melted rocks can be sorted, grey-green glass and pumices, beige to red-brown pumices, dark lavas, dark veinlets and crushed granite. The distribution of these rocks is studied. Optical microscopy, X-rays and chemical analysis, study by electron probe, are made. The results complete previously published data. They are interesting as far as the use of nuclear explosions for industrial applications is concerned. (author)

  16. Alpha particles emitted from the surface of granite, clay, and its fired products, 1

    International Nuclear Information System (INIS)

    Aratani, Michi; Otsuka, Hideko

    1975-01-01

    As a part of an investigation on ''the effect of long-time irradiation from a trace amount of radioisotopes'', the emitting rate of alpha particles per unit surface area (apparent) coming from natural alpha-particle emitters has been measured. The samples measured were granite and its weathered product; clay, especially potter's clay, and its fired product; pottery ware. The values obtained were 39.1 +-0.9--0.73+-0.08 cpm/100 cm 2 in granite, 16.8+-0.4--6.4+-0.2 cpm/100cm 2 in potter's clay, and 1.36+-0.04--0.82+-0.04 cpm/100cm 2 in pottery ware on substrate, and 1.33+-0.05--0.32+-0.02 cpm/100cm 2 on glazer. (auth.)

  17. Gas chromatography applied to cultural heritage. Analysis of dark patinas on granite surfaces.

    Science.gov (United States)

    Aira, N; Jurado, V; Silva, B; Prieto, B

    2007-04-13

    The formation of dark patinas has been mainly related with deposition of gases and particles, and sulphation mechanisms particularly in calcareous rocks. However, in granitic monuments located in Galicia (northwest of Spain), especially in rural areas, this origin is unlikely since granite is a very poor calcium-containing rock and the atmospheric pollution in this area is negligible. A biological origin seems to be most probable. In order to know the importance of biological and atmospheric factors in the formation of dark patinas on granitic monuments, a number of analyses using several techniques are needed. The characterization of fatty acids in patinas by gas chromatography has established clear differences among samples. Thus, all of the samples having a biological origin displayed a similar fatty acid pattern, with unsaturated fatty acids predominating, especially oleic and linoleic acids; these were followed in abundance by the branched fatty acid 18:00 anteiso, and palmitic acid. Different patterns of fatty acid allowed establishment of an anthropogenic origin of the some of the patinas analysed.

  18. [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.

  19. 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

  20. Thermal cracking in Lac du Bonnet granite during slow heating to 205 degrees celsius

    International Nuclear Information System (INIS)

    Chernis, P.J.; Robertson, P.B.

    1993-09-01

    Acoustic emissions (AE) were recorded as drill core samples of Lac du Bonnet granite were slowly heated to between 66 and 205 degrees celsius to evaluate the effects of temperature on the properties of rock samples. Longitudinal and shear velocities of the samples were measured, and Young's moduli, shear moduli and Poisson's ratios were calculated. No significant AE activity was detected until temperatures reached approximately 73-80 degrees celsius. Above this 'threshold' temperature, calculated rock properties decreased, and at 205 degrees celsius calculated Young's modulus, shear modulus, and Poisson's ratio were reduced by 30, 26, and 29% respectively

  1. Characterization of microbial communities in deep groundwater from granitic rock

    International Nuclear Information System (INIS)

    Jain, D.K.; Stroes-Gascoyne, S.; Providenti, M.; Tanner, C.; Cord, I.

    1997-01-01

    The microbial characteristics of deep granitic nutrient-poor groundwater from two boreholes at the Underground Research Laboratory of Atomic Energy of Canada Limited were studied. Scanning electron microscopy of the groundwater samples revealed significant numbers of bacteria of various sizes and shapes, including spherical, rod, and curved shaped. A few bacteria with appendages were also observed. Significant numbers of bacteria (∼l0 5 /mL) were enumerated using acridine orange (AO) staining. An active microbial population was detected with three direct methods and it ranged from 1 to 83% of the AO count, depending on the method used. Culturable aerobic and anaerobic (including facultative) heterotrophic bacteria ranged from 0.06 to 10.2% and 0.008 to 7.35%, respectively, of the AO count. Denitrifying. N 2 - fixing, sulphate-reducing, and iron-precipitating bacteria were present, but no iron-oxidizing bacteria or methanogens could be detected. Tentative identification of 160 isolates using the Biolog system showed a predominance of three Pseudomonas species, P. fluorescens, P. marginalis, and P. corrugata. Phospholipid fatty acid analysis showed that the bacteria in the groundwater samples faced starvation stress. However, laboratory studies showed that these bacteria can efficiently uptake and mineralize organic substrates when supplied. (author)

  2. Musa's granite and Rio Maria's granodiorite Rb/Sr isotopic ages and geochemistry

    International Nuclear Information System (INIS)

    Gastal, M.C.P.; Macambira, M.J.B.; Medeiros, H.; Dall'Agnol, R.

    1987-01-01

    The Musa Granite and the Rio Maria Granodiorite are located at the eastern margin of the Amazonian craton, in the Rio Maria region, where a typical granite-greenstone terrain is characterized. Rb-Sr dating of six samples from different facies of Rio Maria Granodiorite furnished an age of 2564 ± 68 Ma with initial 87 Sr/ 86 Sr radio (IR) of 0.70288 ± 0.00092 (whole rock isochron; 1 ο error; MSWD = 2.26). Thirteen samples from the three facies of Musa Granite (monzogranites, syenogranites and intermediate to felsic hypabyssal rocks) gave Rb-Sr whole rock isochron with an age of 1692 ± 11 Ma and IR of 0.70777 ± 0.00023 (1 ο error, MSWD = 1.89). A preliminary attempt to individualize geochronologically the three facies was done resulting different ages and IRs. There is a coincidence between these ages and the emplacement sequence of these facies of the pluton. The actual meaning of the Rio Maria Granodiorite Rb-Sr age is still uncertain. It could be related to the end of the magmatic crystallization of the batholith as well as to the metamorphic-mylonitic event that affect it. Considering that the Jamon and Musa Granites are petrologically similar that they occur in the same area, it is interesting to note that latter is apparently a little older than the former. The IRs obtained for the two plutons are also not coincident. The isotopic Rb-Sr available data show that the exposed rocks of the Rio Maria Granodiorite have not been able to generate magmas with the compositions of the monzongranitic and the hypabyssal facies of the Musa pluton. On the other hand, rocks isotopically similar to the Rio Maria Granodiorite would theorically be able to generate the Jamon and a magma with the characteristics of the syenogranitic facies of the Musa pluton. (author) [pt

  3. Engineering Geological Properties of Oil-Contaminated Granitic and Meta sedimentary Soils

    International Nuclear Information System (INIS)

    Zulfahmi Ali Rahman; Umar Hamzah; Noorulakma Ahmad

    2011-01-01

    Hydrocarbon is a light-non aqueous phase liquid or known as LNAPL. It poses environmental hazard if accidentally spilled out into the soil and water systems as a result of its insoluble nature in water. LNAPL component infiltrates into soil through pore spaces and afloat at the top of groundwater level. Some of this hydrocarbon would trap and clog within the voids, difficult to remove and costly to clean. The occurrence of hydrocarbon in the soil definitely degraded the behaviour of soils in terms of engineering properties. This study aimed to investigate the engineering properties of oil-contaminated soil for two different residual soils originally developed from in-situ weathering of granitic and meta sedimentary rocks. The physical characterisations of the soil were determined including particle size distribution, specific gravity test and x-ray diffraction (XRD). The engineering parameters for the contaminated and uncontaminated soils were Atterberg limits, compaction and soil shear strength (UU tests). The amounts of hydrocarbon added to soil were varied at 0 %, 4 %, 8 %, 12 % and 16 % of dried weight of soil samples. The results from the particle size distribution analysis showed that residual soil from granitic rock comprises of 38 % sand, 33 % silt and 4 % clay while meta sedimentary soil consists of 4 % sand, 43 % silt dan 29 % clay. The mean values of specific gravity for the granitic and meta sedimentary soils were 2.56 and 2.61, respectively. The types of minerals present in granitic soil sample were quartz, kaolinite and gibbsite while meta sedimentary soil consists of quartz and kaolinite. The Atterberg limits value decreased as a result of increasing amount of added hydrocarbon into the soil. A similar behavior was observed with the values of maximum dry density and optimum water content with increasing hydrocarbon content. The overall unconsolidated undrained shear strength, C u showed a decreasing trend with the increase in hydrocarbon content

  4. Laboratory Investigation on Physical and Mechanical Properties of Granite After Heating and Water-Cooling Treatment

    Science.gov (United States)

    Zhang, Fan; Zhao, Jianjian; Hu, Dawei; Skoczylas, Frederic; Shao, Jianfu

    2018-03-01

    High-temperature treatment may cause changes in physical and mechanical properties of rocks. Temperature changing rate (heating, cooling and both of them) plays an important role in those changes. Thermal conductivity tests, ultrasonic pulse velocity tests, gas permeability tests and triaxial compression tests are performed on granite samples after a heating and rapid cooling treatment in order to characterize the changes in physical and mechanical properties. Seven levels of temperature (from 25 to 900 °C) are used. It is found that the physical and mechanical properties of granite are significantly deteriorated by the thermal treatment. The porosity shows a significant increase from 1.19% at the initial state to 6.13% for samples heated to 900 °C. The increase in porosity is mainly due to three factors: (1) a large number of microcracks caused by the rapid cooling rate; (2) the mineral transformation of granite through high-temperature heating and water-cooling process; (3) the rapid cooling process causes the mineral particles to weaken. As the temperature of treatment increases, the thermal conductivity and P-wave velocity decrease while the gas permeability increases. Below 200 °C, the elastic modulus and cohesion increase with temperature increasing. Between 200 and 500 °C, the elastic modulus and cohesion have no obvious change with temperature. Beyond 500 °C, as the temperature increases, the elastic modulus and cohesion obviously decrease and the decreasing rate becomes slower with the increase in confining pressure. Poisson's ratio and internal frictional coefficient have no obvious change as the temperature increases. Moreover, there is a transition from a brittle to ductile behavior when the temperature becomes high. At 900 °C, the granite shows an obvious elastic-plastic behavior.

  5. 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.)

  6. Extreme alkali bicarbonate- and carbonate-rich fluid inclusions in granite pegmatite from the Precambrian Rønne granite, Bornholm Island, Denmark

    Science.gov (United States)

    Thomas, Rainer; Davidson, Paul; Schmidt, Christian

    2011-02-01

    Our study of fluid and melt inclusions in quartz and feldspar from granite pegmatite from the Precambrian Rønne granite, Bornholm Island, Denmark revealed extremely alkali bicarbonate- and carbonate-rich inclusions. The solid phases (daughter crystals) are mainly nahcolite [NaHCO3], zabuyelite [Li2CO3], and in rare cases potash [K2CO3] in addition to the volatile phases CO2 and aqueous carbonate/bicarbonate solution. Rare melt inclusions contain nahcolite, dawsonite [NaAl(CO3)(OH)2], and muscovite. In addition to fluid and melt inclusions, there are primary CO2-rich vapor inclusions, which mostly contain small nahcolite crystals. The identification of potash as a naturally occurring mineral would appear to be the first recorded instance. From the appearance of high concentrations of these carbonates and bicarbonates, we suggest that the mineral-forming media were water- and alkali carbonate-rich silicate melts or highly concentrated fluids. The coexistence of silicate melt inclusions with carbonate-rich fluid and nahcolite-rich vapor inclusions indicates a melt-melt-vapor equilibrium during the crystallization of the pegmatite. These results are supported by the results of hydrothermal diamond anvil cell experiments in the pseudoternary system H2O-NaHCO3-SiO2. Additionally, we show that boundary layer effects were insignificant in the Bornholm pegmatites and are not required for the origin of primary textures in compositionally simple pegmatites at least.

  7. Tectonic imprints within a granite exposed near Srinagar, Rajasthan ...

    Indian Academy of Sciences (India)

    Partial melting in the middle to lower crustal level produces melts of granitic composition ..... of D1G generations with a steep easterly dipping limb and gently westerly ..... The great circles represent the average fracture orientation for each set.

  8. On the sources of uranium in some Scottish Caledonian granites

    International Nuclear Information System (INIS)

    Halliday, A.N.

    1982-01-01

    The lead isotope systematics, zircon uranium concentrations and whole-rock rubidium concentrations of 11 Scottish Caledonian granites are examined for clues to the origin of their uranium. A positive correlation between U in zircon and initial lead isotope ratios suggests that U and Pb were derived from the same source which, as some of these granites contain their U in inherited zircons, is likely to have been within the crust. It is argued, therefore, that most of the uranium in these granites had a crustal derivation but lead isotope ratios indicate that any Lewisian contribution was minor in comparison with those from postulated Grenville, Morarian or Caledonian metamorphic reservoirs. However, additional data are required before this conclusion can be extended to include uraniferous Caledonian granites such as Cairngorm. (author)

  9. Characteristics of pegmatoidal granite exposed near Bayalan, Ajmer ...

    Indian Academy of Sciences (India)

    near Bayalan, Ajmer district, Rajasthan. Nilanjan ... eastern flank of the South Delhi Fold Belt (Sinha. Roy 1984 .... gneisses in a lit-par-lit manner producing alternate layers of granite and ... shows a point concentration (table 1) with a mean.

  10. 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.

  11. Granite-related hypothermal uranium mineralization in South China

    International Nuclear Information System (INIS)

    Liu, X.; Wu, J.; Pan, J.; Zhu, M.

    2014-01-01

    As one of the important geological types, granite-related uranium deposits account for about 29% of the total discovered natural uranium resources in China. Most of the granite-related uranium deposits located in Taoshan - Zhuguang uranium metallogenic belt, South China. In addition to the typical pitchblende vein-type uranium mineralization of epithermal metallogenic system, a new type of granite-related uranium mineralization with characteristics of hypothermal matallogenic system was discovered in South China by current studies. However, hypothermal is contact thermal to epithermal mineralization, and not the conventional intrusive high temperature mineralization. Hypothermal uranium mineralization is presented by disseminated uraninite or pitchblende stockwork in fissures in granites normally with extensive alkaline alteration. The high temperature mineral assemblage of uraninite associate with scheelite and tourmaline was identified in hypothermal uranium mineralization. Fluid inclusion studies on this type mineralization indicated the middle to high temperature (>250℃) mineralization with the mixing evidence of ore forming solution derived from deep level, and the boiling and mixing of ore forming solution are regarded as the dominant mineralization mechanism for the precipitating of uranium. In contrast to the mineralization ages of 67 Ma to 87 Ma for typical pitchblende vein mineralization of epithermal metallogenic system, the mineralization age is older than 100 Ma for hypothermal uranium mineralization in granite. In the Shituling deposit, Xiazhuang uranium ore field, uraninite and pitchblende micro veins with extensive potassic alteration, chloritization and sericitization are hosted in fissures of Indo-Chinese epoch granites with the uranium mineralization age of 130 Ma to 138 Ma with a mineralization temperature of 290℃ to 330℃ indicated. Other examples sharing the similar characters of hypothermal uranium mineralization have been recognized in

  12. 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)

  13. Crystal Cargo Characterization: Unravelling Granite Petrogenesis through Combined MicroXRF Imaging and In-situ Analyses.

    Science.gov (United States)

    McLeod, C. L.; Brown, K.; Brydon, R.; Haley, M.; Hill, T.; Shaulis, B.; Tronnes, R. G.

    2017-12-01

    Advances in the capabilities of microanalysis over the past several decades have promoted a redefinition of traditional petrological terminology. This has allowed a more accurate evaluation of a samples petrogenetic history. For example, the term "phenocryst", specifically describes crystals that grew from the liquid that solidified into the groundmass. Evolving from this idea is the term xenocryst, referring to crystals that did not originate in the magma but were gathered by it, and antecrysts, which crystallized from a progenitor of the magma that solidified into the groundmass. Through identification of a magmas different, and distinct, crystal populations, the petrogenetic history of a magmatic rock can therefore be unraveled. This approach has been widely applied to terrestrial volcanic systems throughout the past several decades. This study presents results from a combined microimaging and in-situ microanalytical investigation of granitic magmas crystal cargoes in order to unravel how granitic batholiths are constructed. 27 lithological units from two granite batholiths in the Oslo Rift, Norway form the basis of this investigation. Micro X-Ray Fluorescence (µXRF) mapping of major elements and selected trace elements is used in order to chemically map each granitic unit, identify any characteristic growth zoning, and compare the crystal cargoes of the different units. Major and trace elemental abundances of the major phases (feldspars, biotite, amphibole) and minor phases (apatite and titanite) are to be quantified through electron microprobe analysis (EPMA) and laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) respectively. Through chemically fingerprinting the crystal cargoes of these Oslo Rift granitic magmas, the open vs. closed nature of granitic, intrusive, magmatic systems will be investigated. Within the context of the Oslo Rift, this study also offers an opportunity to evaluate the processes inherent to granitoid magmatism

  14. Quality control chart for crushed granite concrete

    Directory of Open Access Journals (Sweden)

    Ewa E. DESMOND

    2016-07-01

    Full Text Available A chart for assessing in-situ grade (strength of concrete, has been developed in this study. Four grades of concrete after the Nigerian General Specification for Roads and bridges (NGSRB-C20, C25, C30 and C35, is studied at different water-cement ratios for medium and high slump range. The concrete mixes are made from crushed granite rock as coarse aggregate with river sand as fine aggregate. Compression test on specimens are conducted at curing age of 1, 3, 7, 14, 21, 28 and 56 days. Results on concrete workability from slump values, and water-cement ratios revealed that specimens with lower water-cement ratio were less workable but had higher strength, compared to mixes with higher water cement ratio. A simple algorithm using nonlinear regression analysis performed on each experimental data set produced Strength-Age (S-A curves which were used to establish a quality control chart. The accuracy of these curves were evaluated by computing average absolute error (AAS, the error of estimate (EoE and the average absolute error of estimate (Abs EoE for each concrete mix. These were done based on the actual average experimental strengths to measure how close the predicted values are to the experimental data set. The absolute average error of estimate (Abs. EoE recorded was less than ±10% tolerance zone for concrete works.

  15. Hydraulic fracturing in granite under geothermal conditions

    Science.gov (United States)

    Solberg, P.; Lockner, D.; Byerlee, J.D.

    1980-01-01

    The experimental hydraulic fracturing of granite under geothermal conditions produces tensile fracture at rapid fluid injection rates and shear fracture at slow injection rates and elevated differential stress levels. A sudden burst of acoustic emission activity accompanies tensile fracture formation whereas the acoustic emission rate increases exponentially prior to shear fracture. Temperature does not significantly affect the failure mechanism, and the experimental results have not demonstrated the occurrence of thermal fracturing. A critical result of these experiments is that fluid injection at intermediate rates and elevated differential stress levels increases permeability by more than an order of magnitude without producing macroscopic fractures, and low-level acoustic emission activity occurs simultaneously near the borehole and propagates outward into the specimen with time. Permeability measurements conducted at atmospheric pressure both before and after these experiments show that increased permeability is produced by permanent structural changes in the rock. Although results of this study have not demonstrated the occurrence of thermal fracturing, they suggest that fluid injection at certain rates in situ may markedly increase local permeability. This could prove critical to increasing the efficiency of heat exchange for geothermal energy extraction from hot dry rock. ?? 1980.

  16. Heat transfer studies in salt and granite

    International Nuclear Information System (INIS)

    Just, R.A.

    1978-10-01

    Results are presented of a scoping study on the feasibility of using a multi-layer terminal repository design in both salt and granite formations to store either high-level waste or spent fuel. Calculations have been made to determine temperature profiles within the repository and to provide an estimate of the thermal uplift that can be expected. Near-field models developed to compare temperature profiles in the regions close to the waste canisters indicated that maximum thermal gradients and maximum temperature increases could be significantly reduced by changing from a single to a multi-layer repository design. For both high-level waste and for spent fuel, the maximum temperature increase in the multi-level repositories was reduced to approximately 60 percent of the temperature increase predicted for the single-level repositories at the same areal loading. After the near-field models had verified that maximum thermal gradients and temperature increases could be reduced by using a multilevel repository design, a series of far-field models was developed. The far-field models used to provide qualitative comparisons of the maximum thermal uplift indicate that the thermal uplift is roughly proportional to the energy supplied to the formation. Changing from a single- to a multi-layer repository but keeping the areal loading constant results in increased thermal uplifts

  17. Groundwater evolution of the granite area, Korea

    International Nuclear Information System (INIS)

    Kim, C.S.; Bae, D.S.; Koh, Y.K.; Kim, K.S.; Kim, G.Y.

    2001-01-01

    The geochemistry and environmental isotopes of groundwater in the Cretaceous granite of the Yeongcheon area has been investigated. The hydrochemistry of groundwater belongs to the Ca-HCO 3 type. The oxygen-18 and deuterium data are clustered along the meteoric water line, indicating that the groundwater is of meteoric water origin. Tritium data show that the groundwaters were mostly recharged before pre-thermonuclear period and have been mixed with younger surface water flowing rapidly along fractured zones. Based on the mass balance and reaction simulation approaches using both the hydrochemistry of groundwater and the secondary mineralogy of fracture-filling materials, the low-temperature hydrogeochemical evolution of groundwater in the area has been modeled. The results of geochemical simulation show that the concentrations of Ca, Na and HCO 3 and pH of waters increase progressively owing to the dissolution of reactive minerals in flow paths. The concentrations of Mg and K first increase with the dissolution of reactant minerals, but later decrease when montmorillonite and illitic material are precipitated respectively. The continuous adding of reactive minerals, i. e. the progressively larger degrees of water/rock interaction, causes the formation of secondary minerals with the following sequence: hematite > gibbsite > kaolinite > montmorillonite > illitic material > microcline. The results of reaction simulation agree well with the observed water chemistry and secondary mineralogy, indicating the successful applicability of this simulation technique to delineate the complex hydrogeochemistry of bedrock groundwaters. (author)

  18. Uranium occurrences in the Granite Zone

    International Nuclear Information System (INIS)

    Nyegaard, P.; Armour-Brown, A.

    1986-04-01

    This report describes the work and results of the South Greenland Exploration Programme (Sydex) during the 1984 field season in the Granite Zone, and discusses the results and conclusions that can be drawn from them. It also contains a structural analysis of the Ivigtut-Julianehaab region, which will help in future exploration by indicating the likely directions of uraniferous faults and fractures. It also includes suggestions for future work with both exploration and scientific aspects. The project was carried out by the Geological Survey Greenland (GGU) in co-operation with Risoe National Laboratory. It was financed by the Danish Ministry of Energy. The structural analysis was carried out using previous geological maps, our own field observations and an analysis of lineament frequencies taken from aerial photographs and satellite images. Major lineaments in the region are due to E-W sinistral wrench faults and NE-SW normal faults. Analysis of the minor lineaments showed that the region could be divided into three blocks which have each reacted differently to the same regional stress field which was active throughout the Gardar period. A northern block which has been influenced by an older system of faults in the Archaean gneiss, a central block dominated by a graben, and a southern block where there is a change to a less intensively faulted area. 2 maps, 27 refs. (EG)

  19. Nature of the Yucatan Block Basement as Derived From Study of Granitic Clasts in the Impact Breccias of Chicxulub Crater

    Science.gov (United States)

    Vera-Sanchez, P.; Rebolledo-Vieyra, M.; Perez-Cruz, L.; Urrutia-Fucugauchi, J.

    2008-05-01

    The tectonic and petrologic nature of the basement of the Yucatan Block is studied from analyses of basement clasts present in the impact suevitic breccias of Chicxulub crater. The impact breccias have been sampled as part of the drilling projects conducted in the Yucatan peninsula by Petroleos Mexicanos, the National University of Mexico and the Chicxulub Scientific Drilling Project. Samples analyzed come mainly from the Yaxcopoil-1, Tekax, and Santa Elena boreholes, and partly from Pemex boreholes. In this study we concentrate on clasts of the granites, granodiorites and quartzmonzonites in the impact breccias. We report major and trace element geochemical and petrological data, which are compared with data from the granitic and volcanic rocks from the Maya Mountains in Belize and from the Swannee terrane in Florida. Basement granitic clasts analyzed present intermediate to acidic sub-alkaline compositions. Plots of major oxides (e.g., Al2O3, Fe2O3, TiO2 and CaO) and trace elements (e.g., Th, Y, Hf, Nb and Zr) versus silica allow separation of samples into two major groups, which can be compared to units in the Maya Mountains and in Florida basement. The impact suevitic breccia samples have been affected by alteration likely related to the hydrothermal processes associated with the crater melt sheet. Cloritization, seritization and fenitization alterations are recognized, due to the long term hydrothermalism. Krogh et al. (1993) reported U-Pb dates on zircons from the suevitic breccias, which gave dates of 545 +/- 5 Ma and 418 +/- 6 Ma, which were interpreted in terms of the deep granitic metamorphic Yucatan basement. The younger date correlates with the age for the Osceola Granite and the St. Lucie metamorphic complex of the Swannee terrane in the Florida peninsula. The intrusive rocks in the Yucatan basement may be related to approx. 418 Ma ago collisional event in the Late Silurian.

  20. Thermophysical and mechanical properties of granite and its effects on borehole stability in high temperature and three-dimensional stress.

    Science.gov (United States)

    Wang, Yu; Liu, Bao-lin; Zhu, Hai-yan; Yan, Chuan-liang; Li, Zhi-jun; Wang, Zhi-qiao

    2014-01-01

    When exploiting the deep resources, the surrounding rock readily undergoes the hole shrinkage, borehole collapse, and loss of circulation under high temperature and high pressure. A series of experiments were conducted to discuss the compressional wave velocity, triaxial strength, and permeability of granite cored from 3500 meters borehole under high temperature and three-dimensional stress. In light of the coupling of temperature, fluid, and stress, we get the thermo-fluid-solid model and governing equation. ANSYS-APDL was also used to stimulate the temperature influence on elastic modulus, Poisson ratio, uniaxial compressive strength, and permeability. In light of the results, we establish a temperature-fluid-stress model to illustrate the granite's stability. The compressional wave velocity and elastic modulus, decrease as the temperature rises, while poisson ratio and permeability of granite increase. The threshold pressure and temperature are 15 MPa and 200 °C, respectively. The temperature affects the fracture pressure more than the collapse pressure, but both parameters rise with the increase of temperature. The coupling of thermo-fluid-solid, greatly impacting the borehole stability, proves to be a good method to analyze similar problems of other formations.

  1. 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.)

  2. 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.

  3. 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.)

  4. 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.

  5. Modelling of bentonite-granite solutes transfer from an in situ full-scale experiment to simulate a deep geological repository (Grimsel Test Site, Switzerland)

    International Nuclear Information System (INIS)

    Buil, B.; Gomez, P.; Pena, J.; Garralon, A.; Turrero, M.J.; Escribano, A.; Sanchez, L.; Duran, J.M.

    2010-01-01

    Research highlights: → The FEBEX experiment is a 1:1 simulation of a high level waste disposal facility in crystalline rock according to the Spanish radwaste disposal concept. → Solute transfer processes occurrs at the bentonite-granite interface. → An increase of Cl and Na is observed in granitic water of the surrounding of the experiment. → Solute transfer does not affect the sealing and thermo-hydromechanical properties of the engineered barriers. → A diffusive transport of Cl and Na simulated by 1D transport modeling with an effective diffusion coefficient of D e ≅ 5.0 E-11 m 2 /s. - Abstract: The FEBEX experiment is a 1:1 simulation of a high level waste disposal facility in crystalline rock according to the Spanish radwaste disposal concept. This experiment has been performed in a gallery drilled in the underground laboratory Grimsel Test Site (Switzerland). Two boreholes parallel to the FEBEX drift were drilled 20 and 60 cm away from the granite-bentonite interface to provide data on potential bentonite-granite solutes transfer. Periodic sampling and analysis of the major ions showed: (a) the existence of solutes transfer from the bentonite porewater towards the granite groundwater, explaining the Cl - and Na + contents of the latter; (b) that the concentration of the natural tracers coming into the granite groundwater from the bentonite porewater increased over time. This bentonite-granite solutes transfer was modelled in order to predict the increase in the Cl - and Na + concentrations of the granite groundwater. The modelled results seem to confirm that the mechanism of solute migration in this scenario is that of diffusive transport. An effective diffusion coefficient of D e = 5 x 10 -11 m 2 /s was that which best fitted the data obtained.

  6. Application of Ga-Al discrimination plots in identification of high strength granitic host rocks for deep geological repository of high level radioactive waste

    International Nuclear Information System (INIS)

    Bajpai, R.K.; Narayan, P.K.; Trivedi, R.K.; Purohit, M.K.

    2010-01-01

    detail study has been undertaken wherein a total of 30 granite samples were analysed for Ga, Al, Y, Nb, Ta and other major oxides

  7. 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.

  8. 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).

  9. Zircon U-Pb ages and geochemistry of migmatites and granites in the Foping dome: Evidence for Late Triassic crustal evolution in South Qinling, China

    Science.gov (United States)

    Zhang, He; Li, Shuang-Qing; Fang, Bo-Wen; He, Jian-Feng; Xue, Ying-Yu; Siebel, Wolfgang; Chen, Fukun

    2018-01-01

    Migmatites provide a record of melt formation and crustal rheology. In this study we present zircon U-Pb ages and geochemical composition of migmatites from the Foping dome and granites from the Wulong pluton. U-Pb results from migmatite zircons indicate two episodes of partial melting. Rim domains from a leucosome in the Longcaoping area yield an age of ca. 209 Ma. Migmatites collected from the Foping dome yield U-Pb zircon ages of 2910 to 190 Ma, suggesting the involvement of meta-sedimentary source components. Rim domains of the zircons with low Th/U ratios (pluton can be subdivided into high Sr/Y and low Sr/Y granites. U-Pb zircon ages vary from 219 to 214 Ma for the high Sr/Y granites and from 214 to 192 Ma for the low Sr/Y granites. High Sr/Y granites have higher Na2O and Sr contents than the low Sr/Y granites. They also lack negative Eu anomalies and are depleted in HREE compared to the low Sr/Y granites. Initial 87Sr/86Sr ratios and εNd values of all the samples roughly overlap with those of Neoproterozoic basement rocks exposed in South Qinling. Including previous studies, we propose that the high and low Sr/Y granites formed by melting of thickened and normal crust, respectively. Close temporal-spatial relationship of the high and low Sr/Y granites with the two-stage migmatization events implies variation of crustal thickness and thermal overprints of the orogenic crust in post-collisional collapse. Following the collision of South Qinling and the Yangtze block prior to 219 Ma, partial melting of the deep crust occurred. The melts migrated upwards to form the high Sr/Y granites. This process occurred rapidly and caused collapse of the thickened crust and carried heat upwards, leading to further partial melting within the shallower crust and formation of the low Sr/Y granites.

  10. The 'Granite' collegial mission of dialogue. Report; Mission collegiale de concertation Granite. Rapport

    Energy Technology Data Exchange (ETDEWEB)

    Boisson, P; Huet, Ph; Mingasson, J

    2000-06-01

    The aim of the 'Granite' collegial mission of dialogue is to inform the French authorities, associations and population about the project of construction of an underground laboratory for the study of the disposal of high level and long-life radioactive wastes in a granitic environment. The aim of the dialogue was not to select a site but to collect the public reactions and advices about such a project. However, such a dialogue has partially failed because of a misunderstanding of the population about the aims of the mission. However, the mission has collected many point of views and questions which are developed in this report. The first and second chapters recall the process of the mission and its progress, while a third chapter stresses on the questions asked by the public and which concern the fear of nuclear wastes and the incompatibility between the disposal of wastes and the socio-economical development of the region concerned. Thanks to the lessons drawn from this experience, the mission has formulated some recommendations (chapter 4) concerning the need for a better information of the population about any topic in relation with the radioactive wastes. Some complementary information is provided in appendixes. (J.S.)

  11. The 'Granite' collegial mission of dialogue. Report; Mission collegiale de concertation Granite. Rapport

    Energy Technology Data Exchange (ETDEWEB)

    Boisson, P.; Huet, Ph.; Mingasson, J

    2000-06-01

    The aim of the 'Granite' collegial mission of dialogue is to inform the French authorities, associations and population about the project of construction of an underground laboratory for the study of the disposal of high level and long-life radioactive wastes in a granitic environment. The aim of the dialogue was not to select a site but to collect the public reactions and advices about such a project. However, such a dialogue has partially failed because of a misunderstanding of the population about the aims of the mission. However, the mission has collected many point of views and questions which are developed in this report. The first and second chapters recall the process of the mission and its progress, while a third chapter stresses on the questions asked by the public and which concern the fear of nuclear wastes and the incompatibility between the disposal of wastes and the socio-economical development of the region concerned. Thanks to the lessons drawn from this experience, the mission has formulated some recommendations (chapter 4) concerning the need for a better information of the population about any topic in relation with the radioactive wastes. Some complementary information is provided in appendixes. (J.S.)

  12. High-spatial resolution SIMS U-Pb zircon dating on Malay tin granites: New insights to crustal evolution of the Malaysian Peninsula

    Science.gov (United States)

    Ng, S.; Searle, M. P.; Whitehouse, M. J.; Chung, S.; Robb, L. J.; Ghani, A. A.; Sone, M.

    2012-12-01

    The Southeast Asian tin granite province has previously been recognized as comprising three distinct granitic belt (Cobbing et al., 1986): (1) Middle Permian - Late Triassic Eastern Province with mainly subduction-related I-type granites associated with Cu-Au deposits, (2) Late Permian - Early Jurassic Main Range Province with mainly S-type granites associated with Sn-W deposits, and (3) Late Triassic - Cretaceous Western Province with mixed I- and S-type granites associated with Sn-W deposits. These ages were obtained mainly using whole rock Rb-Sr and K-Ar geochronology in the 70s and 80s, methods that are no longer considered suitable for obtaining crystallization ages of granites due to unstable behaviour of these isotopes in hydrothermal systems. During 2011 we collected over 50 samples of granites across all three zones in Northern Malaysia for U-Pb dating using high-spatial resolution precision SIMS at the Swedish Museum of Natural History. The results reveal a westward younging trend across the Malay Peninsula. The Eastern Province hornblende- and biotite-granites in Eastern Malaysia formed by subduction-related processes have ages lying between 220-285 Ma. The Main Range Province dominantly S-type granites in west and central Malaysia have ages lying between 206-226 Ma. These include dominantly biotite granites with less common tourmaline+biotite leucocratic granites related to crustal thickening processes following collision of Sibumasu with Indochina and closing of the Palaeo-Tethyan Bentong-Raub suture zone. Some enigmatic young Cretaceous zircon rim ages (c. 81-80 Ma) may indicate a young hydrothermal - metasomatic origin for some tin mineralization from both the Eastern Province (Tioman Island) and the Western province (Phuket, Thailand) (Searle et al., 2012). Granites in Malaysia cannot be simply categorized as I-, S- or A-type as most of them failed to show distinctive minerals for classification and there is considerable overlap in geochemical

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. 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.

  18. Geochemical constraints on genesis of Paleoproterozoic A-type granite in the south margin of North China Craton

    Science.gov (United States)

    Xue, Shuo; Xu, Yang; Ling, Ming-Xing; Kang, Qing-Qing; Jiang, Xiao-Yan; Sun, Sai-Jun; Wu, Kai; Zhang, Zhe-Kun; Luo, Ze-Bin; Liu, Yu-Long; Sun, Weidong

    2018-04-01

    Paleoproterozoic A-type granites are widely outcropped in the North China Craton (NCC), particularly in the Trans-North China Orogen. However, their genesis and tectonic significance remain obscure. Here we report systematic studies on geochronology and geochemical characteristics of A-type granite in Huayangchuan, south margin of the NCC. The samples are enriched in total alkali (K2O + Na2O > 8.97 wt%), and depleted in MgO (0.84-0.93 wt%), CaO (1.28-1.90 wt%) and P2O5 (0.18-0.20 wt%), with high FeOT/MgO (5.69-6.67). They are characterized by high Zr + Y + Nb + Ce values (1293-1392 ppm) and 10,000 × Ga/Al ratios (3.14-3.35), which are typical characteristics of A-type granite. The Huayangchuan A-type granite can be further classified as A1-type subgroup based on particular geochemical features, e.g., low Y/Nb (0.87-1.00) and Yb/Ta (0.88-1.10). High precision zircon U-Pb dating of the A-type granite by secondary ion mass spectrometry (SIMS) yields Paleoproterozoic 207Pb/206Pb ages of 1829.5 ± 2.5 Ma. The low zircon ɛHf(t) values (-6.97 to -10.45), along with zircon Hf model age of 2.7-2.9 Ga, indicate that the Huayangchuan A-type granite was derived from partial melting of the ancient continental crust with contribution of enriched mantle components. The low zircon δ18O composition (4.00 to 6.78‰) indicates that the zircons were crystallized from low δ18O magmas, which derived from the crust metasomatized by low δ18O mantle fluids or melts. The E-W trend A1-type granitic plutons in the NCC are generally outcropped in a rift tectonic regime, which is consistent with the development of the mantle plume in the Xiong'er district. The large volume of basaltic magmas, generated by mantle plume head, underplated the lower continental crust and formed the Huayangchuan A-type granite.

  19. 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

  20. 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.

  1. Determination of Matrix Diffusion Properties of Granite

    International Nuclear Information System (INIS)

    Holtta, Pirkko; Siitari-Kauppi, Marja; Huittinen, Nina; Poteri, Antti

    2007-01-01

    Rock-core column experiments were introduced to estimate the diffusion and sorption properties of Kuru Grey granite used in block-scale experiments. The objective was to examine the processes causing retention in solute transport through rock fractures, especially matrix diffusion. The objective was also to estimate the importance of retention processes during transport in different scales and flow conditions. Rock-core columns were constructed from cores drilled into the fracture and were placed inside tubes to form flow channels in the 0.5 mm gap between the cores and the tube walls. Tracer experiments were performed using uranin, HTO, 36 Cl, 131 I, 22 Na and 85 Sr at flow rates of 1-50 μL.min -1 . Rock matrix was characterized using 14 C-PMMA method, scanning electron microscopy (SEM), energy dispersive X-ray micro analysis (EDX) and the B.E.T. method. Solute mass flux through a column was modelled by applying the assumption of a linear velocity profile and molecular diffusion. Coupling of the advection and diffusion processes was based on the model of generalised Taylor dispersion in the linear velocity profile. Experiments could be modelled applying a consistent parameterization and transport processes. The results provide evidence that it is possible to investigate matrix diffusion at the laboratory scale. The effects of matrix diffusion were demonstrated on the slightly-sorbing tracer breakthrough curves. Based on scoping calculations matrix diffusion begins to be clearly observable for non-sorbing tracer when the flow rate is 0.1 μL.min -1 . The experimental results presented here cannot be transferred directly to the spatial and temporal scales that prevail in an underground repository. However, the knowledge and understanding of transport and retention processes gained from this study is transferable to different scales from laboratory to in-situ conditions. (authors)

  2. Thermomechanical studies in granite at Stripa, Sweden

    International Nuclear Information System (INIS)

    Cook, N.G.W.; Myer, L.R.

    1981-01-01

    Media other than rock salt are being considered for the deep, geologic disposal of nuclear wastes. The disposal of high-level nuclear waste in a deep, underground repository will subject the rock to a thermal pulse that will induce displacements, strains, and stresses in the rock. Thermomechanical experiments, with electrical heaters simulating the thermal output of waste canisters, were carried out in granite at a depth of 340 m below surface adjacent to a defunct iron ore mine at Stripa, Sweden. Changes in temperature, displacement, and stress in the rock around these heaters were measured, and the measurements were compared with predictions calculated from the theory of linear thermoelasticity. Measured temperature changes agreed well with predictions, but measured displacements and stresses were consistently less than those predicted with constant values for the coefficient of thermal expansion and elastic properties of the rock. A laboratory test program to measure these coefficients over ranges of stress and temperature representing those in the field experiment has been initiated. Test specimens were taken from cores recovered from the instrumentation holes in the Stripa experiments. Preliminary results from laboratory tests on specimens free of joints indicate that the values of Young's modulus and Poisson's ratio increase from about 60 to 80 MPa and from 0.15 to 0.22, respectively, as the confining stress is increased from 2 to 55 MPa; these values decrease with increasing temperature, more so at 2 MPa than at 55 MPa. The linear coefficient of thermal expansion at a confining stress of 30 MPa increases from about 10 x 10 - 6 / 0 C at 40 0 C to about 14 x 10 - 6 / 0 C. The magnitudes of these changes are not sufficient to resolve the disparity between measured and predicted results. Perhaps the properties of test specimens containing joints will show greater variations in the values of the thermomechanical coefficients with temperature and pressure

  3. U(VI) sorption on granite: prediction and experiments

    International Nuclear Information System (INIS)

    Nebelung, C.; Brendler, V.

    2010-01-01

    One widely accepted approach - component additivity (CA) - to describe the sorption of contaminants onto complex materials such as rocks or soils is based on the assumption that the surface of a complex mineral assemblage is composed of a mixture of mineral constituents whose surface properties are known from independent studies. An internally consistent SCM (surface complexation model) database can be developed that describes the adsorption reactions of solutes to each phase. Here, the capability of such a methodology was tested, using the code MINTEQA2 including thermodynamic data of the NEA-TDB, and literature data for SCM, namely the DDL model. The sorption characteristics of U(VI) on granite (from Eibenstock, Saxony, Germany, with the main components quartz, albite, orthoclase, and muscovite) was predicted and then compared to batch experiments. Granite plays an important role in the remediation of former uranium ore mining and milling sites, but is also one of the host rocks considered for final disposal of nuclear materials. Safety assessment requires a detailed understanding of this system and its retention potential with regard to hazardous components. Namely the sorption of uranium in this complex rock is not fully understood yet. The experiments thus also provided a better understanding of the far-field behaviour in granitic geological nuclear repositories. The robustness of the prediction was tested by variation of the granite composition and the variation of the specific surface area (SSA) - first all components were predicted with a uniform granite SSA, second with a distinct SSA for each granite component (determined on pure minerals for the same grain size fractions). Changes in compositions yielded only marginal differences in the prediction. Different approaches to SSA showed somewhat larger deviations. In conclusion, the CA methodology is a valid and robust approach to U(VI) sorption onto complex substrates such as granite, provided sufficient

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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%.

  10. Petrographic and mineralogical features of the uraniferous pink granites in the north eastern desert of egypt

    International Nuclear Information System (INIS)

    Atawiya, M.Y.; Salman, A.B.; El-Bayyomi, R.M.

    1998-01-01

    The present work is concerned with the petrological, mineralogical and geochemical studies of some uranium bearing younger granites in the north eastern desert of egypt particularly Gebel Gattar area. The area around Gebel Gattar comprises the following rock units (starting from the oldest): meta volcanic, diorite-grano-diorite complex- Dokhan volcanics- Hammamat sediments, younger granites and dykes. The most significant structural features are represented by NNE-ENE dominantly trending faults and joints. Petrographicaly, the pink granites are divided into normal and mineralized (uraniferous) granites. Normal granites are classified into three types; a) leucocratic perthitic granite, b) hornblende- biotite perthitic granite and c) two feldspars perthitic granite. Mineralized granites are sheared, deformed, pinkish brown in colour and strongly altered. A remarkable secondary uranium mineralization has been recorded along fault and fracture zones

  11. The transition from granite to banded aplite-pegmatite sheet complexes: An example from Megiliggar Rocks, Tregonning topaz granite, Cornwall

    Science.gov (United States)

    Breiter, K.; Ďurišová, J.; Hrstka, T.; Korbelová, Z.; Vašinová Galiová, M.; Müller, A.; Simons, B.; Shail, R. K.; Williamson, B. J.; Davies, J. A.

    2018-03-01

    The genetic relationship between a granite pluton and adjacent complex of rare-metal pegmatite-aplite-banded sheets (Megiliggar Sheet Complex - MSC) has been studied at the border of the Tregonning topaz granite at Megiliggar Rocks, Cornwall, SW England. Similarities in whole-rock chemical and mineralogical compositions, together with a gradual change in textures away from the granite margin, provide strong evidence for a genetic link between the Tregonning Granite and MSC. The sheets are likely to represent apophyses of residual melt which escaped from the largely crystallized roof of the granite pluton. The escaping melt was peraluminous, had a composition near the F, B, Li slightly enriched granite minimum, and, in comparison with other Cornish granites, was enriched in F, Li, Rb, Cs, Sn, W, Nb, Ta, and U, and depleted in Fe, Mg, Ca, Sr, Th, Zr, and REE. With increasing distance from the Tregonning Granite, the silicate melt crystallized as homogeneous leucogranite sheets and banded complex sheets (i.e. combinations of bands with granitic, aplitic and pegmatitic textures), then layered aplite-pegmatites; this sequence becoming progressively more depleted in the fluxing and volatile elements F, Li, Rb, and Cs, but showing no change in Zr/Hf ratios. The fixed Zr/Hf ratio is interpreted as indicating a direct genetic link (parental melt) between all rock types, however the melt progressively lost fluxing and volatile elements with distance from the granite pluton, probably due to wall-rock reaction or fluid exsolution and migration via fractures. Differentiation of the primary melt into Na-Li-F-rich and separate K-B-rich domains was the dominant chemical process responsible for the textural and mineral diversity of the MSC. On a large (cliff-section) scale, the proximal Na-Li-F-rich leucogranite passes through complex sheets into K-B-rich aplite-pegmatites, whilst at a smaller (<1 m) scale, the K-B-rich bands are interspersed (largely overlain) by Na

  12. 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)

  13. 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.

  14. Petrography, mineral chemistry and lithochemistry of the albitite and granite-gneissics rocks of anomaly 35 from Lagoa Real uranium province

    International Nuclear Information System (INIS)

    Santos, Camila Marques dos

    2016-01-01

    In the northwestern portion of the Lagoa Real Uranium Province (LRUP), located in south-central Bahia, it is located one of the most promising uranium anomalies Brazil (an35, Gameleira I deposit), the reserves and proximity to the Cachoeira mine. Other anomalies of this sector (eg. 31 AN and AN34), are also considered strategic for the content of radioactive minerals and REE. The objective was to develop a study of a representative drill core of an35, where the main rocks PULR are present. The research focused on the mineralogical and chemical changes observed in the passages of a lithology to another, from the rock to the meta granitic albitites, through gneiss and transitional rocks, and making comparisons with similar lithologies sampled on testimonies of AN31 and 34. The granites are classified as hypersolvus coarse alkali-feldspar granite and are variably deformed. The main mineral assemblage in granites are perthitic orthoclase+hedenbergite+ quartz +hastingsite + biotite, and zircon, apatite, ilmenite and titanite are accessories. The reddening of these rocks are characterized by feldspars sericitization and hematitization and the presence of 'vazios'. The gneisses are mainly gray and reach milonitic to protomilonitics terms. These rocks have characteristics of subsolidus changes as swapped rims and metasomatic perthites. The tardi-magmatic association (amphibole+biotite) indicates final crystallization or late influx by superficial fluids resulting in an increase in water and volatiles, such as F and Cl in the system, which must also have carried rare-earth elementsGranites have geochemical affinity with A-type ferroan granite, A2, reduced and are post-collisional. Their patterns of incompatible elements and rare earths are comparable to Sao Timoteo Granite, but their petrographic features indicate that it is a less common granite facies. Albitites were classified as garnet albitites, magnetite albitites and biotite albitites. Contacts between

  15. 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

  16. 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 samples, water samples and some salts samples without interfering effect of various cations and anions. Copyright © 2011 Elsevier Ltd. All rights reserved.

  17. Recovery of Picloram and 2,4-Dichlorophenoxyacetic Acid from Aqueous Samples by Reversed-Phase Solid-Phase Extraction

    Science.gov (United States)

    Martha J.M. Wells; Jerry L. Michael

    1987-01-01

    Extensive preparation of samples before chromatographic analysis is usually the most time-consuming process in the determination of many organic compounds in environmental matrices. In the past, removal of some organic from aqueous solution was commonly done by liquid/liquid extraction. However, the introduction of stable, covalently bonded reversed-phase sorbents now...

  18. A nanoparticle-based solid-phase extraction procedure followed by spectrofluorimetry to determine carbaryl in different water samples

    Energy Technology Data Exchange (ETDEWEB)

    Tabrizi, Ahad Bavili, E-mail: a.bavili@tbzmed.ac.ir, E-mail: abavilitabrizia@gmail.com [Biotechnology Research Center, Tabriz University of Medical Sciences, Tabriz (Iran, Islamic Republic of); Rashidi, Mohammad Reza [Research Center for Pharmaceutical Nanotechnology, Tabriz University of Medical Sciences, Tabriz, (Iran, Islamic Republic of); Ostadi, Hadi [Department of Chemistry, Payam-e-noor University, Ardabil Branch, Ardabil (Iran, Islamic Republic of)

    2014-04-15

    In this study, a new method based on Fe{sub 3}O{sub 4} magnetite nanoparticles (MNPs) has been developed for the extraction, preconcentration and determination of trace amounts of carbaryl from environmental water samples. Fe{sub 3}O{sub 4} MNPs were synthesized and modified by the surfactant sodium dodecyl sulfate (SDS), then successfully applied for the extraction of carbaryl and its determination by spectrofluorimetry. Main factors affecting the adsolubilization of carbaryl such as the amount of SDS, pH value, standing time, desorption solvent and maximal extraction volume were optimized. Under the selected conditions, carbaryl could be quantitatively extracted. Acceptable recoveries (84.5-91.9%) and relative standard deviations (6.2%) were achieved in analyzing spiked water samples. A concentration factor of 20 was achieved by the extraction of 100 mL of environmental water samples. The limit of detection and quantification were found to be 2.1 and 6.9 μg L{sup -1}, respectively. The proposed method was successfully applied for the extraction and determination of carbaryl in environmental water samples. (author)

  19. Smolt Monitoring at the Head of Lower Granite Reservoir and Lower Granite Dam, 2002 Annual Report.

    Energy Technology Data Exchange (ETDEWEB)

    Buettner, Edwin W.; Putnam, Scott A. [Idaho Department of Fish and Game

    2009-02-18

    This project monitored the daily passage of Chinook salmon Oncorhynchus tshawytscha, steelhead trout O. mykiss, and sockeye salmon smolts O. nerka during the 2002 spring out-migration at migrant traps on the Snake River and Salmon River. In 2002 fish management agencies released significant numbers of hatchery Chinook salmon and steelhead trout above Lower Granite Dam that were not marked with a fin clip or coded-wire tag. Generally, these fish were distinguishable from wild fish by the occurrence of fin erosion. Total annual hatchery Chinook salmon catch at the Snake River trap was 11.4 times greater in 2002 than in 2001. The wild Chinook catch was 15.5 times greater than the previous year. Hatchery steelhead trout catch was 2.9 times greater than in 2001. Wild steelhead trout catch was 2.8 times greater than the previous year. The Snake River trap collected 3,996 age-0 Chinook salmon of unknown rearing. During 2002, the Snake River trap captured 69 hatchery and 235 wild/natural sockeye salmon and 114 hatchery coho salmon O. kisutch. Differences in trap catch between years are due to fluctuations not only in smolt production, but also differences in trap efficiency and duration of trap operation associated with flow. The significant increase in catch in 2002 was due to a 3.1 fold increase in hatchery Chinook production and a more normal spring runoff. Trap operations began on March 10 and were terminated on June 7. The trap was out of operation for a total of four days due to mechanical failure or debris. Hatchery Chinook salmon catch at the Salmon River trap was 4.2 times greater and wild Chinook salmon catch was 2.4 times greater than in 2001. The hatchery steelhead trout collection in 2002 was 81% of the 2001 numbers. Wild steelhead trout collection in 2002 was 81% of the previous year's catch. Trap operations began on March 10 and were terminated on May 29 due to high flows. The trap was out of operation for four days due to high flow or debris. The

  20. Smolt Monitoring at the Head of Lower Granite Reservoir and Lower Granite Dam, 2003 Annual Report.

    Energy Technology Data Exchange (ETDEWEB)

    Buettner, Edwin W.; Putnam, Scott A. [Idaho Department of Fish and Game

    2009-02-18

    This project monitored the daily passage of Chinook salmon Oncorhynchus tshawytscha, steelhead trout O. mykiss, and sockeye salmon O. nerka smolts during the 2003 spring out-migration at migrant traps on the Snake River and Salmon River. In 2003 fish management agencies released significant numbers of hatchery Chinook salmon and steelhead trout above Lower Granite Dam that were not marked with a fin clip or coded-wire tag. Generally, these fish were distinguishable from wild fish by the occurrence of fin erosion. Total annual hatchery Chinook salmon catch at the Snake River trap was 2.1 times less in 2003 than in 2002. The wild Chinook catch was 1.1 times less than the previous year. Hatchery steelhead trout catch was 1.7 times less than in 2002. Wild steelhead trout catch was 2.1 times less than the previous year. The Snake River trap collected 579 age-0 Chinook salmon of unknown rearing. During 2003, the Snake River trap captured five hatchery and 13 wild/natural sockeye salmon and 36 coho salmon O. kisutch of unknown rearing. Differences in trap catch between years are due to fluctuations not only in smolt production, but also differences in trap efficiency and duration of trap operation associated with flow. The significant differences in catch between 2003 and the previous year were due mainly to low flows during much of the trapping season and then very high flows at the end of the season, which terminated the trapping season 12 days earlier than in 2002. Trap operations began on March 9 and were terminated on May 27. The trap was out of operation for a total of zero days due to mechanical failure or debris. Hatchery Chinook salmon catch at the Salmon River trap was 16.8% less and wild Chinook salmon catch was 1.7 times greater than in 2002. The hatchery steelhead trout collection in 2003 was 5.6% less than in 2002. Wild steelhead trout collection was 19.2% less than the previous year. Trap operations began on March 9 and were terminated on May 24 due to high

  1. The Applicability of the Distribution Coefficient, KD, Based on Non-Aggregated Particulate Samples from Lakes with Low Suspended Solids Concentrations.

    Directory of Open Access Journals (Sweden)

    Aine Marie Gormley-Gallagher

    Full Text Available Separate phases of metal partitioning behaviour in freshwater lakes that receive varying degrees of atmospheric contamination and have low concentrations of suspended solids were investigated to determine the applicability of the distribution coefficient, KD. Concentrations of Pb, Ni, Co, Cu, Cd, Cr, Hg and Mn were determined using a combination of filtration methods, bulk sample collection and digestion and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS. Phytoplankton biomass, suspended solids concentrations and the organic content of the sediment were also analysed. By distinguishing between the phytoplankton and (inorganic lake sediment, transient variations in KD were observed. Suspended solids concentrations over the 6-month sampling campaign showed no correlation with the KD (n = 15 for each metal, p > 0.05 for Mn (r2 = 0.0063, Cu (r2 = 0.0002, Cr (r2 = 0.021, Ni (r2 = 0.0023, Cd (r2 = 0.00001, Co (r2 = 0.096, Hg (r2 = 0.116 or Pb (r2 = 0.164. The results implied that colloidal matter had less opportunity to increase the dissolved (filter passing fraction, which inhibited the spurious lowering of KD. The findings conform to the increasingly documented theory that the use of KD in modelling may mask true information on metal partitioning behaviour. The root mean square error of prediction between the directly measured total metal concentrations and those modelled based on the separate phase fractions were ± 3.40, 0.06, 0.02, 0.03, 0.44, 484.31, 80.97 and 0.1 μg/L for Pb, Cd, Mn, Cu, Hg, Ni, Cr and Co respectively. The magnitude of error suggests that the separate phase models for Mn and Cu can be used in distribution or partitioning models for these metals in lake water.

  2. A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

    2017-07-01

    Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

  3. Preparation and evaluation of a novel molecularly imprinted polymer coating for selective extraction of indomethacin from biological samples by electrochemically controlled in-tube solid phase microextraction

    Energy Tech