Sample records for bulk speciation methods

  1. Speciation of arsenic in bulk and rhizosphere soils from artisanal cooperative mines in Bolivia. (United States)

    Acosta, Jose A; Arocena, Joselito M; Faz, Angel


    Soils near artisanal and small-scale gold mines (ASGM) have high arsenic (As) contents due to the presence of arsenopyrite in gold ores and accelerated accumulations due to mine wastes disposal practices and other mining activities. We determined the content and speciation to understand the fate and environmental risks of As accumulations in 24 bulk and 12 rhizosphere soil samples collected in the Virgen Del Rosario and the Rayo Rojo cooperative mines in the highlands of Bolivia. Mean total As contents in bulk and rhizosphere soils ranged from 13 to 64 mg kg(-1) and exceeded the soil environmental quality guidelines of Canada. Rhizosphere soils always contained at least twice the As contents in the bulk soil. Elemental mapping using 4×5 μm synchrotron-generated X-ray micro-beam revealed As accumulations in areas enriched with Fe. Results of As-X-ray Absorption Near Edge Spectroscopy (As-XANES) showed that only As(V) species was detectable in all samples regardless of As contents, size fractions and types of vegetation. Although the toxicity of As(V) is less than As(III), we suggest that As uptake of commonly-grazed vegetation by alpaca and llama must be determined to fully understand the environmental risks of high As in soils near ASGM in Bolivia. In addition, knowledge on the speciation of the As bio-accessible fraction will provide another useful information to better understand the fate and transfer of As from soils into the food chain in environments associated with the ASGM in Bolivia and other parts of the world. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Bulk and Surface Aqueous Speciation of Calcite: Implications for Low-Salinity Waterflooding of Carbonate Reservoirs

    KAUST Repository

    Yutkin, Maxim P.


    Low-salinity waterflooding (LSW) is ineffective when reservoir rock is strongly water-wet or when crude oil is not asphaltenic. Success of LSW relies heavily on the ability of injected brine to alter surface chemistry of reservoir crude-oil brine/rock (COBR) interfaces. Implementation of LSW in carbonate reservoirs is especially challenging because of high reservoir-brine salinity and, more importantly, because of high reactivity of the rock minerals. Both features complicate understanding of the COBR surface chemistries pertinent to successful LSW. Here, we tackle the complex physicochemical processes in chemically active carbonates flooded with diluted brine that is saturated with atmospheric carbon dioxide (CO2) and possibly supplemented with additional ionic species, such as sulfates or phosphates. When waterflooding carbonate reservoirs, rock equilibrates with the injected brine over short distances. Injected-brine ion speciation is shifted substantially in the presence of reactive carbonate rock. Our new calculations demonstrate that rock-equilibrated aqueous pH is slightly alkaline quite independent of injected-brine pH. We establish, for the first time, that CO2 content of a carbonate reservoir, originating from CO2-rich crude oil and gas, plays a dominant role in setting aqueous pH and rock-surface speciation. A simple ion-complexing model predicts the calcite-surface charge as a function of composition of reservoir brine. The surface charge of calcite may be positive or negative, depending on speciation of reservoir brine in contact with the calcite. There is no single point of zero charge; all dissolved aqueous species are charge determining. Rock-equilibrated aqueous composition controls the calcite-surface ion-exchange behavior, not the injected-brine composition. At high ionic strength, the electrical double layer collapses and is no longer diffuse. All surface charges are located directly in the inner and outer Helmholtz planes. Our evaluation of

  3. Nickel speciation in several serpentine (ultramafic) topsoils via bulk synchrotron-based techniques

    Energy Technology Data Exchange (ETDEWEB)

    Siebecker, Matthew G.; Chaney, Rufus L.; Sparks, Donald L.


    Serpentine soils have elevated concentrations of trace metals including nickel, cobalt, and chromium compared to non-serpentine soils. Identifying the nickel bearing minerals allows for prediction of potential mobility of nickel. Synchrotron-based techniques can identify the solid-phase chemical forms of nickel with minimal sample treatment. Element concentrations are known to vary among soil particle sizes in serpentine soils. Sonication is a useful method to physically disperse sand, silt and clay particles in soils. Synchrotron-based techniques and sonication were employed to identify nickel species in discrete particle size fractions in several serpentine (ultramafic) topsoils to better understand solid-phase nickel geochemistry. Nickel commonly resided in primary serpentine parent material such as layered-phyllosilicate and chain-inosilicate minerals and was associated with iron oxides. In the clay fractions, nickel was associated with iron oxides and primary serpentine minerals, such as lizardite. Linear combination fitting (LCF) was used to characterize nickel species. Total metal concentration did not correlate with nickel speciation and is not an indicator of the major nickel species in the soil. Differences in soil texture were related to different nickel speciation for several particle size fractionated samples. A discussion on LCF illustrates the importance of choosing standards based not only on statistical methods such as Target Transformation but also on sample mineralogy and particle size. Results from the F-test (Hamilton test), which is an underutilized tool in the literature for LCF in soils, highlight its usefulness to determine the appropriate number of standards to for LCF. EXAFS shell fitting illustrates that destructive interference commonly found for light and heavy elements in layered double hydroxides and in phyllosilicates also can occur in inosilicate minerals, causing similar structural features and leading to false positive results in

  4. Surface/bulk partitioning and acid/base speciation of aqueous decanoate: direct observations and atmospheric implications

    Directory of Open Access Journals (Sweden)

    N. L. Prisle


    Full Text Available Dilute aqueous solutions of the atmospheric organic surfactant sodium decanoate have been studied using surface sensitive X-ray photoelectron spectroscopy combined with synchrotron radiation. We studied the decanoate/decanoic acid speciation and preferential adsorption at the vapor–liquid interface, and the responses to mixing in solution with some of the most common atmospheric inorganic ions, Na+, NH4+, Cl, and SO42−. We observe little or no influence of Na+, Cl, or SO42− ions, on neither the relative speciation nor the individual adsorption properties of decanoate and decanoic acid. In particular, no significant salting-out effect due to common Na+ cations of the organic and inorganic salts was observed for these solutions. On the other hand, mixing with NH4+ cations resulted in a pronounced surface enhancement of decanoic acid, which is attributed to surface specific acid–base chemistry. These changes in surface/bulk partitioning and surface speciation may significantly affect properties of aqueous droplets containing decanoate/decanoic acid, and potential implications for several processes critical to the climate effects of atmospheric aerosols are discussed.

  5. Possible method for dissolved organic carbon speciation in forest soils (United States)

    Drabek, O.; Tejnecký, V.; Ash, C.; Hubova, P.; Boruvka, L.


    Dissolved organic carbon (DOC) is a natural part of dissolved organic matter and it plays an important role in the biogeochemistry of soil processes. Low Molecular Mass Organic Acids (LMMOA) are an essential part of DOC. These acids play a key role in chemical processes that affect the entire soil environment. Knowing the amount of DOC and the speciation of LMMOA is required for realistic equilibrium modelling of soil chemical processes and transport mechanisms. There have been a number of proposed methods for the quantitative analysis of DOC and for speciation of LMMOA. The first aim of this contribution is to introduce and test a modified spectroscopic method for the determination of water-extractable organic carbon (WEOC) from forest soils. In general this method is based on the oxidization of WEOC by chromium-sulphuric acid. The presented method can be used as an economical alternative to the classical, more financially demanding elemental analysis. However, the main aim is to test the reliability of the method for LMMOA speciation. Ion exchange chromatography (IC) with hydroxide elution has proven to be a useful tool for the determination of LMMOA in many different water-based samples. However, the influence of multivalent cations (often present in environmental samples) on IC results has not yet been sufficiently studied. In order to assess the influence of Al, Fe, Mn, Mg and Ca on the amount of LMMOA determined by IC, an extensive set of model solutions was prepared and immediately analysed by means of IC. Moreover, the influence of pH on determined amounts of LMMOA in model solutions and representative soil aqueous extracts was investigated. These experimental results were compared to expected values and also to results provided by the chemical equilibrium model - PHREEQC. Based on the above listed research, some modifications to the common IC method for LMMOA speciation are presented.

  6. Evaluation of mercury speciation by EPA (Draft) Method 29

    Energy Technology Data Exchange (ETDEWEB)

    Laudal, D.L.; Heidt, M.K. [Energy & Environmental Research Center, Grand Forks, ND (United States); Nott, B. [Electric Power Research Institute, Palo Alto, CA (United States)


    The 1990 Clean Air Act Amendments require that the U.S. Environmental protection Agency (EPA) assess the health risks associated with mercury emissions. Also, the law requires a separate assessment of health risks posed by the emission of 189 tract chemicals (including mercury) for electric utility steam-generating units. In order to conduct a meaningful assessment of health and environmental effects, we must have, among other things, a reliable and accurate method to measure mercury emissions. In addition, the rate of mercury deposition and the type of control strategies used may depend upon the type of mercury emitted (i.e., whether it is in the oxidized or elemental form). It has been speculated that EPA (Draft) Method 29 can speciate mercury by selective absorption; however, this claim has yet to be proven. The Electric Power Research Institute (EPRI) and the U.S. Department of Energy (DOE) have contracted with the Energy & Environmental Research Center (EERC) at University of North Dakota to evaluate EPA (Draft) Method 29 at the pilot-scale level. The objective of the work is to determine whether EPA (Draft) Method 29 can reliably quantify and speciate mercury in the flue gas from coal-fired boilers.

  7. Arsenic extraction and speciation in plants: Method comparison and development. (United States)

    Zhao, Di; Li, Hong-Bo; Xu, Jia-Yi; Luo, Jun; Ma, Lena Qiying


    We compared four methods to extract arsenic (As) from three different plants containing different As levels for As speciation with the goal of developing a more efficient method, i.e., As-hyperaccumulator Pteris vittata at 459-7714mgkg(-1), rice seedling at 53.4-574mgkg(-1), and tobacco leaf at 0.32-0.35mgkg(-1). The four methods included heating with dilute HNO3, and sonication with phosphate buffered solution, methanol/water, and ethanol/water, with As being analyzed using high-performance liquid chromatography coupled with inductively-coupled plasma mass spectrometry (HPLC-ICP-MS). Among the four methods, the ethanol/water method produced the most satisfactory extraction efficiency (~80% for the roots and >85% for the fronds) without changing As species based on P. vittata. The lower extraction efficiency from P. vittata roots was attributed to its dominance by arsenate (82%) while arsenite dominated in the fronds (89%). The ethanol/water method used sample:solution ratio of 1:200 (0.05g:10mL) with 50% ethanol and 2h sonication. Based on different extraction times (0.5-2h), ethanol concentrations (25-100%) and sample:solution ratios (1:50-1:300), the optimized ethanol/water method used less ethanol (25%) and time (0.5h for the fronds and 2h for the roots). Satisfactory extraction was also obtained for tobacco leaf (78-92%) and rice seedlings (~70%) using the optimized method, which was better than the other three methods. Based on satisfactory extraction efficiency with little change in As species during extraction from three plants containing different As levels, the optimized method has the potential to be used for As speciation in other plants. Copyright © 2015 Elsevier B.V. All rights reserved.


    Directory of Open Access Journals (Sweden)

    Constantin Luca


    Full Text Available Selenium is an essential microelement, sometimes redoubtable, through its beneficial role - risk depending on its concentration in the food chain, at low dose is an important nutrient in the life of humans and animals, contrary at high doses, it becomes toxic. Selenium may be find itself in the environment (soil, sediment, water in many forms (oxidized, reduced, organometallic which determine their mobility and toxicity. Determination of chemical speciation (identification of different chemical forms provides much more complete information for a better understanding of the behavior and the potential impact on the environment. In this work we present the results of methodological research on the extraction of sequential forms of selenium in the soil and the coupling of analytical methods capable of identifying very small amounts of selenium in soils An efficient scheme of sequential extractions forms of selenium (SES consisting in atomic absorption spectrometry coupled with hydride generation (HGAAS has been developed into five experimental steps, detailed in the paper. This operational scheme has been applied to the analysis of chemical speciation in the following areas: the Bărăgan Plain and Central Dobrogea of Romania.

  9. Method for Vanadium Speciation in Aqueous Samples by HPLC-ICP ...

    African Journals Online (AJOL)

    Method for Vanadium Speciation in Aqueous Samples by HPLC-ICP-OES. M Hu, PP Coetzee. Abstract. A method for vanadium speciation is proposed. The method uses a low concentration eluent, 10 mmol L–1 EDTA and 14 mmol L–1 sodium carbonate, for the ion chromatographic separation of vanadium species at a ...

  10. Carbon nanotubes grown on bulk materials and methods for fabrication (United States)

    Menchhofer, Paul A [Clinton, TN; Montgomery, Frederick C [Oak Ridge, TN; Baker, Frederick S [Oak Ridge, TN


    Disclosed are structures formed as bulk support media having carbon nanotubes formed therewith. The bulk support media may comprise fibers or particles and the fibers or particles may be formed from such materials as quartz, carbon, or activated carbon. Metal catalyst species are formed adjacent the surfaces of the bulk support material, and carbon nanotubes are grown adjacent the surfaces of the metal catalyst species. Methods employ metal salt solutions that may comprise iron salts such as iron chloride, aluminum salts such as aluminum chloride, or nickel salts such as nickel chloride. Carbon nanotubes may be separated from the carbon-based bulk support media and the metal catalyst species by using concentrated acids to oxidize the carbon-based bulk support media and the metal catalyst species.

  11. Molecular speciation and transformation of soil legacy phosphorus with and without long-term phosphorus fertilization: Insights from bulk and microprobe spectroscopy. (United States)

    Liu, Jin; Yang, Jianjun; Cade-Menun, Barbara J; Hu, Yongfeng; Li, Jumei; Peng, Chang; Ma, Yibing


    Soil legacy phosphorus (P) represents a substantial secondary P resource to postpone the global P crisis. To fully utilize this P reserve, the transformation of legacy P speciation in a black soil with and without P fertilization for 27 years was investigated by chemical fractionation, molecular-level bulk (P K-edge X-ray absorption near-edge, XANES; solution 31P nuclear magnetic resonance) and microprobe (µ-X-ray fluorescence and µ-XANES) spectroscopy. Results from both fractionation and P bulk-XANES concordantly indicated that Ca2-P [Ca(H2PO4)2] acts as a reserve of labile P in response to soils with or without P fertilization. Cropping for 27 years depleted hydroxyapatite while enriched iron-bound P in soils irrespective of P application. Similar accumulation of soil organic P (Po), probably due to root residue inputs, occurred in both soils with and without P fertilization; the accumulated Po was present as orthophosphate diesters in soils with P fertilization more than in soils without P fertilization, suggesting that the release of labile Po was triggered by soil P deficits. These results provide vital information for agronomically and environmentally sustainable P management by demonstrating the potential crop availability of legacy soil P, which could reduce future P fertilization.

  12. Bulk Electric Load Cost Calculation Methods: Iraqi Network Comparative Study

    Directory of Open Access Journals (Sweden)

    Qais M. Alias


    Full Text Available It is vital in any industry to regain the spent capitals plus running costs and a margin of profits for the industry to flourish. The electricity industry is an everyday life touching industry which follows the same finance-economic strategy. Cost allocation is a major issue in all sectors of the electric industry, viz, generation, transmission and distribution. Generation and distribution service costing’s well documented in the literature, while the transmission share is still of need for research. In this work, the cost of supplying a bulk electric load connected to the EHV system is calculated. A sample basic lump-average method is used to provide a rough costing guide. Also, two transmission pricing methods are employed, namely, the postage-stamp and the load-flow based MW-distance methods to calculate transmission share in the total cost of each individual bulk load. The three costing methods results are then analyzed and compared for the 400kV Iraqi power grid considered for a case study.

  13. A Novel Kinetic Method to Measure Apparent Solubility Product of Bulk Human Enamel

    Directory of Open Access Journals (Sweden)

    Linda Hassanali


    Full Text Available Introduction: Tooth enamel mineral loss is influenced by its solubility product value, which is fundamental to the understanding of de- and remineralization resulting from a carious or erosive challenge. Published pKsp values for human enamel and hydroxyapatite range from 110 to 126 suggesting a heterogeneous nature of enamel solubility. However, this range of values may also result from the variety of methods used, e.g., some authors reporting values for suspensions of enamel powder and others for bulk enamel. The aim of this study was to develop a method to measure the solubility of bulk human enamel under controlled in vitro conditions simulating demineralization behavior of enamel within the oral environment using scanning microradiography (SMR. SMR was used to monitor real-time changes in enamel demineralization rates at increasing calcium concentrations in a caries simulating demineralization solution until the concentration at which thermodynamic equilibrium between enamel and solution was achieved.Method: 2 mm thick caries free erupted human enamel slabs with the natural buccal surfaces exposed were placed in SMR cells exposed to circulating caries-simulating 2.0 L 0.1 M pH = 4.0 acetic acid, at 25°C. SMR was used to continuously measure in real-time the decrease in mineral mass during the demineralization at 5 different points from on each slab. Demineralization rates were calculated from a linear regression curve of projected mineral mass against demineralization time. Changes in the demineralization rates were monitored following a series of successive increases in calcium (and phosphate at hydroxyapatite stoichiometric ratios of Ca:P 1.67 were added to the demineralizing solution, until demineralization ceased. The pH was maintained constant throughout.Results: Demineralization halted when the calcium concentration was ~30 mM. At higher calcium concentrations, mineral deposition (remineralization occurred. By comparison with results

  14. Uranium Speciation As a Function of Depth in Contaminated Hanford Sediments - A Micro-XRF, Micro-XRD, and Micro- And Bulk-XAFS Study

    Energy Technology Data Exchange (ETDEWEB)

    Singer, David M. [Stanford Univ., CA (United States); Zachara, John M. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Brown, Gordon E. [SLAC National Accelerator Lab., Menlo Park, CA (United States)


    Processing ponds at the Hanford, Washington Area 300 site were used for storing basic sodium aluminate and acidic U(VI)-Cu(II)-containing waste from 1943 to 1975. One result of this use is a groundwater plume containing elevated levels of U and Cu beneath the dry ponds and adjacent to the Columbia River. We have used synchrotron-based micro-X-ray fluorescence (μXRF) imaging, micro-X-ray absorption fine structure (μXANES) spectroscopy, and micro-X-ray diffraction (μXRD) techniques combined with bulk U LIII-edge X-ray absorption fine structure (XAFS) spectroscopy to determine the distribution and speciation of U and Cu through the vadose and groundwater zones beneath North Processing Pond #2 (NPP2). Sediment samples were collected from the vadose zone (8’ and 12’ depths), and a sample from the groundwater zone was collected just below the water table (12’-14’ depth). μXRF imaging revealed two major U occurrences within the vadose and groundwater zones: (1) low to moderate concentrations of U(VI) associated with mineral surfaces (particularly chlorite), and (2) high concentration U(VI)-containing micron-sized particles associated with surface coatings on grains of muscovite and chlorite. These U(VI) hot spots are frequently spatially correlated with Cu(II) hot spots. In the groundwater zone, these particles were identified as the copper-uranyl-silicate cuprosklodowskite and the cupper-uranyl-phosphate metatorbernite. In contrast, the U-Cu-containing particles are X-ray amorphous in the vadose zone. Fits of U LIII-edge XAFS spectra by linear-combination fitting indicate that U speciation consists of ~ 75% uranyl sorbed to clays and ~25% metatorbernite-like X-ray amorphous U-Cu-phosphates (8’ depth); nearly 100% sorbed uranyl (12’ depth); and ~70% sorbed uranyl and ~30% cuprosklodowskite/metatorbernite (ground water zone). These findings suggest that the dissolution of U(VI)-Cu(II)-bearing solids as well as the desorption of U(VI), mainly from

  15. A new method for antimony speciation in plant biomass and nutrient media using anion exchange cartridge. (United States)

    Tisarum, Rujira; Ren, Jing-Hua; Dong, Xiaoling; Chen, Hao; Lessl, Jason T; Ma, Lena Q


    A selective separation method based on anion exchange cartridge was developed to determine antimony (Sb) speciation in biological matrices by graphite furnace atomic absorption spectrophotometry (GFAAS). The selectivity of the cartridge towards antimonite [Sb(III)] and antimonate [Sb(V)] reversed in the presence of deionized (DI) water and 2mM citric acid. While Sb(V) was retained by the cartridge in DI water, Sb(III) was retained in citric acid media. At pH 6, Sb(III) and Sb(V) formed Sb(III)- and Sb(V)-citrate complexes, but the cartridge had higher affinity towards the Sb(III)-citrate complex. Separation of Sb(III) was tested at various concentrations in fresh and spent growth media and plant tissues. Our results showed that cartridge-based Sb speciation was successful in plant tissues, which was confirmed by HPLC-ICP-MS. The cartridge retained Sb(III) and showed 92-104% Sb(V) recovery from arsenic hyperaccumulator Pteris vittata roots treated with Sb(III) and Sb(V). The cartridge procedure is an effective alternative for Sb speciation, offering low cost, reproducible results, and simple Sb analysis using GFAAS. Published by Elsevier B.V.

  16. An empirical method to estimate bulk particulate refractive index for ocean satellite applications

    Digital Repository Service at National Institute of Oceanography (India)

    Suresh, T.; Desa, E.; Mascarenhas, A.A.M.Q.; Matondkar, S.G.P.; Naik, P.; Nayak, S.R.

    An empirical method is presented here to estimates bulk particulate refractive index using the measured inherent and apparent optical properties from the various waters types of the Arabian Sea. The empirical model, where the bulk refractive index...

  17. Nondestructive Method for Bulk Chemical Characterization of Barred Olivine Chondrules (United States)

    Montoya-Perez, M. A.; Cervantes-de la Cruz, K. E.; Ruvalcaba-Sil, J. L.


    This work develops a bulk chemical characterization of barred olivine chondrules based on the XRF analysis using a portable equipment at the National Research and Conservation Science Laboratory of Cultural Heritage (LANCIC-IF) in Mexico City.

  18. Methods for analysis of the distribution and speciation of iron and zinc in the cereal grain

    DEFF Research Database (Denmark)

    Hansen, Thomas Hesselhøj

    micronutrients in cereal grain primarily depends on two main components; phytic acid and proteins. Most of the phosphorus (P) found in the grain is bound in phytic acid and most sulphur (S) is incorporated into the amino acids cysteine and methionine that are part of different proteins. Co...... mineral micronutrients in extracts of a cereal grain, especially because S was measured with an increased sensitivity without decreasing that of the other elements. This novel analytical method paved the road for multi-elemental speciation and elemental imaging studies of the cereal grain. In addition...

  19. A novel method for speciation of chromium: coprecipitation without carrier element by using a triazole derivative. (United States)

    Duran, Celal; Bulut, Volkan N; Ozdes, Duygu; Gundogdu, Ali; Soylak, Mustafa


    A coprecipitation method has been established for speciation of chromium(III) and chromium(VI) in real samples. The procedure is based on the coprecipitation of Cr(III), by using a new organic coprecipitant, 3-phenyl-4-o-hydroxybenzyl-idenamino-4,5-dihydro-1,2,4-triazole-5-one, without adding any carrier element. After reduction of Cr(VI) by concentrated H2SO4 and ethanol, the method was applied to the determination of total Cr. The level of Cr(VI) was calculated by the difference of total Cr and Cr(III) levels. For optimum recovery of Cr(III), different analytical factors such as pH, amount of coprecipitant, centrifugation rate and time, and effect of sample volume, were investigated. The influences of some anions, cations, and transition metals on the recoveries were also investigated, and no significant interferences were observed. The preconcentration factor was 100. The detection limit based on 3 times standard deviation (sigma) of the blank (n = 10) for Cr(III) was 0.50 microg/L. In order to evaluate the accuracy of the method, certified reference materials (CRM-TMDW-500 Drinking Water and National Institute of Standards and Technology Standard Reference Material 1573a Tomato Leaves) were analyzed, and the results obtained were in good agreement with certified values. The presented procedure was applied for Cr speciation in various solid and liquid samples with successful results.

  20. Application of the Rietveld method to assess chromium(VI) speciation in chromite ore processing residue. (United States)

    Chrysochoou, Maria; Dermatas, Dimitris


    The Rietveld method allows the quantification of crystalline phases and amorphous material identified by X-ray powder diffraction (XRPD) and other diffraction methods. The method assists in determining the speciation of contaminants in solid matrices both qualitatively and quantitatively in a statistically defensible approach, as it does not focus on a microscale. Rietveld was applied to chromite ore processing residue (COPR), a cementitious waste containing hexavalent chromium. Calcium aluminum chromium oxide hydrates (CACs) were the crystalline phases identified by XRPD that bind Cr(6+) in COPR according to their chemical formula. Rietveld quantification, combined with mass balances on Cr(6+), showed that CACs may bind Cr(6+) in variable percentages, ranging from 25% to 85%. Analysis of duplicate samples showed that material variability is the predominant factor of uncertainty in evaluating the role of CACs in Cr(6+) speciation, provided that a consistent quantification strategy is pursued. The choice of strategy was performed on the basis of the pertinent literature, preliminary analyses of the equipment and the software settings, and mass balances. The correlation between the average CAC-bound Cr(6+) concentration and the total Cr(6+) for five samples (R(2)=0.94), extracted from different zones and soil borings, suggests that CACs are a primary sink for Cr(6+) in COPR.

  1. Comparison of Mercury Measurement Methods Using Two Active Filter Measurement Methods and a Tekran Speciation Unit (United States)

    Pierce, A.; Gustin, M. S.; Huang, J.; Heidecorn, K.


    Three active mercury (Hg) measurement methods were operated side by side at an urban site (University of Nevada, Reno College of Agriculture Greenhouse facility, elev. 1370 m) in Reno, and at a high elevation site (Peavine Peak, elev. 2515 m) adjacent to Reno from December 2013 to October 2014. A model 602 BetaPlus Teledyne Advanced Pollution Instrumentation (TAPI, San Diego, CA USA) particulate measurement system was used to collect particulate matter on a 47 mm diameter cation exchange membrane (CEM, PN# MSTGS3R Mustang S, Pall Corp. Port Washington, NY) at a rate of 16.7 lpm for 24 hours to four days. Particulate concentrations were calculated using beta attenuation across the filters (non-destructive to filter material); the CEM filters were then analyzed for total Hg on a Tekran Total Hg Analysis system (model 2600, Tekran Instruments Corp. Knoxville, TN, USA). Concurrently, samples were collected on an active Hg membrane system. The active Hg membrane system consisted of 3 CEM filters sampling at a rate of 1 lpm for one to two weeks. CEM filters were then analyzed on the Tekran 2600. A Tekran speciation unit (model 1130, 1135, 2537) was also in operation and ambient air samples were analyzed for gaseous elemental Hg (GEM), gaseous oxidized Hg (GOM), and particulate bound Hg (PBM). Both the 602 BetaPlus system and the active Hg membrane system should collect RM on the CEM filters. The active Hg membrane system most likely captures mainly GOM based on previous tests with the Teflon inlet setup that indicated there was high static electricity effective in removing particulate matter. Flow rate and length of measurement (24 hours vs. four days) affected the Hg concentrations on the 602 BetaPlus system. Based on these measurements we hypothesize that, due to the high flow rate, and therefore short retention time, the 602 BetaPlus only captured PBM. It is also possible that there was loss of Hg to inlet walls due to the longer inlet on the 602 BetaPlus system

  2. Estimating forest canopy bulk density using six indirect methods (United States)

    Robert E. Keane; Elizabeth D. Reinhardt; Joe Scott; Kathy Gray; James Reardon


    Canopy bulk density (CBD) is an important crown characteristic needed to predict crown fire spread, yet it is difficult to measure in the field. Presented here is a comprehensive research effort to evaluate six indirect sampling techniques for estimating CBD. As reference data, detailed crown fuel biomass measurements were taken on each tree within fixed-area plots...

  3. Isentropic Bulk Modulus: Development of a Federal Test Method (United States)


    bulk modulus space from synthetic iso -paraffinic fuels to petroleum-based diesel fuels. The test fuels are identified in Table 1. A testing order and...13000 100 14000 100 15000 100 UNCLASSIFIED UNCLASSIFIED 7 3.3 ROUND ROBIN PROCEDURE The following notes were provided to the participating...2 Table A-1. Sample 6065 at 35 °C Density psi 1000 2000 3000 4000 5000 6000 7000 8000 9000 10000 11000 12000 13000 14000 15000 Avg g/cm3

  4. Exact and heuristic methods to solve the berth allocation problem in bulk ports


    Umang, Nitish; Bierlaire, Michel; Vacca, Ilaria


    While significant contributions have been made in the use of operations research methods and techniques to optimize container terminals, relatively less attention has been directed to bulk ports. In this paper, we consider the problem of allocating vessels along the quay in a bulk port for hybrid berth layout and dynamic vessel arrivals. A key difference that distinguishes the berth allocation problem in bulk ports from that in container terminals is the presence of fixed specialized equipmen...

  5. A Comparison of Bulk Aerodynamic Methods for Calculating Air-Sea Flux

    National Research Council Canada - National Science Library

    Eleuterio, Daniel


    The Louis et al. (1982) bulk aerodynamic method for air-sea flux estimates is currently used in mesoscale models such as COAMPS, while the TOGA-COARE method is a state of the art flux parameterization involving recent...

  6. Systems and Methods for Implementing Bulk Metallic Glass-Based Macroscale Compliant Mechanisms (United States)

    Hofmann, Douglas C. (Inventor); Agnes, Gregory (Inventor)


    Systems and methods in accordance with embodiments of the invention implement bulk metallic glass-based macroscale compliant mechanisms. In one embodiment, a bulk metallic glass-based macroscale compliant mechanism includes: a flexible member that is strained during the normal operation of the compliant mechanism; where the flexible member has a thickness of 0.5 mm; where the flexible member comprises a bulk metallic glass-based material; and where the bulk metallic glass-based material can survive a fatigue test that includes 1000 cycles under a bending loading mode at an applied stress to ultimate strength ratio of 0.25.

  7. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Jian [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Sengupta, Mrinal K. [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Thermo Fisher Scientific, Dionex Products, 445 Lakeside Drive, Sunnyvale, CA, 94085 (United States); Yuan, Dongxing [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Dasgupta, Purnendu K., E-mail: [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States)


    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  8. A new method of determining the reversible magnetization loop of bulk high-temperature superconductors

    NARCIS (Netherlands)

    Ermolaev, YS; Rudnev, IA


    A new method of calculation of the magnetization loop of bulk high-temperature superconductors is proposed which employs the results of measurements of the magnetic levitation force. (C) 2004 MAIK "Nauka / Interperiodica".

  9. Bulk superhard B-C-N nanocomposite compact and method for preparing thereof (United States)

    Zhao, Yusheng; He, Duanwei


    Bulk, superhard, B-C-N nanocomposite compact and method for preparing thereof. The bulk, superhard, nanocomposite compact is a well-sintered compact and includes nanocrystalline grains of at least one high-pressure phase of B-C-N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compact has a Vicker's hardness of about 41-68 GPa. It is prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture, and sintering the encapsulated ball-milled mixture at a pressure of about 5-25 GPa and at a temperature of about 1000-2500 K.

  10. Carrier element-free coprecipitation (CEFC) method for the separation, preconcentration and speciation of chromium using an isatin derivative. (United States)

    Bulut, Volkan Numan; Ozdes, Duygu; Bekircan, Olcay; Gundogdu, Ali; Duran, Celal; Soylak, Mustafa


    A new, simple, rapid and sensitive separation, preconcentration and speciation procedure for chromium in environmental liquid and solid samples has been established. The present speciation procedure for Cr(III) and Cr(VI) is based on combination of carrier element-free coprecipitation (CEFC) and flame atomic absorption spectrometric (FAAS) determinations. In this method a newly synthesized organic coprecipitant, 5-chloro-3-[4-(trifluoromethoxy) phenylimino]indolin-2-one (CFMEPI), was used without adding any carrier element for coprecipitation of chromium(III). After reduction of chromium(VI) by concentrated H(2)SO(4) and ethanol, the procedure was applied for the determination of total chromium. Chromium(VI) was calculated as the difference between the amount of total chromium and chromium(III). The optimum conditions for coprecipitation and speciation processes were investigated on several commonly tested experimental parameters, such as pH of the solution, amount of coprecipitant, sample volume, etc. No considerable interference was observed from the other investigated anions and cations, which may be found in natural water samples. The preconcentration factor was found to be 40. The detection limit for chromium(III) corresponding to three times the standard deviation of the blank (N=10) was found 0.7 microg L(-1). The present procedure was successfully applied for speciation of chromium in several liquid and solid environmental samples. In order to support the accuracy of the method, the certified reference materials (CRM-TMDW-500 Drinking Water and CRM-SA-C Sandy Soil C) were analyzed, and standard APDC-MIBK liquid-liquid extraction method was performed. The results obtained were in good agreement with the certified values.

  11. Methods for Investigating Mercury Speciation, Transport, Methylation, and Bioaccumulation in Watersheds Affected by Historical Mining (United States)

    Alpers, C. N.; Marvin-DiPasquale, M. C.; Fleck, J.; Ackerman, J. T.; Eagles-Smith, C.; Stewart, A. R.; Windham-Myers, L.


    Many watersheds in the western U.S. have mercury (Hg) contamination from historical mining of Hg and precious metals (gold and silver), which were concentrated using Hg amalgamation (mid 1800's to early 1900's). Today, specialized sampling and analytical protocols for characterizing Hg and methylmercury (MeHg) in water, sediment, and biota generate high-quality data to inform management of land, water, and biological resources. Collection of vertically and horizontally integrated water samples in flowing streams and use of a Teflon churn splitter or cone splitter ensure that samples and subsamples are representative. Both dissolved and particulate components of Hg species in water are quantified because each responds to different hydrobiogeochemical processes. Suspended particles trapped on pre-combusted (Hg-free) glass- or quartz-fiber filters are analyzed for total mercury (THg), MeHg, and reactive divalent mercury. Filtrates are analyzed for THg and MeHg to approximate the dissolved fraction. The sum of concentrations in particulate and filtrate fractions represents whole water, equivalent to an unfiltered sample. This approach improves upon analysis of filtered and unfiltered samples and computation of particulate concentration by difference; volume filtered is adjusted based on suspended-sediment concentration to minimize particulate non-detects. Information from bed-sediment sampling is enhanced by sieving into multiple size fractions and determining detailed grain-size distribution. Wet sieving ensures particle disaggregation; sieve water is retained and fines are recovered by centrifugation. Speciation analysis by sequential extraction and examination of heavy mineral concentrates by scanning electron microscopy provide additional information regarding Hg mineralogy and geochemistry. Biomagnification of MeHg in food webs is tracked using phytoplankton, zooplankton, aquatic and emergent vegetation, invertebrates, fish, and birds. Analysis of zooplankton in

  12. Speciation of Dissolved Cadmium

    DEFF Research Database (Denmark)

    Holm, Peter Engelund; Andersen, Sjur; Christensen, Thomas Højlund


    Equilibrium dialysis and ion exchange methods, as well as computer calculations (GEOCHEM), were applied for speciation of dissolved cadmium (Cd) in test solutions and leachate samples. The leachate samples originated from soil, compost, landfill waste and industrial waste. The ion exchange (IE...... leachates showed different Cd speciation patterns as expected. Some leachates were dominated by free divalent Cd (1-70%), some by inorganic complexes (1-87%), and some by organic complexes (7-98%)....

  13. Anthropogenic VOC speciation in emission inventories: a method for improvement and evaluation (United States)

    von Schneidemesser, E.; D'angiola, A.; Granier, C.; Monks, P. S.; Law, K.


    Volatile organic compounds (VOCs) are important precursor compounds for the formation of ozone and other secondary organic aerosols. Anthropogenic sources of VOCs are dominated by industrial usage and transportation sources, the latter being extremely important in urban areas. Megacities and large urban conglomerations are emission hot spots that exert disproportionately large adverse health effects on the population and surrounding environment, owing to their high population density and concentrated emission sources. Exceedances of ozone air quality standards are a problem in many urban areas. Improvements in the modelling of ozone precursors would benefit our understanding of the impact of changes in emissions and the effect of future legislation on air quality. As many VOCs are extremely reactive in the atmosphere and have high ozone forming potential, improved speciation of VOCs in models could lead to better predictions of ozone levels and secondary organic aerosol formation. Previously, VOC and carbon monoxide (CO) data from urban areas around the world were compared. Significant differences in VOC concentrations were observed, however, when normalized to CO, the VOC-CO ratios were similar for many locations and over time, even as emission reductions were implemented. The largest variation was found in the lighter alkanes due to the use of alternative transportation fuels in various world regions. These ratios were grouped by region and used to develop a new speciation for surface emissions of VOCs, by applying the regional observed VOC-CO ratios to the CO emissions for the urban areas. Urban areas were defined as 150 inhabitants per km2 or greater. Model simulations were performed using the MOZART-4 chemistry transport model to assess the improved speciation of the VOC emissions. The model outputs were compared to urban observational data where available. The impact of the new speciation of the distribution of CO, OH and ozone at the global scale will be

  14. Effect of the method for producing Cu–Cr3C2 bulk composites on ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 5. Effect of the method for producing Cu–Cr 3 C 2 bulk composites on the structure and properties ... A composite obtained bythe MPC of the powders synthesized using solid-phase mechano synthesis (MS) (copper, chromium and graphite) had thehighest ...

  15. Use of thermal neutron reflection method for chemical analysis of bulk samples

    Energy Technology Data Exchange (ETDEWEB)

    Papp, A., E-mail: [Institute of Nuclear Research of the Hungarian Academy of Sciences, (ATOMKI), 4001 Debrecen, Pf. 51 (Hungary); Csikai, J. [Institute of Nuclear Research of the Hungarian Academy of Sciences, (ATOMKI), 4001 Debrecen, Pf. 51 (Hungary); Institute of Experimental Physics, University Debrecen (IEP), 4010 Debrecen-10, Pf. 105 (Hungary)


    Microscopic, σ{sub β}, and macroscopic, Σ{sub β}, reflection cross-sections of thermal neutrons averaged over bulk samples as a function of thickness (z) are given. The σ{sub β} values are additive even for bulk samples in the z=0.5–8 cm interval and so the σ{sub βmol}(z) function could be given for hydrogenous substances, including some illicit drugs, explosives and hiding materials of ∼1000 cm{sup 3} dimensions. The calculated excess counts agree with the measured R(z) values. For the identification of concealed objects and chemical analysis of bulky samples, different neutron methods need to be used simultaneously. - Highlights: • Check the proposed analytical expression for the description of the flux. • Determination of the reflection cross-sections averaged over bulk samples. • Data rendered to estimate the excess counts for various materials.

  16. Speciation of arsenic by IC-ICP-MS: future standard method and its application on baby food samples

    DEFF Research Database (Denmark)

    Kollander, Barbro; Sloth, Jens Jørgen

    of the intended murder. For example the organic compound arsenobetaine, the main arsenic species in marine organisms, is regarded as basically harmless to humans while the inorganic forms of arsenic, arsenite and arsenate found in rice, are toxic. To enable the evaluation of the true toxicity from arsenic in food......, some kind of speciation analysis has to be performed. In this work, the concentration of inorganic arsenic in some baby food samples is evaluated. The applied methodology has recently been tested in a collaborative trial as a candidate standardized method for the determination of inorganic arsenic...

  17. Depth of cure of resin composites: is the ISO 4049 method suitable for bulk fill materials? (United States)

    Flury, Simon; Hayoz, Stefanie; Peutzfeldt, Anne; Hüsler, Jürg; Lussi, Adrian


    To evaluate if depth of cure D(ISO) determined by the ISO 4049 method is accurately reflected with bulk fill materials when compared to depth of cure D(new) determined by Vickers microhardness profiles. D(ISO) was determined according to "ISO 4049; Depth of cure" and resin composite specimens (n=6 per group) were prepared of two control materials (Filtek Supreme Plus, Filtek Silorane) and four bulk fill materials (Surefil SDR, Venus Bulk Fill, Quixfil, Tetric EvoCeram Bulk Fill) and light-cured for either 10s or 20s. For D(new), a mold was filled with one of the six resin composites and light-cured for either 10 s or 20 s (n=22 per group). The mold was placed under a microhardness indentation device and hardness measurements (Vickers hardness, VHN) were made at defined distances, beginning at the resin composite that had been closest to the light-curing unit (i.e. at the "top") and proceeding toward the uncured resin composite (i.e. toward the "bottom"). On the basis of the VHN measurements, Vickers hardness profiles were generated for each group. D(ISO) varied between 1.76 and 6.49 mm with the bulk fill materials showing the highest D(ISO). D(new) varied between 0.2 and 4.0 mm. D(new) was smaller than D(ISO) for all resin composites except Filtek Silorane. For bulk fill materials the ISO 4049 method overestimated depth of cure compared to depth of cure determined by Vickers hardness profiles. Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  18. Interferometric method for quantitatively testing the RadOptic effect in bulk semiconductors (United States)

    Peng, Bo-dong; Song, Yan; Hei, Dong-wei; Zhao, Jun


    For the quantitative investigation of MeV-photon-induced changes in the refractive indices of bulk semiconductors, a model was established to describe the evolution of the excess carrier density, including the generation and recombination processes. The two key parameters of the evolution model, namely, the summed injection intensity and the gamma intensity curve, were obtained via dose measurements and gamma pulse monitoring, respectively. An interferometric method of measuring instantaneous changes in the refractive index and obtaining real-time measurements of the excess carrier density in bulk materials was successfully implemented. The probe beam was transmitted through a single-mode fiber to form double-beam interference in a slab geometry. Two bulk samples, one consisting of intrinsic GaAs and one of intrinsic ZnO, were tested. The recombination time constant of the intrinsic GaAs sample was found to be approximately 0.6 ns and did not vary distinctly with the photon energy, whereas the ZnO sample's recombination behavior consisted of two components. The short component was evident when short and intense pulses were incident, whereas the long component dominated under long and relatively weak pulses. The method reported in this work can be used to study the excess carrier dynamics induced by pulsed gamma radiation and to investigate the mechanisms of refractive index modulation under pulsed gamma conditions; thus, it is expected to be beneficial for guiding the development of RadOptic systems based on bulk materials.

  19. Mercury speciation in coastal sediments from the central east coast of India by modified BCR method.

    Digital Repository Service at National Institute of Oceanography (India)

    Chakraborty, P.; Babu, P.V.R.; Vudamala, K.; Ramteke, D.; Chennuri, K.

    and bioavailability of Hg in sediments is very much dependent on its chemical speciation rather than its total concentrations in the sediments. Non‐residual/dynamic complexes of Hg, methylmercury (CH3Hg+) in sediments are expected to have strong biological impacts... is not industrially developed. The approximate population of this city is ~50,000. Vishakhapatnam (VSKP) is the second largest city in the state of Andhra Pradesh and the third largest city (after Kolkata and Chennai) in the east coast of India. VSKP has become a...

  20. Determination of prilocaine HCl in bulk drug and pharmaceutical formulation by GC-NPD method

    Directory of Open Access Journals (Sweden)

    Atila Alptug


    Full Text Available The novel analytical method was developed and validated for determination of prilocaine HCl in bulk drug and pharmaceutical formulation by gas chromatography-nitrogen phosphorus detection (GC-NPD. The chromatographic separation was performed using a HP-5MS column. The calibration curve was linear over the concentration range of 40-1000 ng ml-1 with a correlation coefficient of 0.9998. The limits of detection (LOD and quantification (LOQ of method were 10 ng ml-1 and 35 ng ml-1, respectively. The within-day and between-day precision, expressed as the percent relative standard deviation (RSD% was less than 5.0%, and accuracy (percent relative error was better than 4.0%. The developed method can be directly and easily applied for determination of prilocaine HCl in bulk drug and pharmaceutical formulation using internal standard methodology.

  1. A new method for the measurement of meteorite bulk volume via ideal gas pycnometry (United States)

    Li, Shijie; Wang, Shijie; Li, Xiongyao; Li, Yang; Liu, Shen; Coulson, Ian M.


    To date, of the many techniques used to measure the bulk volume of meteorites, only three methods (Archimedean bead method, 3-D laser imaging and X-ray microtomography) can be considered as nondestructive or noncontaminating. The bead method can show large, random errors for sample sizes of smaller than 5 cm3. In contrast, 3-D laser imaging is a high-accuracy method even when measuring the bulk volumes of small meteorites. This method is both costly and time consuming, however, and meteorites of a certain shape may lead to some uncertainties in the analysis. The method of X-ray microtomography suffers from the same problems as 3-D laser imaging. This study outlines a new method of high-accuracy, nondestructive and noncontaminating measurement of the bulk volume of meteorite samples. In order to measure the bulk volume of a meteorite, one must measure the total volume of the balloon vacuum packaged meteorite and the volume of balloon that had been used to enclose the meteorite using ideal gas pycnometry. The difference between the two determined volumes is the bulk volume of the meteorite. Through the measurement of zero porosity metal spheres and tempered glass fragments, our results indicate that for a sample which has a volume of between 0.5 and 2 cm3, the relative error of the measurement is less than ±0.6%. Furthermore, this error will be even smaller (less than ±0.1%) if the determined sample size is larger than 2 cm3. The precision of this method shows some volume dependence. For samples smaller than 1 cm3, the standard deviations are less than ±0.328%, and these values will fall to less than ±0.052% for samples larger than 2 cm3. The porosities of nine fragments of Jilin, GaoGuenie, Zaoyang and Zhaodong meteorites have been measured using our vacuum packaging-pycnometry method, with determined average porosities of Jilin, GaoGuenie, Zaoyang and Zhaodong of 9.0307%, 2.9277%, 17.5437% and 5.9748%, respectively. These values agree well with the porosities

  2. A hybrid finite volume - finite element method for bulk-surface coupled problems (United States)

    Chernyshenko, Alexey Y.; Olshanskii, Maxim A.; Vassilevski, Yuri V.


    The paper develops a hybrid method for solving a system of advection-diffusion equations in a bulk domain coupled to advection-diffusion equations on an embedded surface. A monotone nonlinear finite volume method for equations posed in the bulk is combined with a trace finite element method for equations posed on the surface. In our approach, the surface is not fitted by the mesh and is allowed to cut through the background mesh in an arbitrary way. Moreover, a triangulation of the surface into regular shaped elements is not required. The background mesh is an octree grid with cubic cells. As an example of an application, we consider the modeling of contaminant transport in fractured porous media. One standard model leads to a coupled system of advection-diffusion equations in a bulk (matrix) and along a surface (fracture). A series of numerical experiments with both steady and unsteady problems and different embedded geometries illustrate the numerical properties of the hybrid approach. The method demonstrates great flexibility in handling curvilinear or branching lower dimensional embedded structures.

  3. Development and application of an ultratrace method for speciation of organotin compounds in cryogenically archived and homogenized biological materials. (United States)

    Point, David; Davis, W Clay; Christopher, Steven J; Ellisor, Michael B; Pugh, Rebecca S; Becker, Paul R; Donard, Olivier F X; Porter, Barbara J; Wise, Stephen A


    An accurate, ultra-sensitive and robust method for speciation of mono, di, and tributyltin (MBT, DBT, and TBT) by speciated isotope-dilution gas chromatography-inductively coupled plasma-mass spectrometry (SID-GC-ICPMS) has been developed for quantification of butyltin concentrations in cryogenic biological materials maintained in an uninterrupted cryo-chain from storage conditions through homogenization and bottling. The method significantly reduces the detection limits, to the low pg g(-1) level (as Sn), and was validated by using the European reference material (ERM) CE477, mussel tissue, produced by the Institute for Reference Materials and Measurements. It was applied to three different cryogenic biological materials-a fresh-frozen mussel tissue (SRM 1974b) together with complex materials, a protein-rich material (whale liver control material, QC03LH03), and a lipid-rich material (whale blubber, SRM 1945) containing up to 72% lipids. The commutability between frozen and freeze-dried materials with regard to spike equilibration/interaction, extraction efficiency, and the absence of detectable transformations was carefully investigated by applying complementary methods and by varying extraction conditions and spiking strategies. The inter-method results enabled assignment of reference concentrations of butyltins in cryogenic SRMs and control materials for the first time. The reference concentrations of MBT, DBT, and TBT in SRM 1974b were 0.92 +/- 0.06, 2.7 +/- 0.4, and 6.58 +/- 0.19 ng g(-1) as Sn (wet-mass), respectively; in SRM 1945 they were 0.38 +/- 0.06, 1.19 +/- 0.26, and 3.55 +/- 0.44 ng g(-1), respectively, as Sn (wet-mass). In QC03LH03, DBT and TBT concentrations were 30.0 +/- 2.7 and 2.26 +/- 0.38 ng g(-1) as Sn (wet-mass). The concentration range of butyltins in these materials is one to three orders of magnitude lower than in ERM CE477. This study demonstrated that cryogenically processed and stored biological materials are a promising alternative to

  4. Use of a modified, high-sensitivity, anodic stripping voltammetry method for determination of zinc speciation in the North Atlantic Ocean. (United States)

    Jakuba, Rachel Wisniewski; Moffett, James W; Saito, Mak A


    Zinc speciation is considered to be an important determinant of the biological availability of zinc. Yet in oceanic surface waters, characterization of zinc speciation is difficult due to the low concentrations of this essential micronutrient. In this study, an anodic stripping voltammetry method previously developed for the total determination of cadmium and lead was successfully adapted to the measurement of zinc speciation. The method differs from previous zinc speciation anodic stripping voltammetry methods in that a fresh mercury film is plated with each sample aliquot. The fresh film anodic stripping voltammetry method was compared to competitive ligand exchange cathodic stripping voltammetry in a profile from the North Atlantic Ocean. Results using the fresh film anodic stripping voltammetry method were similar to those determined using the cathodic stripping voltammetry method, though ligand concentrations determined by fresh film anodic stripping voltammetry were generally slightly higher than those determined by cathodic stripping voltammetry. There did not seem to be a systematic difference between methods for the estimates of conditional stability constants. The ligand concentration in the North Atlantic profile ranged from 0.9 to 1.5 nmol L(-1) as determined by fresh film anodic stripping voltammetry and 0.6 to 1.3 nmol L(-1) as determined by cathodic stripping voltammetry. The conditional stability constants determined by fresh film anodic stripping voltammetry were 10(9.8)-10(10.5) and by cathodic stripping voltammetry were 10(9.8)-10(11.3).

  5. Speciation Analysis of Radionuclides in the Environment - NSK-B SPECIATION project report 2009

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Aldahan, Ala; Possnert, Göran

    The second stage of the NKS-B project SPECIATION was complemented in 2008-2009, which mainly focus on three aspects: (1) Further improvement and development of methods for speciation analysis of radionuclides; (2) Investigation of speciation of some radionuclides in the environment (water......, sediments, particles); and (3) Intercomparison excise for speciation analysis of radionu-clides in soil and sediment. This report summarizes the work completed in the project partners’ laboratories, Method developments include: Development of an rapid and in-suit separation method for the speciation...... analysis of 129I in seawater samples; Development of a simple method for the speciation analysis of 129I in fresh water and seawater samples; Development of an on-line HPLC-ICP-MS method for the direct speciation analysis of 127I in water and leachate samples; Speciation of radionuclides in water includes...

  6. Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt


    by a factor of four by continuously introducing carbon as methanol via the mobile phase into the ICP. Sources of error in the HPLC system (column overload), in the sample introduction system (memory by organic solvents) and in the ICP-MS (spectroscopic interferences) and their prevention are also discussed...... speciation in the shrimp sample. With this analytical technique the HPLC retention time in combination with mass analysis of the molecular ions and their collision-induced fragments provide almost conclusive evidence of the identity of the analyte species. The speciation methods are validated by establishing...

  7. Validation and method development of Tadalafil in bulk and tablet dosage form by RP-HPLC. (United States)

    Bojanapu, A; Subramaniam, A T; Munusamy, J; Dhanapal, K; Chennakesavalu, J; Sellappan, M; Jayaprakash, V


    A novel, precise, rapid and sensitive reverse phase high performance liquid chromatographic method has been developed for the validated estimation of Tadalafil in bulk and tablet dosage form. The separation was achieved on Agilent Eclipse XDB C18 column (150 mm×4.6 mm, 5 µ) using a mobile phase that consists of the buffer (potassium dihydrogen orthophosphate) and acetonitrile in the ration of 50:50 V/V, pH 6 was adjusted with orthophosphoric acid. The flow rate was maintained at 1.2 ml/min and the detection wavelength was 285 nm. The method was validated for linearity, specificity, sensitivity as per ICH guidelines. The retention time was found to be 3.181 for Tadalafil. The calibration curve was linear over the concentration range of 10-150 µg/ml. The % RSD was satisfactory which showed the method found to be reliable. The high percentage recovery confirmed the suitability of the method for estimation of Tadalafil in pharmaceutical dosage form. The developed method could be applicable for routine analysis of Tadalafil in bulk and tablet dosage form. © Georg Thieme Verlag KG Stuttgart · New York.

  8. A GaN bulk crystal with improved structural quality grown by the ammonothermal method. (United States)

    Hashimoto, Tadao; Wu, Feng; Speck, James S; Nakamura, Shuji


    The realization of high-performance optoelectronic devices, based on GaN and other nitride semiconductors, requires the existence of a high-quality substrate. Non-polar or semipolar substrates have recently been proven to provide superior optical devices to those on conventional c-plane substrates. Bulk GaN growth enables GaN substrates sliced along various favourable crystal orientations. Ammonothermal growth is an attractive method for bulk GaN growth owing to its potential to grow GaN ingots at low cost. Here we report on improvement in the structural quality of GaN grown by the ammonothermal method. The threading dislocation densities estimated by plan-view transmission electron microscopy observations were less than 1 x 10(6) cm(-2) for the Ga face and 1 x 10(7) cm(-2) for the N face. No dislocation generation at the interface was observed on the Ga face, although a few defects were generated at the interface on the N face. The improvement in the structural quality, together with the previous report on growth rate and scalability, demonstrates the commercial feasibility of the ammonothermal GaN growth.

  9. Method for Manufacturing Bulk Metallic Glass-Based Strain Wave Gear Components (United States)

    Hofmann, Douglas C. (Inventor); Wilcox, Brian H. (Inventor)


    Systems and methods in accordance with embodiments of the invention implement bulk metallic glass-based strain wave gears and strain wave gear components. In one embodiment, a method of fabricating a strain wave gear includes: shaping a BMG-based material using a mold in conjunction with one of a thermoplastic forming technique and a casting technique; where the BMG-based material is shaped into one of: a wave generator plug, an inner race, an outer race, a rolling element, a flexspline, a flexspline without a set of gear teeth, a circular spline, a circular spline without a set of gear teeth, a set of gear teeth to be incorporated within a flexspline, and a set of gear teeth to be incorporated within a circular spline.

  10. Efficient method for storage of long conveyor belts passages inside the bulk containers

    Directory of Open Access Journals (Sweden)



    Full Text Available The paper introduces the family of the algorithms designed to improve the process of winding up the long conveyor belt passages on reels located inside the bulk containers, used for i.e. rail transport. The proposed method provides the convenient storage technique of the long belt passages , enabling their transport on the standardized rail wagons. Presented solution also addresses the problems related with binding the smaller belt passages, such as shorter life span in comparison to the single-part belt. Moreover, the presented work contains not only the details of the two algorithms representative for the proposed method, but also the outlook of the system of the automatic control required for the successful application of the proposed technique.

  11. Bulk Electrical Cable Non-Destructive Examination Methods for Nuclear Power Plant Cable Aging Management Programs

    Energy Technology Data Exchange (ETDEWEB)

    Glass, Samuel W. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Jones, Anthony M. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Fifield, Leonard S. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hartman, Trenton S. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)


    This Pacific Northwest National Laboratory milestone report describes progress to date on the investigation of nondestructive test methods focusing particularly on bulk electrical test methods that provide key indicators of cable aging and damage. The work includes a review of relevant literature as well as hands-on experimental verification of inspection capabilities. As nuclear power plants consider applying for second, or subsequent, license renewal to extend their operating period from 60 years to 80 years, it is important to understand how the materials installed in plant systems and components will age during that time and develop aging management programs to assure continued safe operation under normal and design basis events (DBE). Normal component and system tests typically confirm the cables can perform their normal operational function. The focus of the cable test program, however, is directed toward the more demanding challenge of assuring the cable function under accident or DBE. The industry has adopted 50% elongation at break (EAB) relative to the un-aged cable condition as the acceptability standard. All tests are benchmarked against the cable EAB test. EAB, however, is a destructive test so the test programs must apply an array of other nondestructive examination (NDE) tests to assure or infer the overall set of cable’s system integrity. Assessment of cable integrity is further complicated in many cases by vendor’s use of dissimilar material for jacket and insulation. Frequently the jacket will degrade more rapidly than the underlying insulation. Although this can serve as an early alert to cable damage, direct test of the cable insulation without violating the protective jacket becomes problematic. This report addresses the range of bulk electrical NDE cable tests that are or could be practically implemented in a field-test situation with a particular focus on frequency domain reflectometry (FDR). The FDR test method offers numerous advantages

  12. Bulk Crystal Growth of Nonlinear Optical Organic Materials Using Inverted Vertical Gradient Freeze Method (United States)

    Choi, J.; Cruz, Magda; Metzl, R.; Wang, W. S.; Aggarwal, M. D.; Penn, Benjamin G.; Frazier, Donald O.


    A new process for producing large bulk single crystals of benzil (C6H5COCOC6H5) is reported in this paper. Good quality crystals have been successfully grown using this approach to crystal growth. This method seems to be very promising for other thermally stable NLO organic materials also. The entire contents vycor crucible 1.5 inch in diameter and 2 inch deep was converted to single crystal. Purity of the starting growth material is also an important factor in the final quality of the grown crystals. The entire crystal can be very easily taken out of the crucible by simple maneuvering. Initial characterization of the grown crystals indicated that the crystals are as good as other crystals grown by conventional Bridgman Stockbarger technique.

  13. Elemental Analysis and Comparison of Bulk Soil Using LA-ICP-MS and LIBS methods (United States)

    Almirall, J.


    Elemental analysis methods utilizing Laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) and laser-induced breakdown spectroscopy (LIBS) were developed and used in the characterization of soil samples from the US and Canada as part of a comprehensive forensic evaluation of soils. A LA-ICP-MS method was recently optimized for analysis and comparison between different soil samples in an environmental forensic application [1,2] and LIBS has recently attracted the interest of analytical chemists and forensic laboratories as a simpler, lower cost alternative to the more established analytical methods. In developing a LIBS method, there are many parameters to consider, including laser wavelength, spectral resolution, sensitivity, and matrix effects. The first LIBS method using a 266 nm laser for forensic soil analysis has also been recently reported by our group [3]. The results of an inter-laboratory comparison involving thirteen (13) laboratories conducting bulk elemental analysis by various methods are also reported. The aims of the inter-laboratory tests were: a) to evaluate the inter-laboratory performance of three methods (LA-ICP-MS, µXRF and LIBS) in terms of accuracy (bias), precision (relative standard deviation, RSD) and sensitivity using standard reference materials (SRMs); b) to evaluate the newly released NIST SRM 2710a, which supersedes 2710; and c) to evaluate the utility of LIBS as an alternative technique to LA-ICP-MS and µXRF for bulk analysis of soils. Each sample and standard was homogenized in a high-speed ball mill and pressed into pellets. Participants were instructed to measure the following elements: 7Li, 25Mg, 27Al, 42Ca, 45Sc, 47,49Ti, 51V, 55Mn, 88Sr, 137Ba, 206,207,208 Pb (LA-ICP-MS); Ti, Cr, Mn, Fe, Cu, Sr, Zr, Pb (µXRF); Ba, Cr, Cu, Fe, Li, Mg, Mn, Pb, Sr, Ti, Zr (LIBS). For both LIBS and µXRF, the choice of appropriate spectral lines was determined by the user, optimizing for linearity, sensitivity and precision

  14. Method development, validation and stability study of ritonavir in bulk and pharmaceutical dosage form by spectrophotometric method

    Directory of Open Access Journals (Sweden)

    Anindita Behera


    Full Text Available Background: Ritonavir is a protease inhibitor and mostly used as a booster for increasing the bioavailability of other protease inhibitors like Atazanavir Sulfate and Lopinavir. Aims: Quality assessment of the new dosage form of Ritonavir i.e. tablets is very essential, so two sensitive, simple and precise methods are developed for quantification of Ritonavir in bulk and tablet dosage forms. Materials and Methods: The first method is based on first order derivative method and the second is based on area under curve method. Both the methods are validated according to international conference of harmonization (ICH guidelines. A stability study of Ritonavir is done in UV - Visible Spectrophotometer under different stress conditions recommended by ICH guidelines. Results: The absorption maximum is found to be 239nm in methanol. The absorption maximum in first method is chosen at 253.2nm, and the linearity is found between 4 - 20 ΅g/ml with coefficient of correlation value 0.9981. In the second method, the range for area under curve selected is 237 - 242nm. The linearity is found between 4 -20 ΅g/ml with coefficient of correlation value 0.9992. Conclusion: The developed methods are validated and found to be simple, rapid, precise and cost-effective. The degradation study in tablet dosage form can be used as a stability indicating assay method.

  15. A Method for Chemical Characterization of the Ambient Organic Aerosol Soluble in Water by Group Speciation: Results From Urban Atlanta (United States)

    Weber, R. J.; Sullivan, A. P.


    Due to the chemical complexity of the organic fraction of ambient particles complete chemical speciation by single component analysis is currently not possible. This is especially true for polar compounds traditionally measured via a derivatization step prior to GC-MS analysis. However, with minor modifications, the application of existing methods for measuring natural organic matter (NOM) to atmospheric particles soluble in water can provide new insights into a large fraction of the ambient carbonaceous aerosol. This paper describes and reports results from a recently developed method that uses a two-step solid phase extraction (SPE) process with total organic carbon (TOC) detection. The method is capable of quantifying, by chemical group, approximately 80 percent of the water-soluble organic carbon (WSOC) in fine (PM2.5) ambient aerosol particles. During summer, this can be from 50 to 70 percent of the total organic aerosol. The chemical groups of WSOC that are quantified are an aliphatic group that is subdivided into acids with less than four to five carbons, neutrals, and bases, and an aromatic group that is divided into acids and phenols. Aspects of this separation method have been confirmed by C-NMR (Carbon - Nuclear Magnetic Resonance). The method is employed to characterize the summer organic aerosol in urban Atlanta Georgia and surrounding area by extraction and analysis of 24-hour integrated HiVol filter samples. Measurements at two sites are compared to a downtown site. One site was located next to a major highway, the other in a rural setting approximately 60 km west of the urban center. The preliminary results suggest most of the compounds that comprise the WSOC fraction are the secondary products of mobile source emissions.

  16. 3D computation of non-linear eddy currents: Variational method and superconducting cubic bulk (United States)

    Pardo, Enric; Kapolka, Milan


    Computing the electric eddy currents in non-linear materials, such as superconductors, is not straightforward. The design of superconducting magnets and power applications needs electromagnetic computer modeling, being in many cases a three-dimensional (3D) problem. Since 3D problems require high computing times, novel time-efficient modeling tools are highly desirable. This article presents a novel computing modeling method based on a variational principle. The self-programmed implementation uses an original minimization method, which divides the sample into sectors. This speeds-up the computations with no loss of accuracy, while enabling efficient parallelization. This method could also be applied to model transients in linear materials or networks of non-linear electrical elements. As example, we analyze the magnetization currents of a cubic superconductor. This 3D situation remains unknown, in spite of the fact that it is often met in material characterization and bulk applications. We found that below the penetration field and in part of the sample, current flux lines are not rectangular and significantly bend in the direction parallel to the applied field. In conclusion, the presented numerical method is able to time-efficiently solve fully 3D situations without loss of accuracy.

  17. Method for Vanadium Speciation in Aqueous Samples by HPLC-ICP ...

    African Journals Online (AJOL)


    methods can only measure the total concentration of vanadium, or one of the two vanadium species, particularly V(V).4–6 Some two-step methods for the determination of the two vanadium species7–10 have been proposed by several groups. These methods normally measure one of the two species in one step, and in the.

  18. Speciative determination of total V and dissolved inorganic vanadium species in environmental waters by catalytic–kinetic spectrophotometric method

    Directory of Open Access Journals (Sweden)

    Ramazan Gürkan


    Full Text Available A kinetic determination of V(V as a catalyst was spectrophotometrically performed by using the indicator reaction of Gallamine blue (GB+ and bromate at pH 2.0. The reaction was followed by measuring absorbance change for a fixed-time of 3 min at 537 nm. The variables such as reagent concentration, pH, buffer concentration, ionic strength and temperature were optimized to improve the selectivity and sensitivity. Under the optimized conditions, the determination of V(V was performed in the range 1–100 μg L−1 with limits of detection and quantification of 0.31 and 0.94 μg L−1. The developed kinetic method is sufficiently sensitive, selective and simple. It was successfully applied to the speciative determination of total V and inorganic dissolved vanadium species, V(V and V(IV in environmental water samples. The oxidizing property of permanganate is used to differentiate between V(IV and V(V species. The V(IV content was found by subtracting the V(V content from those of total V. The recovery is above 95% for V(V spiked samples. Additionally, the accuracy was validated by analysis of a certified water sample, CRM TMDA-53.3, and the results were in good agreement with the certified value.

  19. Bulk synthesis of monodisperse magnetic FeNi3 nanopowders by flow levitation method. (United States)

    Chen, Shanjun; Chen, Yan; Kang, Xiaoli; Li, Song; Tian, Yonghong; Wu, Weidong; Tang, Yongjian


    In this work, a novel bulk synthesis method for monodisperse FeNi3 nanoparticles was developed by flow levitation method (FL). The Fe and Ni vapours ascending from the high temperature levitated droplet was condensed by cryogenic Ar gas under atmospheric pressure. X-ray diffraction was used to identify and characterize the crystal phase of prepared powders exhibiting a FeNi3 phase. The morphology and size of nanopowders were observed by transmission electron microscopy (TEM). The chemical composition of the nanoparticles was determined with energy dispersive spectrometer (EDS). The results indicated that the FeNi3 permalloy powders are nearly spherical-shaped with diameter about 50-200 nm. Measurement of the magnetic property of nanopowders by a superconducting quantum interference device (SQUID, Quantum Design MPMS-7) showed a symmetric hysteresis loop of ferromagnetic behavior with coercivity of 220 Oe and saturation magnetization of 107.17 emu/g, at 293 K. At 5 K, the obtained saturation magnetization of the sample was 102.16 emu/g. The production rate of FeNi3 nanoparticles was estimated to be about 6 g/h. This method has great potential in mass production of FeNi3 nannoparticles.

  20. Bulk Synthesis and Characterization of Ti3Al Nanoparticles by Flow-Levitation Method

    Directory of Open Access Journals (Sweden)

    Shanjun Chen


    Full Text Available A novel bulk synthesis method for preparing high pure Ti3Al nanoparticles was developed by flow-levitation method (FL. The Ti and Al vapours ascending from the high temperature levitated droplet were condensed by cryogenic Ar gas under atmospheric pressure. The morphology, crystalline structure, and chemical composition of Ti3Al nanoparticles were, respectively, investigated by transmission electron microscopy, X-ray diffraction, and inductively coupled plasma atomic emission spectrometry. The results indicated that the Ti3Al powders are nearly spherical-shaped, and the particle size ranges from several nanometers to 100 nm in diameter. Measurements of the d-spacing from X-ray (XRD and electron diffraction studies confirmed that the Ti3Al nanoparticles have a hexagonal structure. A thin oxidation coating of 2-3 nm in thickness was formed around the particles after exposure to air. Based on the XPS measurements, the surface coating of the Ti3Al nanoparticles is a mixture of Al2O3 and TiO2. The production rate of Ti3Al nanoparticles was estimated to be about 3 g/h. This method has a great potential in mass production of Ti3Al nanoparticles.

  1. Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    Garima Balwani


    Full Text Available A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1 and 0.010 μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2% and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

  2. Predicting the effective response of bulk polycrystalline ferroelectric ceramics via improved spectral phase field methods (United States)

    Vidyasagar, A.; Tan, W. L.; Kochmann, D. M.


    Understanding the electromechanical response of bulk polycrystalline ferroelectric ceramics requires scale-bridging approaches. Recent advances in fast numerical methods to compute the homogenized mechanical response of materials with heterogeneous microstructure have enabled the solution of hitherto intractable systems. In particular, the use of a Fourier-based spectral method as opposed to the traditional finite element method has gained significant interest in the homogenization of periodic microstructures. Here, we solve the periodic, electro-mechanically-coupled boundary value problem at the mesoscale of polycrystalline ferroelectrics in order to extract the effective response of barium titanate (BaTiO3) and lead zirconate titanate (PZT) under applied electric fields. Results include the effective electric hysteresis and the associated butterfly curve of strain vs. electric field for mean stress-free electric loading. Computational predictions of the 3D polycrystalline response show convincing agreement with our experimental electric cycling and strain hysteresis data for PZT-5A. In addition to microstructure-dependent effective physics, we also show how finite-difference-based approximations in the spectral solution scheme significantly reduce instability and ringing phenomena associated with spectral techniques and lead to spatial convergence with h-refinement, which have been major challenges when modeling high-contrast systems such as polycrystals.

  3. Spectrophotometric and spectrofluorimetric methods for the determination of saxagliptin and vildagliptin in bulk and pharmaceutical preparations

    Directory of Open Access Journals (Sweden)

    Marwa S. Moneeb


    Full Text Available New simple and sensitive spectrophotometric and spectrofluorimetric methods have been developed and validated for the determination of saxagliptin (SAX and vildagliptin (VDG in bulk and pharmaceutical preparations. The spectrophotometric methods were based on derivatization of the investigated drugs with two reagents: 1,2-naphthoquinone-4-sulfonic acid sodium salt (NQS and 4-chloro-7-nitrobenzofurazan (NBD-Cl. For further increase in the sensitivity, the D1 spectra of the reactions products were also recorded. For NQS reaction, Beer’s law was obeyed over the ranges of 5–30 and 7–45 μg mL−1 for the absorbance readings; and 3–32 and 5–50 μg mL−1 for the derivative readings of SAX and VDG, respectively. For NBD-Cl reaction, Beer’s law was obeyed over the ranges of 3–20 and 4.5–35 μg mL−1 for the absorbance readings; and 1.5–25 and 2.5–40 μg mL−1 for the derivative readings of SAX and VDG, respectively. Spectrofluorimetric methods were developed based on the fact that the derivatized investigated drugs with NBD-Cl reagent are highly fluorescent products. The fluorescence concentration plots were linear over the ranges of 0.02–0.25 and 0.03–0.37 μg mL−1 for SAX and VDG, respectively. The fluorescence measurement enabled the detection of SAX and VDG at concentrations of about 3 and 7 ng mL−1, respectively. The proposed methods have been validated and successfully applied to the determination of the investigated drugs in their pharmaceutical preparations. The results obtained were statistically compared to those obtained from reference methods.

  4. Testing the Bergerhoff method to determine the bulk deposition loads of 49 elements (United States)

    Thöni, Lotti; Krieg, Fritz; Siewers, Ulrich

    The suitability of the simple and rather cheap Bergerhoff method for the determination of bulk deposition loads of 49 elements was tested. The method is suitable for the following elements: Ag, Al, As, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Ga, Ge, In, K, La, Li, Mg, Mn, Mo, Na, Nb, Ni, Pb, Rb, S, Sb, Sc, Se, Sn, Sr, Th, Ti, Tl, V, W, Y and Zn provided that for some of these elements one does not get total recovery with HNO 3-digestion. This, nevertheless, supplies sufficient information for most concerns. Analytical problems were encountered for the following elements: U and Te concentrations in our samples were close to the blanks; P and Ta were highly variable within the sampling areas; B, Hf and Zr leached out of the glass of the digestion vessels; Hg is highly volatile. Field studies at three background sites in Switzerland, two on the northern side of the Alps and one in the southern Alps, showed higher burdens of element emissions in the latter, partly because of higher precipitation, and partly because of higher concentrations in the dust. An anthropogenic influence can be inferred for Ag, Bi, Cd, Cu, Hg, Mo, Pb, Sb, Te, W and Zn and probably also for As, P, S (with associated Se) and Sn.

  5. Comparison and limitations of three different bulk etch rate measurement methods used for gamma irradiated PM-355 detectors

    Energy Technology Data Exchange (ETDEWEB)

    Fazal-ur-Rehman E-mail:; Abu-Jarad, F.; Al-Jarallah, M.I.; Farhat, M


    Samples of Nuclear Track Detectors (PM-355) were exposed to high gamma doses from 1x10{sup 5} Gy (10 Mrad) up to 1.2x10{sup 6} Gy (120 Mrad) at an incremental dose of 1x10{sup 5} Gy (10 Mrad). The gamma source was a 9.03 PBq (244 kCi) Co-60 source used for sterilization of medical syringes. The bulk etch rate (V{sub b}) was measured for various high gamma doses by three different methods: 1--thickness change method; 2--mass change method; 3--fission track diametric method. The study gives a comparison and limitations of these three methods used for bulk etch rate measurements in the detectors as a function of high gamma doses. The track etch rate (V{sub t}) and the sensitivity (V) of the detector were also measured using the fission track diametric method. It was observed that V{sub b} increases with the increase of the gamma absorbed dose at a fixed etching time in each bulk etch measuring method. The bulk etch rate decreases exponentially with the etching time at a fixed gamma absorbed dose in all three methods. The thickness change and mass change methods have successfully been applied to measure V{sub b} at higher gamma doses up to 1.2x10{sup 6} Gy (120 Mrad). The bulk etch rate determined by the mass change and thickness change methods was almost the same at a certain gamma dose and etching time whereas it was quite low in the case of the fission track diametric method due to its limitations at higher doses. Also in this method it was not possible to measure the fission fragment track diameters at higher doses due to the quick disappearance of the fission tracks and therefore the V{sub b} could not be estimated at higher gamma doses.

  6. Vacancy-type defects in bulk GaN grown by the Na-flux method probed using positron annihilation (United States)

    Uedono, Akira; Imanishi, Masayuki; Imade, Mamoru; Yoshimura, Masashi; Ishibashi, Shoji; Sumiya, Masatomo; Mori, Yusuke


    Defects in bulk GaN grown by the Na-flux method have been studied using a positron annihilation technique. Pyramidal bulk samples showed striation and inhomogeneous color distributions. Measurements of the Doppler broadening spectra of the annihilation radiation and lifetime spectra of positrons revealed that the concentration of vacancy-type defects increased with decreasing transparency of the samples. The major defect species was identified as a Ga vacancy coupled with nitrogen vacancies. A correlation between the oxygen incorporation and the introduction of such vacancies was observed. For c-plane GaN grown by a coalescence growth method, the concentration of vacancy-type defects was close to or under the detection limit of positron annihilation technique (≤1015cm-3), suggesting that high-quality bulk GaN can be fabricated using this method.


    Directory of Open Access Journals (Sweden)



    Full Text Available Introduction. Sludge production from municipal wastewater treatment plants should have quality standards before disposal in to the environment. Environmental specialists classified sewage sludge as a hazardous waste because of high organic compounds and pathogenic microorganisms. They belive that sewage should be stabilized before disposal and so composting of sewage sludge is an effective and economical method to stabilize. Sewage sludge compost could be used to improve soil structure and enrich the soil with nutrients. Methods. To evaluate the optimum conditions of aerobic compost, the mixture of dewatered sewage sludge from Isfahan municipal waste water treatment plant and sawdust as bulking agent were used. Pilot scale study were performed in Isfahan municipal waste water treatment plant. To perform this research project, the dewatered sewage sludge with humidity between 78 to 82 percent were mixed with sawdust. Turning over method of the piles with one week interval were applied to aerate the mixture. Temperature of the piles were monitored at different depths daily. Other parameters such as N, G, organic matters and pH were determined weekly. Total and fecal coli form, and salmonella were determined at the beginning and end of the composting process, also heavy metals were measured at the same time. Results. The results of this study showed that after days, temperature of the mixture reached up to 55 G, and were stabled for 15 days. Humidity, organic matter, organic carbon and GIN ratio of the mixture decreased over the period of the study, due to increasing the temperature. Also organic matter and humidity mainly decreased in thermofilic phase. The number of total and fecal coliform and also salmonella decreased to A class standards of US.EPA at the end of the operation. Discussion. The results of the study also showed that, this type of composting method is reliable, and simple to schedule, with high flexibility and low odor

  8. Mercury speciation analysis in seafood by species-specific isotope dilution: method validation and occurrence data

    Energy Technology Data Exchange (ETDEWEB)

    Clemens, Stephanie; Guerin, Thierry [Agence Nationale de Securite Sanitaire de l' Alimentation, Laboratoire de Securite des Aliments de Maisons-Alfort, Unite des Contaminants Inorganiques et Mineraux de l' Environnement, ANSES, Maisons-Alfort (France); Monperrus, Mathilde; Donard, Olivier F.X.; Amouroux, David [IPREM UMR 5254 CNRS - Universite de Pau et des Pays de l' Adour, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Institut des Sciences Analytiques et de Physico-chimie pour l' Environnement et les Materiaux, Pau Cedex (France)


    Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid-liquid extraction, derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit for the selected method were obtained in terms of limit of quantification (1.2 {mu}g Hg kg{sup -1} for MeHg and 1.4 {mu}g Hg kg{sup -1} for THg), repeatability (1.3-1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness (bias error less than 7%). By means of a recent strategy based on accuracy profiles ({beta}-expectation tolerance intervals), the selected method was successfully validated in the range of approximately 0.15-5.1 mg kg{sup -1} for MeHg and 0.27-5.2 mg kg{sup -1} for THg. Probability {beta} was set to 95% and the acceptability limits to {+-}15%. The method was then applied to 62 seafood samples representative of consumption in the French population. The MeHg concentrations were generally low (1.9-588 {mu}g kg{sup -1}), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested, methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure. (orig.)

  9. Growth of bulk GaN crystal by Na flux method (United States)

    Imade, M.; Miyoshi, N.; Yoshimura, M.; Kitaoka, Y.; Sasaki, T.; Mori, Y.


    In this paper, we reported the recent advances in the growth of GaN crystals on GaN templates and spontaneously nucleated GaN seeds by Na flux method. In the growth on GaN templates, it was clarified that the growth mode could be controlled by changing the flux composition. Based on the changes in the growth mode under different flux compositions, a growth sequence that is effective for the growth of thick GaN substrates with a low dislocation density was proposed. In the growth on pyramidal GaN seeds, we investigated the dependence of the growth rate, crystallinity and the growth habit on the flux composition. Results showed that a low Ga composition was preferred to grow high-crystallinity prismatic GaN crystals with a high growth rate. When a spontaneously nucleated GaN seed was used, a bulk GaN crystal with a hexagonal pillar consisting of six m-facets, and its length and diameter were 10 mm and 8 mm, respectively, was obtained. Furthermore, we found that the addition of Ca and Li to Ga-Na melt improved transparency of GaN crystals grown on pyramidal GaN seeds.

  10. Power System Decomposition for Practical Implementation of Bulk-Grid Voltage Control Methods

    Energy Technology Data Exchange (ETDEWEB)

    Vallem, Mallikarjuna R.; Vyakaranam, Bharat GNVSR; Holzer, Jesse T.; Elizondo, Marcelo A.; Samaan, Nader A.


    Power system algorithms such as AC optimal power flow and coordinated volt/var control of the bulk power system are computationally intensive and become difficult to solve in operational time frames. The computational time required to run these algorithms increases exponentially as the size of the power system increases. The solution time for multiple subsystems is less than that for solving the entire system simultaneously, and the local nature of the voltage problem lends itself to such decomposition. This paper describes an algorithm that can be used to perform power system decomposition from the point of view of the voltage control problem. Our approach takes advantage of the dominant localized effect of voltage control and is based on clustering buses according to the electrical distances between them. One of the contributions of the paper is to use multidimensional scaling to compute n-dimensional Euclidean coordinates for each bus based on electrical distance to perform algorithms like K-means clustering. A simple coordinated reactive power control of photovoltaic inverters for voltage regulation is used to demonstrate the effectiveness of the proposed decomposition algorithm and its components. The proposed decomposition method is demonstrated on the IEEE 118-bus system.

  11. Efficient method for storage of long conveyor belts passages inside the bulk containers

    National Research Council Canada - National Science Library



    The paper introduces the family of the algorithms designed to improve the process of winding up the long conveyor belt passages on reels located inside the bulk containers, used for i.e. rail transport...

  12. Three-dimensional Finite Elements Method simulation of Total Ionizing Dose in 22 nm bulk nFinFETs

    Energy Technology Data Exchange (ETDEWEB)

    Chatzikyriakou, Eleni, E-mail:; Potter, Kenneth; Redman-White, William; De Groot, C.H.


    Highlights: • Simulation of Total Ionizing Dose using the Finite Elements Method. • Carrier generation, transport and trapping in the oxide. • Application in three-dimensional bulk FinFET model of 22 nm node. • Examination of trapped charge in the Shallow Trench Isolation. • Trapped charge dependency of parasitic transistor current. - Abstract: Finite Elements Method simulation of Total Ionizing Dose effects on 22 nm bulk Fin Field Effect Transistor (FinFET) devices using the commercial software Synopsys Sentaurus TCAD is presented. The simulation parameters are extracted by calibrating the charge trapping model to experimental results on 400 nm SiO{sub 2} capacitors irradiated under zero bias. The FinFET device characteristics are calibrated to the Intel 22 nm bulk technology. Irradiation simulations of the transistor performed with all terminals unbiased reveal increased hardness up to a total dose of 1 MRad(SiO{sub 2}).

  13. Validated Spectrophotometric Methods for the Determination of Mycophenolate: An Anti-Neoplastic Agent in Bulk and Pharmaceutical Dosage Forms

    Directory of Open Access Journals (Sweden)

    A. Narendra


    Full Text Available Three simple, precise and cost-effective spectrophotometric methods have been developed for the determination of Mycophenolate in bulk and its pharmaceutical formulations. Mycophenolate shows max at 250.0 nm in zero-derivative spectrum (method A, 258.0 nm in first-derivative spectrum (method B and method C is based on the calculation of area under curve (AUC for analysis of Mycophenolate in the wavelength range of 240.0–260.0 nm. The drug follows the Beer-Lambert's law in the concentration range of 1.0–150.0 μg/mL for all the methods. The methods were validated by following the analytical performance parameters suggested by the International Conference on Harmonization. All validation parameters were within the acceptable range. The developed methods were successfully applied to estimate the amount of Mycophenolate in bulk and pharmaceutical dosage forms.

  14. Speciation of vanadium in urban, industrial and volcanic soils by a modified Tessier method. (United States)

    Orecchio, Santino; Amorello, Diana; Barreca, Salvatore; Pettignano, Alberto


    Vanadium (V) concentrations in industrial, urban and volcanic soils were sequentially extracted using a modified Tessier's method. The voltammetric technique was used to determine V concentrations in solutions obtained from the various extraction steps. At the reference stations, the V concentrations (sum of four individual fractions) in soils ranged from 0.72 to 0.24 g kg(-1) dry weight (d.w.) with a mean value of 0.18 g kg(-1) d.w. V concentrations in soils of the Palermo urban area ranged from 0.34 to 2.1 g kg(-1) d.w., in the Milazzo (industrial) area between 0.26 and 5.4 g kg(-1) d.w. and in the volcanic area near Mt. Etna from 0.91 to 2.9 g kg(-1) d.w. When the V concentrations around Mt. Etna were compared with those obtained at the reference stations, it was confirmed that Mt. Etna is a continuous source of V. In all the samples analyzed, the majority of V (from 94 to 100%) was detected in the fourth fraction.

  15. Speciation analysis of radionuclides in the environment. NKS-B speciation project report 2007

    Energy Technology Data Exchange (ETDEWEB)

    Xiaolin Hou (Technical Univ. of Denmark, Risoe National Lab. for Sustainable Energy, Roskilde (Denmark)); Aldahan, A. (Uppsala Univ., Dept. of Earth Science, Uppsala (Sweden)); Possnert, G. (Uppsala Univ., Tandem Lab., Uppsala (Sweden)); Lujaniene, G. (Institute of Physics, Vilnius (Lithuania)); Lehto, J. (Univ. of Helsinki, Dept. of Chemistry, Helsinki (Finland)); Salbu, B. (Norwegian Univ. of Life Sciences (UMB), AAs (Norway))


    This report describes the work carried out under the NUK-B project SPECIATION 2007. In 2007, the project partners had two meeting in April and November, organized a NUK seminar on speciation and hot particles. SPECIATION 2007 t mainly focused on two issues on speciation (1) further development of speciation methods for radionuclides, and (2) investigation of speciation of radionuclides in environment. The report summarized the work done in partners labs, which includes: (1) Further development on the speciation of 129I and 127I in water samples; (2) Speciation method for 129I and 127I in air; (3) Dynamic system for fractionation of Pu and Am in soil and sediment; (4) Investigation on Re-absorption of Pu during the fractionation of Pu in soil and sediment; (5) Speciation of 129I in North Sea surface water; (6) Partition of 137Cs and 129I in the Nordic lake sediment, pore-water and lake water; (7) Sequential extraction of Pu in soil, sediment and concrete samples, (8) Pu sorption to Mn and Fe oxides in the geological materials, (10) Investigation of the adsorbed species of lanthanides and actinides on clays surfaces. In addition, two review articles on the speciation of plutonium and iodine in environmental are planned to be submitted to an international journal for publication. (au)

  16. New method for introducing nanometer flux pinning centers into single domain YBCO bulk superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Yang, W.M., E-mail:; Wang, Miao


    Highlights: • Single domain YBCO bulks with Bi{sub 2}O{sub 3} additions fabricated by TSIG process. • Nanoscale Y{sub 2}Ba{sub 4}CuBiOx(YBi2411) particles introduced by Bi{sub 2}O{sub 3} additions. • The YBi2411 particles are about 150 nm, can act as effective flux pinning centers. • The optimal addition of Bi{sub 2}O{sub 3} is 0.7wt% to achieve higher levitation force. • The result is helpful to improve the quality of REBCO bulk superconductors. -- Abstract: Single domain YBCO superconductors with different additions of Bi{sub 2}O{sub 3} have been fabricated by top seeded infiltration and growth process (TSIG). The effect of Bi{sub 2}O{sub 3} additions on the growth morphology, microstructure and levitation force of the YBCO bulk superconductor has been investigated. The results indicate that single domain YBCO superconductors can be fabricated with the additions of Bi{sub 2}O{sub 3} less than 2 wt%; Bi{sub 2}O{sub 3} can be reacted with Y{sub 2}BaCuO{sub 5} and liquid phase and finally form Y{sub 2}Ba{sub 4}CuBiO{sub x}(YBi2411) nanoscale particles; the size of the YBi2411 particles is about 100 nm, which can act as effective flux pinning centers. It is also found that the levitation force of single domain YBCO bulks is increasing from 13 N to 34 N and decreasing to 11 N with the increasing of Bi{sub 2}O{sub 3} addition from 0.1 wt% to 0.7 wt% and 2 wt%. This result is helpful for us to improve the physical properties of REBCO bulk superconductors.

  17. Speciation analysis of radionuclides in the environment - NSK-B SPECIATION project report 2009

    Energy Technology Data Exchange (ETDEWEB)

    Hou, X. (Technical Univ. of Denmark, Risoe National Lab. for Sustainable Energy, Roskilde (Denmark)); Aldahan, A. (Uppsala Univ., Dept. of Earth Science (Sweden)); Possnert, G. (Uppsala Univ., Tandem Lab. (Sweden)); Lujaniene, G. (Univ. of Helsinki, Lab. of Radiochemistry (Finland)); Lehto, J. (Institute of Physics (Lithuania)); Skipperud, L.; Lind, O.C.; Salbu, B. (Norwegian Univ. of Life Sciences, Isotope Lab., AAs (Norway))


    The second stage of the NKS-B project SPECIATION was complemented in 2008-2009, which mainly focus on three aspects: (1) Further improvement and development of methods for speciation analysis of radionuclides; (2) Investigation of speciation of some radionuclides in the environment (water, sediments, particles); and (3) Intercomparison excise for speciation analysis of radionuclides in soil and sediment. This report summarizes the work completed in the project partners' laboratories. Method developments include: Development of an rapid and in-suit separation method for the speciation analysis of 129I in seawater samples; Development of a simple method for the speciation analysis of 129I in fresh water and seawater samples; Development of an on-line HPLC-ICP-MS method for the direct speciation analysis of 127I in water and leachate samples; Speciation of radionuclides in water includes: Speciation of 129I and 127I in time-series precipitation samples collected in Denmark 2001-2006 and its application for the investigation of geochemistry and atmospheric chemistry of iodine, Speciation of radionuclides in Ob and Yenisey Rivers, and Speciation of 129I and 127I in Lake Heimdalen water. Speciation of radionuclides in soils and sediments includes: Sequential extraction of radionuclides in sediments and of trace elements in soil samples. Sequential extraction of radionuclides in aerosols and particles has also been performed. Furthermore, sorption experiments have been performed to investigate the association of Pu, Am and Cs with different geological materials. The intercomparison exercises included sequential extraction of Pu, 137Cs, U, Th, and 129I in one soil and one sediment standard reference materials (NIST-4354, IAEA-375) and Pu in sediment collected from the Lake Heimdalen, Norway. (author)

  18. High Quality, Low Cost Bulk Gallium Nitride Substrates Grown by the Electrochemical Solution Growth Method

    Energy Technology Data Exchange (ETDEWEB)

    Seacrist, Michael [SunEdison Inc., St. Peters, MO (United States)


    The objective of this project was to develop the Electrochemical Solution Growth (ESG) method conceived / patented at Sandia National Laboratory into a commercially viable bulk gallium nitride (GaN) growth process that can be scaled to low cost, high quality, and large area GaN wafer substrate manufacturing. The goal was to advance the ESG growth technology by demonstrating rotating seed growth at the lab scale and then transitioning process to prototype commercial system, while validating the GaN material and electronic / optical device quality. The desired outcome of the project is a prototype commercial process for US-based manufacturing of high quality, large area, and lower cost GaN substrates that can drive widespread deployment of energy efficient GaN-based power electronic and optical devices. In year 1 of the project (Sept 2012 – Dec 2013) the overall objective was to demonstrate crystalline GaN growth > 100um on a GaN seed crystal. The development plan included tasks to demonstrate and implement a method for purifying reagent grade salts, develop the reactor 1 process for rotating seed Electrochemical Solution Growth (ESG) of GaN, grow and characterize ESG GaN films, develop a fluid flow and reaction chemistry model for GaN film growth, and design / build an improved growth reactor capable of scaling to 50mm seed diameter. The first year’s project objectives were met in some task areas including salt purification, film characterization, modeling, and reactor 2 design / fabrication. However, the key project objective of the growth of a crystalline GaN film on the seed template was not achieved. Amorphous film growth on the order of a few tenths of a micron has been detected with a film composition including Ga and N, plus several other impurities originating from the process solution and hardware. The presence of these impurities, particularly the oxygen, has inhibited the demonstration of crystalline GaN film growth on the seed template. However, the

  19. An introduction to the calculation of valence EELS: quantum mechanical methods for bulk solids. (United States)

    Keast, V J


    The low-loss region of the electron energy-loss spectrum, the valence EELS, provides information about the electronic structure and optical properties of materials. For bulk materials the spectral intensity can be directly connected to the complex dielectric function. Ab initio quantum mechanical calculations have an important role to play in the interpretation of the fine spectral detail and how this can be connected to the material properties. This paper provides an overview of theoretical background to the calculation of valence EELS in bulk solids and gives specific details on how to run such calculations using the WIEN2k code. The comparison of Au and AuAl(2) illustrates how in metals such calculations are successful in reproducing the main spectral details and can be used to understand the origin of the different colours of these two metals. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. Iodine speciation in coastal and inland bathing waters and seaweeds extracts using a sequential injection standard addition flow-batch method. (United States)

    Santos, Inês C; Mesquita, Raquel B R; Bordalo, Adriano A; Rangel, António O S S


    The present work describes the development of a sequential injection standard addition method for iodine speciation in bathing waters and seaweeds extracts without prior sample treatment. Iodine speciation was obtained by assessing the iodide and iodate content, the two inorganic forms of iodine in waters. For the determination of iodide, an iodide ion selective electrode (ISE) was used. The indirect determination of iodate was based on the spectrophotometric determination of nitrite (Griess reaction). For the iodate measurement, a mixing chamber was employed (flow batch approach) to explore the inherent efficient mixing, essential for the indirect determination of iodate. The application of the standard addition method enabled detection limits of 0.14 µM for iodide and 0.02 µM for iodate, together with the direct introduction of the target water samples, coastal and inland bathing waters. The results obtained were in agreement with those obtained by ICP-MS and a colorimetric reference procedure. Recovery tests also confirmed the accuracy of the developed method which was effectively applied to bathing waters and seaweed extracts. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Responses of Mn2+ speciation in Deinococcus radiodurans and Escherichia coli to γ-radiation by advanced paramagnetic resonance methods. (United States)

    Sharma, Ajay; Gaidamakova, Elena K; Matrosova, Vera Y; Bennett, Brian; Daly, Michael J; Hoffman, Brian M


    The remarkable ability of bacterium Deinococcus radiodurans to survive extreme doses of γ-rays (12,000 Gy), 20 times greater than Escherichia coli, is undiminished by loss of Mn-dependent superoxide dismutase (SodA). D. radiodurans radiation resistance is attributed to the accumulation of low-molecular-weight (LMW) "antioxidant" Mn(2+)-metabolite complexes that protect essential enzymes from oxidative damage. However, in vivo information about such complexes within D. radiodurans cells is lacking, and the idea that they can supplant reactive-oxygen-species (ROS)-scavenging enzymes remains controversial. In this report, measurements by advanced paramagnetic resonance techniques [electron-spin-echo (ESE)-EPR/electron nuclear double resonance/ESE envelope modulation (ESEEM)] reveal differential details of the in vivo Mn(2+) speciation in D. radiodurans and E. coli cells and their responses to 10 kGy γ-irradiation. The Mn(2+) of D. radiodurans exists predominantly as LMW complexes with nitrogenous metabolites and orthophosphate, with negligible EPR signal from Mn(2+) of SodA. Thus, the extreme radiation resistance of D. radiodurans cells cannot be attributed to SodA. Correspondingly, 10 kGy irradiation causes no change in D. radiodurans Mn(2+) speciation, despite the paucity of holo-SodA. In contrast, the EPR signal of E. coli is dominated by signals from low-symmetry enzyme sites such as that of SodA, with a minority pool of LMW Mn(2+) complexes that show negligible coordination by nitrogenous metabolites. Nonetheless, irradiation of E. coli majorly changes LMW Mn(2+) speciation, with extensive binding of nitrogenous ligands created by irradiation. We infer that E. coli is highly susceptible to radiation-induced ROS because it lacks an adequate supply of LMW Mn antioxidants.

  2. Standard Test Method for Water Absorption, Bulk Density, Apparent Porosity, and Apparent Specific Gravity of Fired Whiteware Products

    CERN Document Server

    American Society for Testing and Materials. Philadelphia


    1.1 This test method covers procedures for determining water absorption, bulk density, apparent porosity, and apparent specific gravity of fired unglazed whiteware products. 1.2 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  3. Development and Validation of HPTLC method for the estimation of Sitagliptin Phosphate and Simvastatin in bulk and Marketed Formulation


    Rathod Sonali; Patil Pallavi; Chopade Vittal


    Method describes a development and validation of HPTLC method for the estimation of sitagliptin phosphate and simvastatin in bulk and marketed formulation. This employs a precoated silica gel 60 F254 (0.2 mm thickness) on aluminium sheets and mobile phase chloroform: methanol in the ratio of 8:2 v/v, having chamber saturation for 20 min at room temperature. The developing chamber was run up to 8cm. The Rf values were found to be 0.13 and 0.75 for sitagliptin phosphate and simvastatin respecti...

  4. Cosmic bulk flows on 50 h-1 Mpc scales: a Bayesian hyper-parameter method and multishell likelihood analysis (United States)

    Ma, Yin-Zhe; Scott, Douglas


    It has been argued recently that the galaxy peculiar velocity field provides evidence of excessive power on scales of 50 h-1 Mpc, which seems to be inconsistent with the standard Λ cold dark matter (ΛCDM) cosmological model. We discuss several assumptions and conventions used in studies of the large-scale bulk flow to check whether this claim is robust under a variety of conditions. Rather than using a composite catalogue we select samples from the SN, ENEAR, Spiral Field I-band Survey (SFI++) and First Amendment Supernovae (A1SN) catalogues, and correct for Malmquist bias in each according to the IRAS PSCz density field. We also use slightly different assumptions about the small-scale velocity dispersion and the parametrization of the matter power spectrum when calculating the variance of the bulk flow. By combining the likelihood of individual catalogues using a Bayesian hyper-parameter method, we find that the joint likelihood of the amplitude parameter gives σ8 = 0.65+ 0.47- 0.35 (68 per cent confidence region), which is entirely consistent with the ΛCDM model. In addition, the bulk flow magnitude, v ˜ 310 km s-1, and direction, (l, b) ˜ (280° ± 8°, 5.1° ± 6°), found by each of the catalogues are all consistent with each other, and with the bulk flow results from most previous studies. Furthermore, the bulk flow velocities in different shells of the surveys constrain (σ8, Ωm) to be (1.01+ 0.26- 0.20, 0.31+ 0.28- 0.14) for SFI++ and (1.04+ 0.32- 0.24, 0.28+ 0.30- 0.14) for ENEAR, which are consistent with the 7-year Wilkinson and Microwave Anisotropy Probe (WMAP7) best-fitting values. We finally discuss the differences between our conclusions and those of the studies claiming the largest bulk flows.

  5. Fast methods of computing bulk radiative properties of inhomogeneous clouds illuminated by solar radiation

    Energy Technology Data Exchange (ETDEWEB)

    Gabriel, P. [Colorado State Univ., Fort Collins, CO (United States)


    The use of cloud fraction as a means of incorporating horizontal cloud inhomogeneity in radiative transfer calculations is widespread in the atmospheric science community. This research attempts to bypass the use of cloud fraction in radiative transfer modeling for two-dimensional media. Gabriel describes two approximation techniques useful in calculating the domain averaged bulk radiative properties such as albedo, flux divergence and mean radiance that dispense with the need to use cloud fraction as a specifier of cloud inhomogeneity. The results suggest that the variability of the medium can largely be accounted for through the pseudo-source term, offering hope of parameterizing the equation of transfer in terms of the statistical properties of the medium. 1 fig.

  6. Stability indicating high performance thin layer chromatographic method for quantitation of venlafaxine in bulk and pharmaceutical dosage form

    Directory of Open Access Journals (Sweden)

    Sunil K Dubey


    Full Text Available Background: Venlafaxine (VEN is a phenethylamine bicyclic compound, chemically, 1-(2-[dimethyl amino]-1-[4-methoxy phenyl] ethyl cyclo-hexan-1ol hydrochloride. It is a antidepressant. It inhibits the reuptake of serotonin, nor adrenaline and dopamine to a lesser extent at the presynaptic membrane. Aim: A simple, rapid, precise, accurate, and economical high performance thin layer chromatographic (HPTLC method has been developed and validated for the determination of VEN both as a bulk drug and in formulation. Materials and Methods: The method uses aluminum plates precoated with silica gel 60 F254 as the stationary phase and dichloromethane:acetonitrile:N-hexane:triethylamine: 0.5:0.5:4:0.7 (v/v/v/v as mobile phase. Results: This system gave compact spots for VEN (R f = 0.46 ± 0.05. Forced degradation studies were done by subjecting VEN to acid and alkali hydrolysis, oxidation, and reduction. The peak of the degradation product was well resolved from that of the pure drug and had significant different R f values. Analysis of VEN was performed in the absorbance mode at 225 nm. The limit of detection and quantification were 12.48 and 37.81 ng/spot respectively. Conclusions: The developed method was validated and found to be simple, specific, accurate and precise and can be used for routine quality control analysis of VEN in bulk and pharmaceutical formulation.

  7. RP-HPLC Method Development and Validation for Determination of Eptifibatide Acetate in Bulk Drug Substance and Pharmaceutical Dosage Forms. (United States)

    Bavand Savadkouhi, Maryam; Vahidi, Hossein; Ayatollahi, Abdul Majid; Hooshfar, Shirin; Kobarfard, Farzad


    A new, rapid, economical and isocratic reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of eptifibatide acetate, a small synthetic antiplatelet peptide, in bulk drug substance and pharmaceutical dosage forms. The developed method was validated as per of ICH guidelines. The chromatographic separation was achieved isocratically on C18 column (150 x 4.60 mm i.d., 5 µM particle size) at ambient temperature using acetonitrile (ACN), water and trifluoroacetic acid (TFA) as mobile phase at flow rate of 1 mL/min and UV detection at 275 nm. Eptifibatide acetate exhibited linearity over the concentration range of 0.15-2 mg/mL (r2=0.997) with limit of detection of 0.15 mg/mL The accuracy of the method was 96.4-103.8%. The intra-day and inter-day precision were between 0.052% and 0.598%, respectively. The present successfully validated method with excellent selectivity, linearity, sensitivity, precision and accuracy was applicable for the assay of eptifibatide acetate in bulk drug substance and pharmaceutical dosage forms.

  8. A new turn-on fluorimetric method for the rapid speciation of Cr(III)/Cr(VI) species in tea samples with rhodamine-based fluorescent reagent (United States)

    Özyol, Esra; Saçmacı, Şerife; Saçmacı, Mustafa; Ülgen, Ahmet


    A new fluorimetric method with rhodamine-based fluorescent agent was developed for the rapid speciation of Cr(III)/Cr(VI) in tea, soil and water samples. The system, which utilizes a fluorescent reagent, was used for the first time after synthesis/characterization of 3‧,6‧-bis(diethylamino)-2-{[(1E)-(2,4-dimethoxyphenyl)methylene] amino}spiro[isoindole-1,9‧-xanthen]-3(2H)-one (BDAS). The reagent responds instantaneously at room temperature in a 1:1 stoichiometric manner to the amount of Cr(III). The selectivity of this system for Cr(III) over other metal ions is remarkably high, and its sensitivity is below 0.01 mg L- 1 in aqueous solutions which enables a simplification without any pretreatment of the real sample. The method has a wide linear range of 0.1-10 mg L- 1 and a detection limit of 0.15 μg L- 1 for Cr(III) while the relative standard deviation was 0.1% for 0.1 mg L- 1 Cr(III) concentration. The results of detection and recovery experiments for Cr(III) in tea, soil and water were satisfactory, indicating that the method has better feasibility and application potential in the routine determination and speciation of Cr(III)/Cr(VI). The results of analysis of the certified reference material (INCT-TL-1 tea sample and CWW-TM-D waste water) are in good agreement with the certified value.

  9. A new RE + 011 TSIG method for the fabrication of high quality and large size single domain YBCO bulk superconductors (United States)

    Yang, W. M.; Chen, L. P.; Wang, X. J.


    High quality single domain YBCO bulk superconductors, 20 mm in diameter, have been fabricated using a new top seeded infiltration and growth method (called the RE + 011 TSIG method), with a new solid phase (Y2O3 + xBaCuO2) instead of the conventional Y2BaCuO5 solid phase, x = 0, 0.5, 1.0, 1.2, 1.5, 1.8, 2.0, 2.5, 3.0. The effects of different BaCuO2 contents x on the growth morphology, microstructure, and levitation force have been investigated. The results show that the levitation force of the YBCO bulks first increases and then decreases with increasing x, and reaches maximum levitation forces of about 49.2 N (77 K, 0.5 T, with the traditional liquid phase of YBa2Cu3O y + 3 BaCuO2 + 2 CuO) and 47 N (77.3 K, 0.5 T, with the new liquid phase of Y2O3 + 10 BaCuO2 + 6 CuO) when x = 1.2, which is much higher than that of the samples fabricated with the conventional solid phases (23 N). The average Y2BaCuO5 particle size is about 1 μm, which is much smaller than the 3.4 μm in the samples prepared with the conventional Y2BaCuO5 solid phase; this means that the flux pinning force of the sample can be improved by using the new solid phase. Based on this method, single domain YBCO bulks 40 mm, 59 mm, and 93 mm in diameter have also been fabricated using the TSIG process with the new solid phases (Y2O3 + 1.2BaCuO2). These results indicate that the new TSIG process developed by our lab is a very important and practical method for the fabrication of low cost, large size, and high quality single domain REBCO bulk superconductors.

  10. Development and Validation of an RP-HPLC Method for Quantitative Estimation of Eslicarbazepine Acetate in Bulk Drug and Tablets. (United States)

    Singh, M; Kumar, L; Arora, P; Mathur, S C; Saini, P K; Singh, R M; Singh, G N


    A convenient, simple, accurate, precise and reproducible RP-HPLC method was developed and validated for the estimation of eslicarbazepine acetate in bulk drug and tablet dosage form. Objective was achieved under optimised chromatographic conditions on Dionex RP-HPLC system with Dionex C18 column (250×4.6 mm, 5 μm particle size) using mobile phase composed of methanol and ammonium acetate (0.005 M) in the ratio of 70:30 v/v. The separation was achieved using an isocratic elution method with a flow rate of 1.0 ml/ min at room temperature. The effluent was monitored at 230 nm using diode array detector. The retention time of eslicarbazepine acetate is found to be 4.9 min and the standard calibration plot was linear over a concentration range of 10-90 μg/ml with r(2)=0.9995. The limit of detection and quantification were found to be 3.144 and 9.52 μg/ml, respectively. The amount of eslicarbazepine acetate in bulk and tablet dosage form was found to be 99.19 and 97.88%, respectively. The method was validated statistically using the percent relative standard deviation and the values are found to be within the limits. The recovery studies were performed and the percentage recoveries were found to be 98.33± 0.5%.

  11. A Validated TLC-Densitometric Method for the Determination of Mesterolone in Bulk Material and in Tablets. (United States)

    Dołowy, Małgorzata; Pyka-Pająk, Alina; Filip, Katarzyna; Zagrodzka, Joanna


    Mesterolone is a synthetic androgenic steroid indicating a weak anabolic activity. A new, simple in use, and economical TLC-densitometric method in normal phase system (NP-TLC) has been developed and validated for the identification and quantitative determination of mesterolone in bulk drug and in tablet formulation. NP-TLC analysis was performed on aluminium plates precoated with silica gel 60F254 as the stationary phase using chloroform-acetone (40 : 10, v/v) as mobile phase. Densitometric analysis was carried out at λ = 745 nm after staining with phosphomolybdic acid. These conditions were found to give visible (dark blue) spot and sharp peak, respectively, for mesterolone at R F 0.75 ± 0.02 and enabled satisfactory separation of mesterolone from its related substance (potential impurity). The proposed NP-TLC-densitometric method was validated for specificity, linearity, precision, accuracy, robustness, and sensitivity according to ICH guideline and other validation requirements. The limit of detection (LOD) and limit of quantification (LOQ) were 61.0 ng · spot(-1) and 184.0 ng · spot(-1), respectively. The percent content of mesterolone in marketed tablet formulation was found to be 99.40% of label claim. The developed TLC-densitometric method can be successfully used in quality control of mesterolone in bulk material and also tablet formulation.

  12. Potential of a spectroscopic measurement method using adding-doubling to retrieve the bulk optical properties of dense microalgal media. (United States)

    Bellini, Sarah; Bendoula, Ryad; Latrille, Eric; Roger, Jean-Michel


    In the context of algal mass cultivation, current techniques used for the characterization of algal cells require time-consuming sample preparation and a large amount of costly, standard instrumentation. As the physical and chemical properties of the algal cells strongly affect their optical properties, the optical characterization is seen as a promising method to provide an early diagnosis in the context of mass cultivation monitoring. This article explores the potential of a spectroscopic measurement method coupled with the inversion of the radiative transfer theory for the retrieval of the bulk optical properties of dense algal samples. Total transmittance and total reflectance measurements were performed over the 380-1020 nm range on dense algal samples with a double integrating sphere setup. The bulk absorption and scattering coefficients were thus extracted over the 380-1020 nm range by inverting the radiative transfer theory using inverse-adding-doubling computations. The experimental results are presented and discussed; the configuration of the optical setup remains a critical point. The absorption coefficients obtained for the four samples of this study appear not to be more informative about pigment composition than would be classical methods in analytical spectroscopy; however, there is a real added value in measuring the reduced scattering coefficient, as it appears to be strongly correlated to the size distribution of the algal cells.

  13. A heuristic and hybrid method for the tank allocation problem in maritime bulk shipping

    DEFF Research Database (Denmark)

    Vilhelmsen, Charlotte; Larsen, Jesper; Lusby, Richard Martin


    finding a feasible solution. We have developed a heuristic that can efficiently find feasible cargo allocations. Computational results show that it can solve 99 % of the considered instances within 0.4 s and all of them if allowed longer time. We have also modified an optimality based method from...... the literature. The heuristic is much faster than this modified method on the vast majority of considered instances. However, the heuristic struggles on two instances which are relatively quickly solved by the modified optimality based method. These two methods therefore complement each other nicely and so, we...... have created a hybrid method that first runs the heuristic and if the heuristic fails to solve the problem, then runs the modified optimality based method on the parts of the problem that the heuristic did not solve. This hybrid method cuts between 90 and 94 % of the average running times compared...

  14. A Heuristic and Hybrid Method for the Tank Allocation Problem in Maritime Bulk Shipping

    DEFF Research Database (Denmark)

    Vilhelmsen, Charlotte; Larsen, Jesper; Lusby, Richard Martin

    finding a feasible solution. We have developed a heuristic that can efficiently find feasible cargo allocations. Computational results show that it can solve 99% of the considered instances within 0.4 seconds and all of them if allowed longer time. We have also modified an optimality based method from...... the literature. The heuristic is much faster than this modified method on the vast majority of considered instances. However, the heuristic struggles on two instances which are relatively quickly solved by the modified optimality based method. These two methods therefore complement each other nicely and so, we...... have created a hybrid method that first runs the heuristic and if the heuristic fails to solve the problem, then runs the modified optimality based method on the parts of the problem that the heuristic did not solve. This hybrid method cuts between 90% and 94% of the average running times compared...

  15. Quantitative determination of levofloxacin hemihydrate in bulk and tablets by UV-spectrophotometry and first order derivative methods. (United States)

    Shirkhedkar, A A; Surana, S J


    Two simple, rapid, accurate and economical 'UV Spectrophotometry' and 'First Order Derivative' methods have been developed for determination of levofloxacin hemihydrate in bulk and tablets. In (10% v/v) acetonitrile, the lambdamax of the drug was found to be 288 nm. The same spectrum was derivatised into first order derivative, using UV probe software of instrument (Shimadzu-2450), at Deltalambda=4. The amplitude of the trough was recorded at 297 nm. In both the proposed methods, levofloxacin hemihydrate follows linearity in the concentration range 2-12 microg/ml with a correlation coefficient of 0.9999. Assay results were in good agreement with label claim. The methods were validated statistically and by recovery studies. The relative standard deviation were found to be less than 2% with excellent precision and accuracy.

  16. Simple Spectrophotometric Methods for Determination of Tenofovir Fumarate and Emtricitabine in Bulk Powder and in Tablets

    Directory of Open Access Journals (Sweden)

    Mohammad H. AbdelHay


    Full Text Available Two simple and selective methods were developed for the simultaneous determination of tenofovir fumarate (TEN and emtricitabine (EMT in combined tablets. The first method involves the application of first derivative spectrophotometry where the first derivative amplitudes were measured at 298.5 nm for determination of EMT in presence of TEN. The second method involves first derivative of ratio spectra spectrophotometry where the amplitudes at 251.5 nm have been used for quantitation of TEN in the presence of EMT. Different variables affecting each method were carefully investigated and optimized. Reliability and analytical performance of the proposed methods, including linearity, range, precision, accuracy, detection, and quantitation limits, were statistically validated. The methods were successfully applied for the determination of EMT and TEN in laboratory-prepared mixtures and in their combined tablets.

  17. Spectrophotometric method for quantitative determination of triclabendazole in bulk and pharmaceutical

    Directory of Open Access Journals (Sweden)

    Alankar Shrivastava


    Full Text Available Background: Triclabendazole (TCBZ, 6-chloro-5(2-3 dichlorophenoxy-2-methyl thio-benzimidazole, an halogenated benzimidazole (BZD thiol derivative, shows high efficacy against both the immature and mature stages of Fasciola hepatica in sheep and cattle, which is a differential feature compared to other available trematodicidal drugs. As a consequence of its excellent activity against the liver fluke, it has been extensively used and this has inevitably promoted the selection of TCBZ-resistant populations, which is now a worrying problem in several areas of the world. We propose simple ultraviolet spectrophotometric method for the estimation of triclabendazole in 0.1 methanolic HCl for the estimation of the drug. Method was validated as per ICH guidelines. Materials and Methods: Spectral absorbance measurements were made on Shimadzu UV-1800 with 10 mm matched quartz cells and dilutions were made in 0.1 M methanolic HCl. Results: The LOD and LOQ of triclabendazole at 305 nm were found to be 0.068434 and 2.73×10-4 μg/ml respectively. The calibration was linear in the range of 1-10 μg/ml. Analytical parameters such as stability, selectivity, accuracy, and precision have been established for the method in Endex and Fasinex tablets and evaluated statistically to assess the application of the method. Conclusion: Method passes all parameters with in desirable limits and found to be simple, stable, sensitive, reproducible, and accurate for the routine analysis of the drug in pharmaceutical formulations and in pharmaceutical investigations involving triclabendazole.

  18. A Heuristic and Hybrid Method for the Tank Allocation Problem in Maritime Bulk Shipping

    DEFF Research Database (Denmark)

    Vilhelmsen, Charlotte; Larsen, Jesper; Lusby, Richard Martin

    ship route. We have developed a randomised heuristic for eciently nding feasible allocations and computational results show that it can solve 99% of the considered instances within 0.5 seconds and all of them if allowed longer time. The heuristic is designed to work as an ecient subproblem solver...... and in such a setting with running times below e.g. 5 seconds, the heuristic clearly outperforms an earlier method by consistently solving more instances and eectively cutting 84% of the average running time. Furthermore, we have combined our heuristic with a modied version of the earlier method to derive a hybrid...

  19. Bulk-scaffolded hydrogen storage and releasing materials and methods for preparing and using same (United States)

    Autrey, S Thomas [West Richland, WA; Karkamkar, Abhijeet J [Richland, WA; Gutowska, Anna [Richland, WA; Li, Liyu [Richland, WA; Li, Xiaohong S [Richland, WA; Shin, Yongsoon [Richland, WA


    Compositions are disclosed for storing and releasing hydrogen and methods for preparing and using same. These hydrogen storage and releasing materials exhibit fast release rates at low release temperatures without unwanted side reactions, thus preserving desired levels of purity and enabling applications in combustion and fuel cell applications.

  20. Simultaneous Estimation of Ibuprofen and Phenylephrine Hydrochloride in Bulk and Combined Dosage Form by First Derivative UV Spectrophotometry Method

    Directory of Open Access Journals (Sweden)

    Mehul Patel


    Full Text Available A simple, precise, rapid, and economic method was developed for the simultaneous determination of Ibuprofen and Phenylephrine HCl in bulk and combined dosage form. This method involves first-order derivative spectroscopy using 248 nm and 237 nm as zero crossing points for Ibuprofen and Phenylephrine HCl, respectively. For spectrophotometric method 0.1 N NaOH was used as a solvent. The linearity was established over the concentration range of 12–72 μg/mL and 1.5–22 μg/mL for Ibuprofen and Phenylephrine HCl with correlation coefficient (r2 of 0.9972 and 0.9981, respectively. The mean % recoveries were found to be in the range of 98.88% and 98.54% for Ibuprofen and Phenylephrine HCl, respectively. Interday and intraday studies showed repeatability of the method. The method was found to be specific and robust. The method was successfully applied to pharmaceutical formulation, with no interference from excipients as indicated by the recovery study. Results of analysis were validated statistically and by recovery studies.


    Directory of Open Access Journals (Sweden)

    Iván Machín


    Full Text Available This paper presents a set of procedures based on mathematical optimization methods to establish optimal active sulphide phases with higher HDS activity. This paper proposes a list of active phases as a guide for orienting the experimental work in the search of new catalysts that permit optimize the HDS process. Studies in this paper establish Co-S, Cr-S, Nb-S and Ni-S systems have the greatest potential to improve HDS activity.

  2. Fabrication of ordered bulk heterojunction organic photovoltaic cells using nanopatterning and electrohydrodynamic spray deposition methods. (United States)

    Park, Sung-Eun; Kim, Sehwan; Kim, Kangmin; Joe, Hang-Eun; Jung, Buyoung; Kim, Eunkyoung; Kim, Woochul; Min, Byung-Kwon; Hwang, Jungho


    Organic photovoltaic cells with an ordered heterojunction (OHJ) active layer are expected to show increased performance. In the study described here, OHJ cells were fabricated using a combination of nanoimprinting and electrohydrodynamic (EHD) spray deposition methods. After an electron donor material was nanoimprinted with a PDMS stamp (valley width: 230 nm, period: 590 nm) duplicated from a Si nanomold, an electron acceptor material was deposited onto the nanoimprinted donor layer using an EHD spray deposition method. The donor-acceptor interface layer was observed by obtaining cross-sectional images with a focused ion beam (FIB) microscope. The photocurrent generation performance of the OHJ cells was evaluated with the current density-voltage curve under air mass (AM) 1.5 conditions. It was found that the surface morphology of the electron acceptor layer affected the current and voltage outputs of the photovoltaic cells. When an electron acceptor layer with a smooth thin (250 nm above the valley of the electron donor layer) surface morphology was obtained, power conversion efficiency was as high as 0.55%. The electrohydrodynamic spray deposition method used to produce OHJ photovoltaic cells provides a means for the adoption of large area, high throughput processes.

  3. Speciation of Long-Lived Radionuclides in the Environment

    DEFF Research Database (Denmark)

    Hou, Xiaolin

    This project started in November 2005 and ended in November 2008, the work and research approaches are summarized in this report. This project studied the speciation of radionuclides in environment. A number of speciation analytical methods are developed for determination of species of 129I, 99Tc......, isotopes of Pu, and 237Np in seawater, fresh water, soil, sediment, vegetations, and concrete. The developed methods are used for the investigation of the chemical speciation of these radionuclides as well as their environmental behaviours, especially in Danish environment. In addition the speciation of Pu...

  4. Spectrophotometric methods for the determination of letrozole in bulk and pharmaceutical dosage forms

    Directory of Open Access Journals (Sweden)

    Sasmita Kumari Acharjya


    Full Text Available Ultraviolet (UV, first derivative, second derivative, and AUC-spectrophotometric methods for the determination of letrozole in pharmaceutical formulations have been developed. For UV-spectrophotometry, the standard solutions were measured at 240.0 nm. The linearity ranges were found to be 0.25-20.0 μgml−1 in methanol and the regression equation was A=1.20×10−1 C+2.22×10−2 (r 2 =0.9994. For the first derivative spectrophotometry, the response (dA/dλ of standard solutions was measured at 224.0 nm. The calibration curve was constructed by plotting dA/dλ values against concentrations 0.25-20.0 μgml−1 , of letrozole. The regression equation of the linear calibration graph was calculated as D 1 =3.89×10−3 C+1.85×10−4 (r 2 =0.9987. For the second derivative spectrophotometry, the response (d 2 A/dλ2 of standard solutions was measured at 241.0 nm. The calibration curve was constructed by plotting d 2 A/dλ2 values against concentrations 0.5-20.0 μgml−1 of letrozole standards in methanol. The regression equation of the linear calibration graph was calculated as D 2 =-1.59×10−3 C -4.66×10−4 (r 2 =0.9985. The AUC-spectrophotometric method was based on the calculation of Area under Curve (AUC, for analysis of letrozole in the wavelength range of 235.0-245.0 nm. The calibration curve was constructed by plotting AUC values against concentrations 0.25-20.0 μgml−1 , of letrozole. The regression equation of the linear calibration graph was calculated as AUC=1.132C+0.2153 (r 2 =0.9994. The methods were validated by following the analytical performance parameters suggested by the International Conference on Harmonization (ICH. All validation parameters were within the acceptable range. The developed methods were successfully applied to estimate the amount of letrozole in pharmaceutical formulations.

  5. Spectrophotometric methods for the determination of letrozole in bulk and pharmaceutical dosage forms (United States)

    Acharjya, Sasmita Kumari; Mallick, Priyambada; Panda, Pinakini; Kumar, K. Ravi; Annapurna, M. Mathrusri


    Ultraviolet (UV), first derivative, second derivative, and AUC-spectrophotometric methods for the determination of letrozole in pharmaceutical formulations have been developed. For UV-spectrophotometry, the standard solutions were measured at 240.0 nm. The linearity ranges were found to be 0.25–20.0 μgml–1 in methanol and the regression equation was A=1.20×10–1C+2.22×10–2(r2=0.9994). For the first derivative spectrophotometry, the response (dA/dλ) of standard solutions was measured at 224.0 nm. The calibration curve was constructed by plotting dA/dλ values against concentrations 0.25–20.0 μgml–1, of letrozole. The regression equation of the linear calibration graph was calculated as D1=3.89×10–3C+1.85×10–4(r2=0.9987). For the second derivative spectrophotometry, the response (d2A/dλ2) of standard solutions was measured at 241.0 nm. The calibration curve was constructed by plotting d2A/dλ2 values against concentrations 0.5–20.0 μgml–1 of letrozole standards in methanol. The regression equation of the linear calibration graph was calculated as D2=-1.59×10–3C-4.66×10–4(r2=0.9985). The AUC-spectrophotometric method was based on the calculation of Area under Curve (AUC), for analysis of letrozole in the wavelength range of 235.0–245.0 nm. The calibration curve was constructed by plotting AUC values against concentrations 0.25–20.0 μgml–1, of letrozole. The regression equation of the linear calibration graph was calculated as AUC=1.132C+0.2153 (r2=0.9994). The methods were validated by following the analytical performance parameters suggested by the International Conference on Harmonization (ICH). All validation parameters were within the acceptable range. The developed methods were successfully applied to estimate the amount of letrozole in pharmaceutical formulations. PMID:22247870

  6. Spectrophotometric method for estimation of amiloride in bulk and tablet dosage form

    Directory of Open Access Journals (Sweden)

    Aitha Vijaya Lakshmi


    Full Text Available Introduction: Amiloride chemically, 3,5-diamino-6-chloro-N-(diaminomethylene pyrazine-2-carboxamide. It is used in the management of congestive heart failure, available as Amifru tab, Amimide. It causes adverse effects like Nausea, diarrhea and dizziness. Materials: 0.1 N Hydrochloric acid, 0.1 N Sodium hydroxide and 1 mg/ml amiloride drug solution were required. Spectral and absorbance measurements were made using ELICO UV-160 double beam Spectrophotometer. Method: Amiloride drug solution concentration range of 25 to 125ug/ml in 0.1N HCl medium was scanned over the wave length range of 235-320 against blank prepared in 0.1N NaOH solution. Two wavelengths are selected one at positive peak 245 nm and another at negative peak 290 nm, the amplitude is calculated from these values. Results and Discussion: The sum of the absolute values at these wavelengths is called amplitude. The amplitude is proportional to the amount of drug. High accuracy, reproducibility and low t-values were reported from the calibration curve plotted with the amplitude verses amount of drug. So the proposed method is simple, less time consuming and it can be successfully adopted for the estimation of amiloride.

  7. Mechanochemical Effects on the Synthesis of Copper Orthophosphate and cyclo-Tetraphosphate Bulks by the Hydrothermal Hot Pressing Method

    Directory of Open Access Journals (Sweden)

    Isao Tanaka


    Full Text Available Copper orthophosphate, Cu3(PO42, and cyclo-tetraphosphates, Cu2P4O12, were synthesized using phosphoric acid and basic copper carbonate, and then treated with a planetary mill for up to 360 minutes. The un-milled and milled samples were characterized by X-ray diffraction (XRD and Fourier transform infrared (FT-IR spectroscopy. SEM images, particle size distribution, specific surface area, UV-Vis reflectance spectra were also used to evaluate the materials. The un-milled and milled materials were used to fabricate copper phosphate bulks by a hydrothermal hot pressing method. The influence of powder condition on the sintering behavior of the copper phosphates was studied.

  8. Quantification of Newly Discovered Anti-Cancer Drug Enzalutamide in Bulk and Synthetic Mixture by Stability Indicating TLC method. (United States)

    Chhalotiya, Usmangani K; Prajapati, Dharmendra J; Prajapati, Minesh D; Patel, Jalpa U; Desai, Jaineel


    Objective A impressionable, discriminatory and precise stability indicating high performance thin layer chromatographic method has been developed and validated for the estimation of of Enzalutamide in bulk and synthetic mixture. Method The method engaged HPTLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase while the solvent system was ethyl acetate: toluene (4.5:5.5, v/v). The Rf value of enzalutamide was detected to be 0. 39 ± 0. 005 and the densitometric analysis were carried out in absorbance mode at 246 nm. The linear regression analysis data for the calibration plots presented a virtuous linear relationship for enzalutamide over a concentration range of 20 - 1000ng/band. Results The limit of detection and limit of quantification for enzalutamide was found to be 9.05 and 27.43ng/band. Enzalutamide was imperilled to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photolytic degradation. The degraded product peaks were well resolved from the pure drug peak with substantial difference in their Rf values. Conclusion Stressed samples were assayed using developed TLC technique. Suggested method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of enzalutamide in synthetic mixture. Copyright© Bentham Science Publishers; For any queries, please email at

  9. Novel LC Method Development and Validation for Simultaneous Determination of Montelukast and Doxofylline in Bulk and Pharmaceutical Dosage Forms

    Directory of Open Access Journals (Sweden)

    Gadapa Nirupa


    Full Text Available A novel rapid HPLC method was developed for simultaneous determination of montelukast and doxofylline in bulk and pharmaceutical dosage forms. Development of an analytical method for simultaneous estimation of drugs requires a lot of efforts and of course it is a challenging task. The method was developed by using C18 (150 mm×4.6 mm, 5 μm column; mobile phase consisting of methanol and phosphate buffer at pH 4.5; the flow rate of 1.0 mL/min and ultraviolet detection at 280 nm. Both drugs were sufficiently resolved having retention time of 4.7 min and 1.9 min for montelukast and doxofylline, respectively. The method was validated as per ICH Guidelines for various parameters like precision, linearity, accuracy, ruggedness, and robustness. The validated method was applied to the commercially available pharmaceutical dosage form and obtained the desired result.

  10. Two methods of tuning threshold voltage of bulk FinFETs with replacement high-k metal-gate stacks (United States)

    Xu, Miao; Zhu, Huilong; Zhang, Yanbo; Xu, Qiuxia; Zhang, Yongkui; Qin, Changliang; Zhang, Qingzhu; Yin, Huaxiang; Xu, Hao; Chen, Shuai; Luo, Jun; Li, Chunlong; Zhao, Chao; Ye, Tianchun


    In this work, we propose two threshold voltage (VTH) tuning methods for bulk FinFETs with replacement high-k metal gate. The first method is to perform a vertical implantation into fin structure after dummy gate removal, self-aligned forming halo & punch through stop pocket (halo & PTSP) doping profile. The second method is to execute P+/BF2+ ion implantations into the single common work function (WF) layer in N-/P-FinFETs, respectively. These two methods have been investigated by TCAD simulations and MOS-capacitor experiments respectively, and then integrated into FinFET fabrication successfully. Experimental results show that the halo & PTSP doping profile can reduce VTH roll off and total variation. With P+/BF2+ doped WF layer, the VTH-sat shift -0.43 V/+1.26 V for N-FinFETs and -0.75 V/+0.11 V for P-FinFETs, respectively, with gate length of 500 nm. The proposed two methods are simple and effective for FinFET VTH tuning, and have potential for future application of massive production.

  11. Method of aeration disinfecting and drying grain in bulk and pretreating seeds and a transverse blow silo grain dryer therefor (United States)

    Danchenko, Vitaliy G [Dnipropetrovsk, UA; Noyes, Ronald T [Stillwater, OK; Potapovych, Larysa P [Dnipropetrovsk, UA


    Aeration drying and disinfecting grain crops in bulk and pretreating seeds includes passing through a bulk of grain crops and seeds disinfecting and drying agents including an ozone and air mixture and surrounding air, subdividing the disinfecting and drying agents into a plurality of streams spaced from one another in a vertical direction, and passing the streams at different heights through levels located at corresponding heights of the bulk of grain crops and seeds transversely in a substantially horizontal direction.

  12. Magnetic Forces Investigation of Bulk HTS over Permanent Magnetic Guideway under Different Lateral Offset with 3D-Model Numerical Method

    Directory of Open Access Journals (Sweden)

    Yiyun Lu


    Full Text Available Magnetic forces of a cylinder shape bulk high-temperature superconductor (HTS over a permanent magnet guideway (PMG are studied mathematically. One cylindrical bulk HTS with a diameter of 30 mm and 15 mm in height is used. Two types of PMG are employed for external magnetic fields consideration. The relationship of magnetic forces of bulk HTS under different lateral offsets over PMG is studied with 3D-model finite element method (FEM. The calculation results show that the maximum magnetic levitation force of bulk HTS over PMG is tightly related to the applied magnetic field distribution. For the symmetrical PMG, the maximum magnetic levitation force decreases linearly with the increase of lateral offset of the bulk sample. For the Halbach PMG, when lateral offset changes from 0 mm to 25 mm, the maximum magnetic levitation force increases with the increase of lateral offset of the bulk HTS. When the lateral offset exceeds the center of the Halbach by 25 mm, the maximum levitation force decreases rapidly with the increase of the lateral offset of the bulk sample.

  13. Development and validation of a simple spectrophotometric method for the determination of methyldopa in both bulk and marketed dosage formulations

    Directory of Open Access Journals (Sweden)

    Paulo Roberto da Silva Ribeiro


    Full Text Available A simple, precise, sensitive, rapid, specific and economical spectrophotometric method was developed to determine methyldopa (MTD content in bulk and pharmaceutical dosage formulations. The proposed method was based on the formation of a colored product from the nitrosation reaction of MTD with sodium nitrite in an acid medium. The resultant nitroso derivative species reacts further with sodium hydroxide and is converted it into a more stable compound. This yellow nitrosation product exhibited an absorption maximum at 430 nm. Beer's Law was obeyed in a concentration range of 6.37 to 82.81 μg mL-1 MTD with an excellent coefficient of determination (R2 = 0.9998. No interference was observed from common excipients in formulations. The results showed the method to be simple, accurate and readily applied for the determination of MTD in pure form and in pharmaceutical preparations. The analytical results obtained for these products using the proposed method are in agreement with those of the Brazilian Pharmacopoeia procedure at a 95% confidence level.

  14. Arsenic speciation results (United States)

    U.S. Environmental Protection Agency — Linear combination fitting results of synchrotron data to determine arsenic speciation in soil samples. This dataset is associated with the following publication:...

  15. Searching for speciation genes

    DEFF Research Database (Denmark)

    Holt, Benjamin George; Côté, Isabelle M; Emerson, Brent C


    Closely related species that show clear phenotypic divergence, but without obvious geographic barriers, can provide opportunities to study how diversification can occur when opportunities for allopatric speciation are limited. We examined genetic divergence in the coral reef fish genus Hypoplectrus...

  16. Uranium speciation in plants

    Energy Technology Data Exchange (ETDEWEB)

    Guenther, A.; Bernhard, G.; Geipel, G.; Reich, T.; Rossberg, A. [Forschungszentrum Rossendorf e.V., Inst. of Radiochemistry, Dresden (Germany); Nitsche, H. [Univ. of California at Berkeley and Lawrence Berkeley National Lab., Nuclear Sciences Div., Berkeley, CA (United States)


    Detailed knowledge of the nature of uranium complexes formed after the uptake by plants is an essential prerequisite to describe the migration behavior of uranium in the environment. This study focuses on the determination of uranium speciation after uptake of uranium by lupine plants. For the first time, time-resolved laser-induced fluorescence spectroscopy and X-ray absorption spectroscopy were used to determine the chemical speciation of uranium in plants. Differences were detected between the uranium speciation in the initial solution (hydroponic solution and pore water of soil) and inside the lupine plants. The oxidation state of uranium did not change and remained hexavalent after it was taken up by the lupine plants. The chemical speciation of uranium was identical in the roots, shoot axis, and leaves and was independent of the uranium speciation in the uptake solution. The results indicate that the uranium is predominantly bound as uranyl(VI) phosphate to the phosphoryl groups. Dandelions and lamb's lettuce showed uranium speciation identical to lupine plants. (orig.)

  17. Potential sources and processes affecting speciated atmospheric mercury at Kejimkujik National Park, Canada: comparison of receptor models and data treatment methods (United States)

    Xu, Xiaohong; Liao, Yanyin; Cheng, Irene; Zhang, Leiming


    Source apportionment analysis was conducted with positive matrix factorization (PMF) and principal component analysis (PCA) methods using concentrations of speciated mercury (Hg), i.e., gaseous elemental mercury (GEM), gaseous oxidized mercury (GOM), and particulate-bound mercury (PBM), and other air pollutants collected at Kejimkujik National Park, Nova Scotia, Canada, in 2009 and 2010. The results were largely consistent between the 2 years for both methods. The same four source factors were identified in each year using PMF method. In both years, factor photochemistry and re-emission had the largest contributions to atmospheric Hg, while the contributions of combustion emission and industrial sulfur varied slightly between the 2 years. Four components were extracted with air pollutants only in each year using PCA method. Consistencies between the results of PMF and PCA include (1) most or all PMF factors overlapped with PCA components, (2) both methods suggest strong impact of photochemistry but little association between ambient Hg and sea salt, and (3) shifting of PMF source profiles and source contributions from one year to another was echoed in PCA. Inclusion of meteorological parameters led to identification of an additional component, Hg wet deposition in PCA, while it did not affect the identification of other components. The PMF model performance was comparable in 2009 and 2010. Among the three Hg forms, the agreements between model-reproduced and observed annual mean concentrations were excellent for GEM, very good for PBM, and acceptable for GOM. However, on a daily basis, the agreement was very good for GEM but poor for GOM and PBM. Sensitivity tests suggest that increasing sample size by imputation is not effective in improving model performance, while reducing the fraction of concentrations below method detection limit, by either scaling GOM and PBM to higher concentrations or combining them to reactive mercury, is effective. Most of the data

  18. A Validated RP-HPLC Method for the Determination of Recombinant Human Insulin in Bulk and Pharmaceutical Dosage Form

    Directory of Open Access Journals (Sweden)

    B. A. Moussa


    Full Text Available A modified RP-HPLC method was developed for the quantitative determination of recombinant human insulin in bulk and pharmaceutical dosage form with reduced retention time. Study of the effects of the column temperature, pH of the mobile phase and presence of vial additives (phenol and m-cresol, or impurities (A-21 Disamido on the accuracy of the assay were assessed. Separation was achieved using a Hypersil BDS C-18 column and the mobile phase was composed of solution A (aqueous solution of 28.3 anhydrous Na2SO4g/L, pH 2.3 and solution B (28.5 g anhydrous Na2SO4 g/L in 50:50 mixture of water and acetonitrile, pH 2.3 in a ratio 48:52 (v/v at 45–50 °C. The column temperature was 40 °C, the flow rate was 1 mL/min and detection was performed at 216 nm. The procedures were validated according to international conference on harmonization (ICH guidelines. Recovery study was done applying standard addition technique for further validation of the procedure. The retention time of recombinant human insulin was 19.7 min as compared to 29 min obtained by the reference method. Analytical conditions fluctuations or presence of vial additives or impurities did not show any significant effect on the accuracy of the method. The prepared standard insulin solution in 0.01 N HCl was found to be stable for 5 days. Statistical comparison showed no significant difference between the described method and reference method regarding the accuracy and precision. The modified method can be applied for routine quality control applications for determination of recombinant human insulin.

  19. Bulk Nanostructured Materials (United States)

    Koch, C. C.; Langdon, T. G.; Lavernia, E. J.


    This paper will address three topics of importance to bulk nanostructured materials. Bulk nanostructured materials are defined as bulk solids with nanoscale or partly nanoscale microstructures. This category of nanostructured materials has historical roots going back many decades but has relatively recent focus due to new discoveries of unique properties of some nanoscale materials. Bulk nanostructured materials are prepared by a variety of severe plastic deformation methods, and these will be reviewed. Powder processing to prepare bulk nanostructured materials requires that the powders be consolidated by typical combinations of pressure and temperature, the latter leading to coarsening of the microstructure. The thermal stability of nanostructured materials will also be discussed. An example of bringing nanostructured materials to applications as structural materials will be described in terms of the cryomilling of powders and their consolidation.

  20. New method for the speciation of ruthenium-based chemotherapeutics in human serum by conjoint liquid chromatography on affinity and anion-exchange monolithic disks. (United States)

    Martinčič, Anže; Milačič, Radmila; Vidmar, Janja; Turel, Iztok; Keppler, Bernhard K; Sčančar, Janez


    An important step in pharmacological characterisation of a candidate drug is the study of the drugs interactions with serum proteins. In the present work, conjoint liquid chromatography (CLC) was used for separation of ruthenium (Ru)-based drug candidates in human serum. CIM Protein G and CIM DEAE disks were assembled together in a single housing forming a CLC monolithic column. By applying isocratic elution with Tris-HCl-NaHCO3 buffer (pH 7.4) in the first min, followed by gradient elution with 1 mol L(-1) NH4Cl (pH 7.4) in the next 9 min, immunoglobulins (IgG) were retained by the Protein G disk enabling subsequent separation of unbound Ru species from Ru species bound to human serum transferrin (Tf) and albumin (HSA) on the CIM DEAE disk. Finally, elution with acetic acid (AcOH) in the next 3 min allowed separation of Ru species associated with IgG. Protein elution was followed on-line with UV detection at 278nm, while the separated Ru species were quantified by post-column isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS). The instrumental set-up enabled fast two-dimensional separation by affinity and ion-exchange modes to be carried out in a single chromatographic run. Two Ru-based chemotherapeutics: a newly synthesised compound chlorido(η6-p-cymene)(nalidixicato-κ2O,O)Ru(II) (1) and (H2im)[trans-Ru(III)Cl4(Him)2] (2; KP418), which is currently undergoing preclinical studies, were investigated. The CLC procedure applied is sensitive with low limit of detection (LOD) (0.027 μg Ru mL(-1) for (1)) and good method repeatability (RSD±3.5%). The experimental data revealed that it enables investigation of the kinetics of interaction of positively charged and neutral complexes of metallodrugs with serum proteins as well as the distribution of metallodrug species in human serum. However, negatively charged metallic complexes co-eluted with Tf and HSA and thus hindered their speciation analysis. An example of successful application of the

  1. New, simple and validated UV-spectrophotometric methods for the estimation of gatifloxacin in bulk and formulations. (United States)

    Venugopal, K; Saha, Ranendra N


    New, simple and cost effective UV-spectrophotometric methods were developed for the estimation of gatifloxacin in bulk and pharmaceutical formulations. Gatifloxacin was estimated at 286 nm in 100 mM phosphate buffer (pH 7.4) and 292 nm in 100 mM hydrochloric acid (pH 1.2). Linearity range was found to be 1-18 mug ml(-1) (regression equation: absorbance=0.0684 x Concentration in microg ml(-1) + 0.0050; r2 = 0.9998) in the phosphate buffer (pH 7.4) and 1-14 microg ml(-1) (regression equation: absorbance = 0.0864 x Concentration in microg ml(-1) + 0.0027; r2 = 0.9999) in hydrochloric acid medium (pH 1.2). The apparent molar absorptivity was found to be 2.62 x 10(4) l mol(-1) cm(-1) in the phosphate buffer and 3.25 x 10(4) l mol(-1) cm(-1) in hydrochloric acid media. In both the proposed methods sandell's sensitivity was found to be about 0.01 microg cm(-2)/0.001A. These methods were tested and validated for various parameters according to ICH guidelines and USP. The quantitation limits were found to be 0.312 and 0.3 microg ml(-1) in the phosphate buffer and hydrochloric acid medium, respectively. The proposed methods were successfully applied for the determination of gatifloxacin in pharmaceutical formulations (tablets, injection and ophthalmic solution). The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation <2%), while being simple, cheap and less time consuming and can be suitably applied for the estimation of gatifloxacin in different dosage forms and dissolution studies.

  2. A new spectrofluorometric method for the determination of total arsenic in sediments and its application to kinetic speciation

    Digital Repository Service at National Institute of Oceanography (India)

    Chakraborty, P.; RaghunadhBabu, P.V.; Sarma, V.V.

    A simple and sensitive spectrofluorometric method has been developed for the determination of arsenic (As) using rhodamine-B as a fluorescent agent. This method is based on the reaction of As(III) with potassium iodate (KIO sub(3)) in acid medium...

  3. The EU network on trace element speciation in full swing

    NARCIS (Netherlands)

    Cornelis, R.; Camara, C.; Ebdon, L.; Pitts, L.; Sperling, M.; Morabito, R.; Donard, O.F.X.; Crews, H.; Larsen, E.H.; Neidhart, B.; Ariese, F.; Rosenberg, E.; Berrouiguet, O.; Morrison, G.M.; Cordier, G.; Adams, F.; Dero, B.; Marshall, J.; Stojanik, B.; Ekvall, A.; Quevauviller, P.


    The EC-funded thematic network 'Speciation 21' links scientists in analytical chemistry working in method development for the chemical speciation of trace elements, and potential users from industry and representatives of legislative agencies, in the field of environment, food and occupational

  4. Systems and Methods for Implementing Bulk Metallic Glass-Based Strain Wave Gears and Strain Wave Gear Components (United States)

    Hofmann, Douglas C. (Inventor); Wilcox, Brian (Inventor)


    Bulk metallic glass-based strain wave gears and strain wave gear components. In one embodiment, a strain wave gear includes: a wave generator; a flexspline that itself includes a first set of gear teeth; and a circular spline that itself includes a second set of gear teeth; where at least one of the wave generator, the flexspline, and the circular spline, includes a bulk metallic glass-based material.

  5. A novel method for the quantification, characterisation and speciation of silver nanoparticles in earthworms exposed in soil

    NARCIS (Netherlands)

    Makama, S.I.; Peters, R.J.B.; Undas, A.K.; Brink, van den N.W.


    Currently, metal engineered nanoparticles (ENPs) in tissues are generally quantified based on total concentrations after acid digestion of samples. Electron microscopy has also been used for non-quantitative characterisation of NPs in situ, and can be enhanced with tissue-processing methods that can

  6. Development of off-line layer chromatographic and total reflection X-ray fluorescence spectrometric methods for arsenic speciation

    Energy Technology Data Exchange (ETDEWEB)

    Mihucz, Victor G. [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); Moricz, Agnes M. [L. Eoetvoes University, Department of Chemical Technology and Environmental Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Kroepfl, Krisztina [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Szikora, Szilvia [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Tatar, Eniko [Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Parra, Lue Meru Marco [Universidad Centro-occidental Lisandro Alvarado, Decanato de Agronomia, Departamento de Quimica y Suelos Unidad de Analisis Instrumental, Apartado Postal 4076, Cabudare 3023 (Venezuela); Zaray, Gyula [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary) and Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary) and L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary)]. E-mail:


    Rapid and low cost off-line thin layer chromatography-total reflection X-ray fluorescence spectrometry and overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods have been developed for separation of 25 ng of each As(III), As(V), monomethyl arsonic acid and dimethylarsinic acid applying a PEI cellulose stationary phase on plastic sheets and a mixture of acetone/acetic acid/water = 2:1:1 (v/v/v) as eluent system. The type of eluent systems, the amounts (25-1000 ng) of As species applied to PEI cellulose plates, injection volume, development distance, and flow rate (in case of overpressured thin layer chromatography) were taken into consideration for the development of the chromatographic separation. Moreover, a microdigestion method employing nitric acid for the As spots containing PEI cellulose scratched from the developed plates divided into segments was developed for the subsequent total reflection X-ray fluorescence spectrometry analysis. The method was applied for analysis of root extracts of cucumber plants grown in As(III) containing modified Hoagland nutrient solution. Both As(III) and As(V) were detected by applying the proposed thin layer chromatography/overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods.

  7. Speciation analysis of gadolinium chelates in hospital effluents and wastewater treatment plant sewage by a novel HILIC/ICP-MS method. (United States)

    Künnemeyer, Jens; Terborg, Lydia; Meermann, Björn; Brauckmann, Christine; Möller, Ines; Scheffer, Andy; Karst, Uwe


    The behavior of Gd chelates used in magnetic resonance imaging (MRI) within the process of sewage treatment is widely unknown. Due to the varying toxicity of the particular Gd species [J. M. Idee et al. Fundam. Clin. Pharmacol. 2006, 20, 563-576], it is important to not only investigate total Gd concentrations, but the Gd species as well. This work describes a novel method for speciation analysis of the most important gadolinium chelates in wastewaters. This novel approach consists of coupling hydrophilic interaction chromatography (HILIC) with inductively coupled plasma mass spectrometry (ICP-MS). HILIC/ICP-MS exhibits high separation efficiency for the simultaneous separation of the five predominantly applied MRI contrast agents and the required selectivity and sensitivity for trace determination in wastewater samples. For the first time, the distribution of particular Gd chelate complexes was determined in hospital effluent, municipal sewage, and wastewater treatment plant (WWTP) samples. The data were compared with the total concentration of Gd as determined by ICP-MS. The active compounds of Multihance, Dotarem, and Gadovist were identified in local WWTP samples. Interestingly, the macrocyclic, nonionic compound Gd-BT-DO3A (Gadovist) was found to be the most abundant Gd complex in all investigated samples. This is in contrast to prevalent assumptions that linear ionic Gd chelates such as Gd-DTPA (Magnevist) would be the predominant species [G. Morteani et al. Environ. Geochem. Health 2006, 28, 257-264 and M. Bau and P. Dulski, Earth Planet. Sci. Lett. 1996, 143, 245-255]. Although contrast agent concentrations tend to be reduced during wastewater treatment, Gd-BT-DO3A was still found in WWTP effluents.

  8. Gas chromatographic sulphur speciation in heavy crude oil using a modified standard D5623 method and microfluidic Deans switching. (United States)

    Heshka, Nicole E; Choy, Joanne M; Chen, Jinwen


    A modification to American Society for Testing and Materials (ASTM) method D5623 is proposed to enable successful and repeatable analysis of heavy crude oil samples. A two-dimensional gas chromatography configuration was implemented, with separation of sulphur compounds occurring on two columns. A Deans switch is used to enable heart-cutting of volatile sulphur compounds onto a DB-Sulfur stationary phase, and separation occurs concurrently with the backflushing of the primary column. The use of a sulphur-selective detector increases selectivity, and 22 volatile sulphur species are quantified in less than 15min, which is almost half the time of the original ASTM method. Samples ranging from light distillation cuts to whole crudes (boiling from 100°C to >750°C) were analyzed with minimal sample preparation. The calculated limit of detection was 0.7mg/kg, repeatability was 3% relative standard deviation (RSD), and a linear range of 1-250mg/kg was obtained, with an R2 value of 0.994 or better, depending on the compound. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  9. A validated stability indicating HPLC method for the determination of process-related impurities in pantoprazole bulk drug and formulations

    Directory of Open Access Journals (Sweden)

    Saurabh Pandey


    Full Text Available A stability-indicating high-performance liquid chromatographic (HPLC method was developed with short run time and validated for the assay of process related impurities of pantoprazole in bulk form. Resolution of drug, its potential impurities and degradation products were achieved on a Hypersil ODS column utilizing a gradient with 0.01 M phosphate buffer of pH 7 and acetonitrile as eluent, at the detection wavelength of 290 nm. Flow rate was set at 1 mL min-1. The procedure was found to be specific, linear (r=0.999, recovery (97.9-103%, LOD (0.043-0.047 µgmL-1, LOQ (0.13-0.14 µgmL-1 and robust. Acceptable robustness indicates that the assay method remains unaffected by small but deliberate variations. Pantoprazole was found to degrade in acidic, oxidative and under photolytic stress conditions. The drug was stable to alkaline and dry heat conditions. This method has been successively applied to pharmaceutical formulation and no interference from the excipients was found.Desenvolveu-se método indicador de estabilidade por Cromatografia a Líquido de Alta Eficiência (CLAE com pequeno tempo de corrida e validado para o ensaio de impurezas relacionadas ao processo de produção de pantoprazol em batelada. A determinação do fármaco, de suas impurezas potenciais e dos produtos de degradação foi realizada com coluna de ODS Hypersil, utilizando gradiente com tampão de fosfato 0,01 M pH 7 e acetonitrila como eluente, no comprimento de onda de detecção de 290 nm. A velocidade de fluxo foi fixada em 1 mLmin-1. O procedimento se mostrou específico, linear (r=0,999, com recuperação (97,9-103%, LOD (0,043-0,047 µgmL-1, LOQ (0,13-0,14 µg mL-1 e robusto. Robustez aceitável indica que o método de ensaio não é afetado por variações pequenas, exceto as planejadas. O pantoprazole degradou em condições ácidas, oxidativas e sob condições de estresse fotolítico. O fármaco foi estável em condições alcalinas e de calor seco. Este m

  10. 40 CFR Appendix E to Subpart E of... - Interim Method of the Determination of Asbestos in Bulk Insulation Samples (United States)


    ... manner prescribed in Reference 5 and information on design of sampling and analysis programs may be found... • Sample Mill: SPEX, Inc., freezer mill or equivalent. • Bulk Sample Holders • Silver Membrane Filters: 25...., Spex Freezer Mill, or equivalent) for a maximum time of 10 min. is recommended to obtain satisfactory...


    Background: Determination of arsenic species in human saliva is potentially useful for biomonitoring of human exposure to arsenic and for studying arsenic metabolism. However, there is no report on the speciation analysis of arsenic in saliva. Methods: Arsenic species in saliva ...

  12. Actinide speciation in environmental remediation

    Energy Technology Data Exchange (ETDEWEB)

    Plaue, Jon; Czerwinski, Ken R. [Massachusetts Institute of Technology, Nuclear Engineering Dept., Cambridge, MA (United States)


    Environmental actinide remediation is often performed in the absence of a clear understanding of the contaminant chemical forms. Remediation efforts are more concerned with the initial and final concentration of the contaminant actinides. Allowable final concentrations of actinides in remediation sites are mainly based on expected dose or prenegotiated levels. However, understanding the chemical forms of actinides in the environment is key to assessing their long-term behavior and developing enhanced analytical methods for their environmental detection. The dominant environmental chemical form will dictate the actinide transport behavior through solubility, colloid formation, or the interaction with natural ligands. This information can be used to evaluate the fate and potential transport of actinides. If the dominant environmental chemical species are understood, analytical methods for enhanced counting statistics and a reduction of counting error can be developed. A reduction in counting error will increase the fraction of verifiable waste below a given threshold, thereby increasing the rate of site clean up while reducing the cost. The impact of actinide speciation is presented in 2 sites contaminated with Am and Pu undergoing remediation. Actinide speciation has affected remediation strategies, regulatory response, and costs. (author)

  13. Bulk-Fill Resin Composites

    DEFF Research Database (Denmark)

    Benetti, Ana Raquel; Havndrup-Pedersen, Cæcilie; Honoré, Daniel


    the restorative procedure. The aim of this study, therefore, was to compare the depth of cure, polymerization contraction, and gap formation in bulk-fill resin composites with those of a conventional resin composite. To achieve this, the depth of cure was assessed in accordance with the International Organization...... for Standardization 4049 standard, and the polymerization contraction was determined using the bonded-disc method. The gap formation was measured at the dentin margin of Class II cavities. Five bulk-fill resin composites were investigated: two high-viscosity (Tetric EvoCeram Bulk Fill, SonicFill) and three low......-viscosity (x-tra base, Venus Bulk Fill, SDR) materials. Compared with the conventional resin composite, the high-viscosity bulk-fill materials exhibited only a small increase (but significant for Tetric EvoCeram Bulk Fill) in depth of cure and polymerization contraction, whereas the low-viscosity bulk...

  14. SPECIATE and using the Speciation Tool to prepare VOC and PM chemical speciation profiles for air quality modeling (United States)

    This product provides training to air pollution inventory and modeling professionals to understand the US EPA's SPECIATE database base and Speciation Tool and their use to develop speciated emission inventories.

  15. Robustness of the Approximate Likelihood of the Protracted Speciation Model. (United States)

    Simonet, Camille Anna; Scherrer, Raphaël; Rego-Costa, Artur; Etienne, Rampal S


    The protracted speciation model presents a realistic and parsimonious explanation for the observed slowdown in lineage accumulation through time, by accounting for the fact that speciation takes time. A method to compute the likelihood for this model given a phylogeny is available and allows estimation of its parameters (rate of initiation of speciation, rate of completion of speciation, and extinction rate) and statistical comparison of this model to other proposed models of diversification. However this likelihood computation method makes an approximation of the protracted speciation model to be mathematically tractable: it sometimes counts fewer species than one would do from a biological perspective. This approximation may have large consequences for likelihood-based inferences: it may render any conclusions based on this method completely irrelevant. Here we study to what extent this approximation affects parameter estimations. We simulated phylogenies from which we reconstructed the tree of extant species according to the original, biologically meaningful protracted speciation model and according to the approximation. We then compared the resulting parameter estimates. We found that the differences were larger for high values of extinction rates and small values of speciation-completion rates. Indeed, a long speciation-completion time and a high extinction rate promote the appearance of cases to which the approximation applies. However, surprisingly, the deviation introduced is largely negligible over the parameter space explored, suggesting that this approximate likelihood can be applied reliably in practice to estimate biologically relevant parameters under the original protracted speciation model. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  16. Structural differences existing in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}: Investigated by experimental and theoretical methods

    Energy Technology Data Exchange (ETDEWEB)

    Nigam, Sandeep, E-mail: [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Sudarsan, V., E-mail: [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Majumder, C.; Vatsa, R.K. [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India)


    Present manuscript deals with the structural changes associated with transformation of bulk Y{sub 2}Sn{sub 2}O{sub 7} into nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. Nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} both undoped and Eu{sup 3+} doped, were prepared at a relatively low temperature (700 °C) and investigated for their structural and luminescence properties and compared them with that of bulk Y{sub 2}Sn{sub 2}O{sub 7} sample prepared by the solid-state method at 1300 °C. Significant distortion in geometry and electron density distribution around Y{sup 3+}/Eu{sup 3+} ions in nanoparticles are confirmed from the Rietveld refinement of the powder X-ray diffraction patterns and theoretical calculations based on the density functional theory (DFT). The SnO{sub 6} octahedron in Y{sub 2}Sn{sub 2}O{sub 7} is more expanded in nanoparticles compared to bulk. Iso-surface density distribution reveals that while bulk sample shows typical ionic feature in Y/Eu--O bonds, nanoparticle sample shows sharing of electron density along bond axis pertaining to covalent character. These inferences are further supported by the doped Eu{sup 3+} luminescence and calculated Ω{sub 2} and Ω{sub 4} parameters. - Graphical abstract: YO{sub 8} scalenohedron present in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}.Variation of the electron density around Y{sup 3+} ions in YO{sub 8} polyhedron is also shown in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. The difference in the extent of ionic/covalent nature of the Y--O bond is clearly seen the contour plot of electron density. Highlights: ► YO{sub 8} scalenohedron is axially and equatorially distorted in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles. ► Enlargement of SnO{sub 6} octahedron in nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} compared to bulk. ► Less symmetric charge distribution around Y{sup 3+} ions in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles.

  17. Mixing and speciation algorithms for geochemical and reactive transport problems


    De Gaspari, Francesca


    Geochemical and reactive transport modelling are essential tools in hydrogeology. They help to identify and assess geochemical processes occurring in applications such as groundwater contamination, water-rock interactions and geologic carbon sequestration. In this thesis we present methods for mixing and speciation calculations to be used for both interpretation of hydrochemical data and numerical modelling. The first method presented allows solving geochemical speciation using redundant i...

  18. Preparation by Poly(Acrylic Acid) Sol-Gel Method and Thermoelectric Properties of γ-Na x CoO2 Bulk Materials (United States)

    Li, Xiaoyu; Zhang, Li; Tang, Xinfeng


    γ-Na x CoO2 single-phase powders have been synthesized by a poly(acrylic acid) (PAA) sol-gel (SG) method, and γ-Na x CoO2 bulk ceramic fabricated using spark plasma sintering. The effects of the PAA concentration on the sample phase composition and morphology were investigated. The thermoelectric properties of the γ-Na x CoO2 bulk ceramic were also studied. The results show that the PAA concentration did not significantly affect the crystalline phase of the product. However, agglomeration of γ-Na x CoO2 crystals was suppressed by the steric effect of PAA. The Na x CoO2 bulk ceramic obtained using the PAA SG method had higher crystallographic anisotropy, better chemical homogeneity, and higher density than the sample obtained by solid-state reaction (SSR), leading to improved thermoelectric performance. The PAA SG sample had power factor (in-plane PF = σS 2) of 0.61 mW m-1 K-2 and dimensionless figure of merit ( ZT) along the in-plane direction of 0.19 at 900 K, higher than for the SSR sample (in-plane PF = 0.51 mW m-1 K-2, in-plane ZT = 0.17). These results demonstrate that a simple and feasible PAA SG method can be used for synthesis of Na x CoO2 ceramics with improved thermoelectric properties.

  19. Developing bulk exchange spring magnets

    Energy Technology Data Exchange (ETDEWEB)

    Mccall, Scott K.; Kuntz, Joshua D.


    A method of making a bulk exchange spring magnet by providing a magnetically soft material, providing a hard magnetic material, and producing a composite of said magnetically soft material and said hard magnetic material to make the bulk exchange spring magnet. The step of producing a composite of magnetically soft material and hard magnetic material is accomplished by electrophoretic deposition of the magnetically soft material and the hard magnetic material to make the bulk exchange spring magnet.

  20. Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry; Redoxspeziation von endlagerrelevanten Elementen mit Hilfe von Trennmethoden gekoppelt an ein Massenspektrometer mit induktiv gekoppeltem Plasma

    Energy Technology Data Exchange (ETDEWEB)

    Graser, Carl-Heinrich


    The long-term safety assessment for nuclear waste repositories requires a detailed understanding of the chemistry of actinide elements in the geosphere. The development of advanced analytical tools is required to gain detailed insights into actinide redox speciation in a given system. The mobility of radionuclides is mostly determined by the geochemical conditions which control the redox state of radionuclides. Besides the longlived radionuclides plutonium (Pu) and neptunium (Np), which are key elements in high level nuclear waste, iron (Fe) represents a main component in natural systems controlling redox related geochemical processes. Analytical techniques for determining oxidation state distribution for redox sensitive radionuclides and other metal ions often have a lack of sensitivity. The detection limits of these methods (i.e. UV/vis, TRLFS, XANES) are in general in the range of ≥ 10{sup -6} mol.L{sup -1}. As a consequence ultrasensitive new analytical techniques are required. Capillary electrophoresis (CE) and ion chromatography (IC) are powerful separation methods for metal ions. In the course of this thesis different speciation method for iron, neptunium and plutonium were optimized. With the optimized setup redox speciation analysis of these elements in different samples were done. Furthermore CE hyphenated to inductively coupled plasma sector field mass spectrometry (CE - ICP - SF - MS) was used to measure the redox speciation of Pu (III, IV, V, VI), Np (IV, V, VI) and Fe (II, III) at concentrations lower than 10{sup -7} mol.L{sup -1}. CE coupling and separation parameters such as sample gas pressure, make up flow rate, capillary position, auxiliary gas flow, as well as the electrolyte system were optimized to obtain the maximum sensitivity. The methodes detection limits are 10{sup -12} mol.L{sup -1} for Np and Pu. The various oxidation state species of Pu and Np in different samples were separated by application of an acetate based electrolyte system

  1. Preparation of a bulk Fe83B17 soft magnetic alloy by undercooling and copper-mold casting methods (United States)

    Yang, Changlin; Sheng, Gang; Chen, Guiyun; Liu, Feng


    Bulk Fe83B17 eutectic alloy rods with diameters up to 3 mm were prepared by undercooling solidification combined with Cu-mold casting. The results showed that the rapid solidification led to an increase in the nucleation rate, an inhibition of the grain growth and a competition between a stable Fe2B phase and a metastable Fe3B phase. Then, pure nano-lamellar eutectic microstructures and the metastable Fe3B phase were successfully obtained in as-solidified alloys, which resulted in improved soft magnetic properties.

  2. The EU network on trace element speciation in full swing

    DEFF Research Database (Denmark)

    Cornelis, R.; Camara, C.; Ebdon, L.


    The EC-funded thematic network 'Speciation 21' links scientists in analytical chemistry working in method development for the chemical speciation of trace elements, and potential users from industry and representatives of legislative agencies, in the field of environment, food and occupational...... as the influence of packing materials. Once the analytical methodology for the measurement of the trace element species has been optimised, the importance of trace element speciation will grow enormously. Food sciences, material sciences, medicine and occupational health, environmental sciences and related fields...

  3. Especiação analítica de compostos de arsênio empregando métodos voltamétricos e polarográficos: uma revisão comparativa de suas principais vantagens e aplicações Speciation analysis of arsenic compounds by voltammetric and polarographic methods: a comparative review of their main advantages and applications

    Directory of Open Access Journals (Sweden)

    Leandro Machado de Carvalho


    Full Text Available This paper provides a review on voltammetric and polarographic methods for the speciation analysis of inorganic and organic arsenic compounds in different matrices. A discussion on the main advantages of electroanalytical methods in comparison with other analytical methods employed for arsenic speciation is presented. The mechanistic aspects of the most relevant techniques employing cathodic and anodic stripping voltammetry as well as polarographic methods published in the last twenty five years are summarized and discussed. The bibliographic references cited in this work were selected from the Web of Science (published by the ISI and the main journals of analytical chemistry.

  4. Speciation of long-lived radionuclides in the environment

    Energy Technology Data Exchange (ETDEWEB)

    Xiaolin Hou


    This project started in November 2005 and ended in November 2008, the work and research approaches are summarized in this report. This project studied the speciation of radionuclides in environment. A number of speciation analytical methods are developed for determination of species of 129I, 99Tc, isotopes of Pu, and 237Np in seawater, fresh water, soil, sediment, vegetations, and concrete. The developed methods are used for the investigation of the chemical speciation of these radionuclides as well as their environmental behaviours, especially in Danish environment. In addition the speciation of Pu isotopes in waste samples from the decommissioning of Danish nuclear facilities is also investigated. The report summarizes these works completed in this project. Through this research project, a number of research papers have been published in the scientific journals, the research results has also been presented in the Nordic and international conference/meeting and communicated to international colleagues. Some publications are also enclosed to this report. (au)

  5. High-Performance Liquid Chromatographic and High-Performance Thin-Layer Chromatographic Method for Quantitative Estimation of Dolutegravir Sodium in Bulk Drug and Pharmaceutical Dosage Form


    Bhavar, Girija B.; Sanjay S. Pekamwar; Aher, Kiran B.; Thorat, Ravindra S.; Chaudhari, Sanjay R.


    Simple, sensitive, precise, and specific high-performance liquid chromategraphic (HPLC) and high-performance thin-layer chromatographic (HPTLC) methods for the determination of dolutegravir sodium in bulk drug and pharmaceutical dosage form were developed and validated. In the HPLC method, analysis of the drug was carried out on the ODS C18 column (150 ? 4.6 mm, 5 ?m particle size) using a mixture of acetonitrile: water (pH 7.5) in the ratio of 80:20 v/v as the mobile phase at the flow rate 1...

  6. Development and Validation of a Stability-Indicating RP-HPLC Method for Rapid Determination of Doxycycline in Pharmaceutical Bulk and Dosage Forms

    Directory of Open Access Journals (Sweden)

    Shabnam Pourmoslemi, Soroush Mirfakhraee, Saeid Yaripour, Ali Mohammadi


    Full Text Available Background: A rapid stability-indicating RP-HPLC method for analysis of doxycycline in the presence of its degradation products was developed and validated. Methods: Forced degradation studies were carried out on bulk samples and capsule dosage forms of doxycycline using acid, base, H2O2, heat, and UV light as described by ICH for stress conditions to demonstrate the stability-indicating power of the method. Separations were performed on a Perfectsil® Target ODS column (3-5µm, 125 mm×4 mm, using a mobile phase consisting of methanol-50 mM ammonium acetate buffer (containing 0.1% v/v trifluoroacetic acid and 0.1% v/v triethylamine, pH 2.5 (50:50 v/v at room temperature. The flow rate was 0.8 mL/min. Results: The method linearity was investigated in the range of 25–500 µg/mL (r > 0.9999. The LOD and LOQ were 5 and 25 µg/mL, respectively. The method selectivity was evaluated by peak purity test using a diode array detector. There was no interference among detection of doxycycline and its stressed degradation products. Total peak purity numbers were in the range of 0.94-0.99, indicating the homogeneity of DOX peaks. Conclusion: These data show the stability-indicating nature of the method for quality control of doxycycline in bulk samples and capsule dosage forms.

  7. Speciation analysis, bioavailability and risk assessment of trace metals in herbal decoctions using a combined technique of in Vitro digestion and biomembrane filtration as sample pretreatment method. (United States)

    Li, Shun-Xing; Lin, Lu-xiu; Lin, Jing; Zheng, Feng-Ying; Wang, Qing-Xiang; Weng, Wen


    Sample preparation is the first crucial step in the speciation analysis, bioavailability and risk assessment of trace metals in plant samples such as herb and vegetables. Two bionic technologies titled 'in vitro digestion' and 'extraction with biomembrane' were developed for pre-treatment of herbal decoction. The decoctions of Aconiteum carmichaeli and Paeonia lactiflora were digested at body temperature, at the acidity of the stomach or intestine and with inorganic and organic materials (digestive enzymes were included for whole-bionic and excluded for semi-bionic) found in the stomach or intestine. Being similar to the biomembrane between the gastrointestinal tract and blood vessels, monolayer liposome was used as a biomembrane model. Affinity-monolayer liposome metals and water-soluble metals were used for speciation analysis and bioavailability assessment of copper and zinc in herbal decoction. In the decoction of Aconiteum carmichaeli and Paeonia lactiflora, Zn was mainly absorbed in the intestine and Cu was mainly absorbed by both stomach and intestine. The safe dosage for males and females is below 257.1 g/day Aconiteum carmichaeli and 529.4 g/day Paeonia lactiflora. Copyright © 2010 John Wiley & Sons, Ltd.

  8. New developed spectrophotometric method for simultaneous determination of salmeterol xinafoate and fluticasone propionate in bulk powder and Seritide® diskus inhalation

    Directory of Open Access Journals (Sweden)

    Ahmed Samir


    Full Text Available A new simple, accurate, precise, rapid and economical method was developed for the simultaneous determination of Salmeterol xinafoate and Fluticasone propionate in their binary mixture in bulk powder and Seritide diskus® inhalation. The new method depends on new calculations using the mixture’s absorbance at 225 and 256.5 nm where the absorptivity of Salmeterol xinafoate is double the absorptivity of Fluticasone propionate, while the content of Salmeterol xinafoate was determined by measuring the absolute value of the first derivative ultraviolet curves at 352 nm, without interference from Fluticasone propionate. The proposed method was validated and the results obtained by adopting the proposed method were statistically analyzed and compared with those obtained by reported methods.

  9. [Speciation analysis and toxicity of arsenic in realgar bioleaching solution]. (United States)

    Zhang, Jing-hong; Fan, Qin; Li, Hong-yu


    To analyze speciation and toxicity of arsenic in realgar bioleaching solution, and to explore its possible relation between speciation and toxicity. Capillary zone electrophoresis (CZE) can be used quickly and simply onto the simultaneous separation and quantitative determination of the speciation of arsenic in realgar bioleaching solution. The effects of three different realgar bioleaching liquids on the acute toxicity level of rat were also investigated as well. Parallel experiments with traditional processing realgar via gastric irrigation were conducted for comparison. There are three different arsenic species in realgar bioleaching solution (iAs(III), iAs(V) MMA(V)), and the processing method largely affected speciation and toxicity of arsenic of it. It was found that the toxicity level was decreased through increasing the amount of MMA(V). These results indicate that the species of arsenic may be tightly relationship to its toxicity in realgar bioleaching solution.

  10. Development and Validation of a RP-HPLC Method for Estimation of Montelukast Sodium in Bulk and in Tablet Dosage Form


    Singh R; Saini P; Mathur S; Singh G; Lal B


    The present work describes a simple, precise and accurate HPLC method for estimation of montelukast sodium in bulk and in tablet dosage form. The separation was achieved by using octadecylsilane column (C18) and acetonitrile:1 mM sodium acetate adjusted to pH 6.3 with acetic acid in proportion of 90:10 v/v as mobile phase, at a flow rate of 1.5 ml/min. Detection was carried out at 285 nm. The retention time of montelukast sodium was found to be 3.4 min. The limit of detection was found 1.31 &...

  11. Development and Validation of a RP-HPLC Method for Estimation of Montelukast Sodium in Bulk and in Tablet Dosage Form. (United States)

    Singh, R M; Saini, P K; Mathur, S C; Singh, G N; Lal, B


    The present work describes a simple, precise and accurate HPLC method for estimation of montelukast sodium in bulk and in tablet dosage form. The separation was achieved by using octadecylsilane column (C18) and acetonitrile:1 mM sodium acetate adjusted to pH 6.3 with acetic acid in proportion of 90:10 v/v as mobile phase, at a flow rate of 1.5 ml/min. Detection was carried out at 285 nm. The retention time of montelukast sodium was found to be 3.4 min. The limit of detection was found 1.31 µg/ml and limit of quantification 3.97 µg/ml. The accuracy and reliability of the proposed method was ascertained by evaluating various validation parameters like linearity (1-100 µg/ml), precision, accuracy and specificity according to ICH guidelines. The proposed method provides an accurate and precise quality control tool for routine analysis of montelukast sodium in bulk and in tablet dosage form.

  12. Monitoring metal speciation in the rivers meuse and rhine using DGT

    NARCIS (Netherlands)

    Cleven, Rob; Nur, Yusuf; Krystek, Petra; Van Den Berg, Gerard

    Although a number of metal speciation methods are nowadays available, most water quality regulations are based on total metal concentrations. One of the main reasons for the ignorance of speciation is the lack of methods with potentiality for monitoring. Conditions that have to be met by such

  13. Spectrophotometric and spectrofluorimetric methods for determination of certain biologically active phenolic drugs in their bulk powders and different pharmaceutical formulations (United States)

    Omar, Mahmoud A.; Badr El-Din, Kalid M.; Salem, Hesham; Abdelmageed, Osama H.


    Two simple and sensitive spectrophotometric and spectrofluorimetric methods for the determination of terbutaline sulfate, fenoterol hydrobromide, etilefrine hydrochloride, isoxsuprine hydrochloride, ethamsylate, doxycycline hyclate have been developed. Both methods were based on the oxidation of the cited drugs with cerium (IV) in acid medium. The spectrophotometric method was based on measurement of the absorbance difference (ΔA), which represents the excess cerium (IV), at 317 nm for each drug. On the other hand, the spectrofluorimetric method was based on measurement of the fluorescent of the produced cerium (III) at emission wavelength 354 nm (λexcitation = 255 nm) for the concentrations studied for each drug. For both methods, the variables affecting the reactions were carefully investigated and the conditions were optimized. Linear relationships were found between either ΔA or the fluorescent of the produced cerium (III) values and the concentration of the studied drugs in a general concentration range of 2.0-24.0 μg mL- 1, 20.0-24.0 ng mL- 1 with good correlation coefficients in the following range 0.9990-0.9999, 0.9990-0.9993 for spectrophotometric and spectrofluorimetric methods respectively. The limits of detection and quantitation of spectrophotometric method were found in general concentration range 0.190-0.787 and 0.634-2.624 μg mL- 1respectively. For spectrofluorimetric method, the limits of detection and quantitation were found in general concentration range 4.77-9.52 and 15.91-31.74 ng mL- 1 respectively. The stoichiometry of the reaction was determined, and the reactions pathways were postulated. The analytical performance of the methods, in terms of accuracy and precision, were statistically validated and the results obtained were satisfactory. The methods have been successfully applied to the determination of the cited drugs in their commercial pharmaceutical formulations. Statistical comparison of the results with the reference methods

  14. Spectrophotometric and spectrofluorimetric methods for determination of certain biologically active phenolic drugs in their bulk powders and different pharmaceutical formulations. (United States)

    Omar, Mahmoud A; Badr El-Din, Kalid M; Salem, Hesham; Abdelmageed, Osama H


    Two simple and sensitive spectrophotometric and spectrofluorimetric methods for the determination of terbutaline sulfate, fenoterol hydrobromide, etilefrine hydrochloride, isoxsuprine hydrochloride, ethamsylate, doxycycline hyclate have been developed. Both methods were based on the oxidation of the cited drugs with cerium (IV) in acid medium. The spectrophotometric method was based on measurement of the absorbance difference (ΔA), which represents the excess cerium (IV), at 317nm for each drug. On the other hand, the spectrofluorimetric method was based on measurement of the fluorescent of the produced cerium (III) at emission wavelength 354nm (λexcitation=255nm) for the concentrations studied for each drug. For both methods, the variables affecting the reactions were carefully investigated and the conditions were optimized. Linear relationships were found between either ΔA or the fluorescent of the produced cerium (III) values and the concentration of the studied drugs in a general concentration range of 2.0-24.0μgmL-1, 20.0-24.0ngmL-1 with good correlation coefficients in the following range 0.9990-0.9999, 0.9990-0.9993 for spectrophotometric and spectrofluorimetric methods respectively. The limits of detection and quantitation of spectrophotometric method were found in general concentration range 0.190-0.787 and 0.634-2.624μgmL-1respectively. For spectrofluorimetric method, the limits of detection and quantitation were found in general concentration range 4.77-9.52 and 15.91-31.74ngmL-1 respectively. The stoichiometry of the reaction was determined, and the reactions pathways were postulated. The analytical performance of the methods, in terms of accuracy and precision, were statistically validated and the results obtained were satisfactory. The methods have been successfully applied to the determination of the cited drugs in their commercial pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent

  15. Stability indicating RP-HPLC method for simultaneous determination of pantoprazole sodium and itopride hydrochloride in bulk and capsule

    Directory of Open Access Journals (Sweden)

    Krishna R. Gupta


    Full Text Available A stability indicating reversed-phase HPLC method has been developed and subsequently validated for simultaneous estimation of pantoprazole present as pantoprazole sodium sesquihydrate (PSS, and itopride hydrochloride from their combination product. The proposed RP-HPLC method utilizes a Phenomenex® C18, 5 µm, 250 mm X 4.6 mm i.d. column, mobile phase consisting of phosphate buffer and acetonitrile in the proportion of 55:45 (v/v with apparent pH adjusted to 5.0, and UV detection at 289.0 nm using a UV detector. PAN, ITH and their combination drug product were exposed to thermal, photolytic, hydrolytic and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. The described method was linear over a range of 4-20 µg/mL for PAN and 15-75 µg/mL for ITH. The mean recoveries were 100.02 and 99.88 for PAN and ITH, respectively. Chromatographic peak purity data of PAN and ITH indicated no co-eluting peaks with the main peaks of drugs which demonstrated the specificity of assay method for their estimation in presence of degradation products. The proposed method can be useful in the quality control of combination drug products.

  16. Effect of reinforcement surface functionalization on the mechanical properties of nacre-like bulk lamellar composites processed by a hybrid conventional method. (United States)

    Gurbuz, Selen N; Dericioglu, Arcan F


    Alumina platelet reinforced epoxy matrix composites with an architecture resembling to natural nacre were fabricated by a hybrid conventional method called Hot-press Assisted Slip Casting process (HASC). Correlation between processing parameters, platelet content, platelet orientation and mechanical property enhancement of the fabricated composites was examined. In order to investigate the effect of interfacial compatibility and bonding on the mechanical properties of the fabricated inorganic-organic composites, platelet surfaces were modified with both epoxy- and amino-functional silanes. As received and functionalized platelet surfaces were studied by X-Ray Photoelectron Spectroscopy (XPS) to confirm the success of surface modification. Fabricated bio-inspired bulk lamellar composite materials were characterized in terms of their microstructural architecture and mechanical properties. The results obtained indicated that HASC processed composites exhibit enhanced flexural strength, stiffness and hardness, as compared to neat epoxy and composites fabricated by simple mixing, as a result of their nacre-like architecture with well aligned platelets. It has been also observed that functionalization by both type of silanes improves interfacial adhesion between platelets and epoxy matrix resulting in further enhancement of the mechanical properties of bulk lamellar composites fabricated by HASC. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. A Validated New Gradient Stability-Indicating LC Method for the Analysis of Doripenem in Bulk and Injection Formulation

    Directory of Open Access Journals (Sweden)

    Singaram Kathirvel


    Full Text Available A sensitive, precise, specific, linear, and stability-indicating gradient HPLC method was developed for the estimation of doripenem in active pharmaceutical ingredient (API and in injectable preparations. Chromatographic separation was achieved on C18 stationary phase with a mobile phase gradient consisting of acetonitrile, methanol, and pH 5.2 phosphate buffer. The mobile phase flow rate was 0.8 mL/min, and the eluted compounds were monitored at 210 nm. The method is linear over the range of 0.335 to 76.129 µg/mL. The correlation coefficient was found to be 0.999. The numbers of theoretical plates and tailing factor for doripenem were 53021 and 0.9, respectively. Doripenem was subjected to the International Conference on Harmonization (ICH prescribed hydrolytic (acid, base, and neutral, oxidative, photolytic, and thermal stress conditions. Among all the above-mentioned conditions, the drug was found to be stable under photolytic degradation. Peak homogeneity data for doripenem in the chromatograms from the stressed samples obtained by use of the photodiode array detector demonstrated the specificity of the method for analysis of doripenem in presence of the degradation products. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, and robustness.

  18. Selenium Speciation and Management in Wet FGD Systems

    Energy Technology Data Exchange (ETDEWEB)

    Searcy, K; Richardson, M; Blythe, G; Wallschlaeger, D; Chu, P; Dene, C


    rapidly than it sorbs to ferric solids. Though it was not possible to demonstrate a decrease in selenium concentrations to levels below the project'ale testing were evident at the pilot scale. Specifically, reducing oxidation air rate and ORP tends to either retain selenium as selenite in the liquor or shift selenium phase partitioning to the solid phase. Oxidation air flow rate control may be one option for managing selenium behavior in FGD scrubbers. Units that cycle load widely may find it more difficult to impact ORP conditions with oxidation air flow rate control alone. Because decreasing oxidation air rates to the reaction tank showed that all new selenium reported to the solids, the addition of ferric chloride to the pilot scrubber could not show further improvements in selenium behavior. Ferric chloride addition did shift mercury to the slurry solids, specifically to the fine particles. Several competing pathways may govern the reporting of selenium to the slurry solids: co-precipitation with gypsum into the bulk solids and sorption or co-precipitation with iron into the fine particles. Simultaneous measurement of selenium and mercury behavior suggests a holistic management strategy is best to optimize the fate of both of these elements in FGD waters. Work conducted under this project evaluated sample handling and analytical methods for selenium speciation in FGD waters. Three analytical techniques and several preservation methods were employed. Measurements of selenium speciation over time indicated that for accurate selenium speciation, it is best to conduct measurements on unpreserved, filtered samples as soon after sampling as possible. The capital and operating costs for two selenium management strategies were considered: ferric chloride addition and oxidation air flow rate control. For ferric chloride addition, as might be expected the reagent makeup costs dominate the overall costs, and range from 0.22 to 0.29 mills/kWh. For oxidation air flow rate

  19. A pilot study of routine quality control of sampling by the SAD method, applied to packaged and bulk foods. (United States)

    Farrington, Derek; Jervis, Andrew; Shelley, Stephen; Damant, Andrew; Wood, Roger; Thompson, Michael


    A recently proposed method of looking at sampling uncertainty has been tested by its application to the sampling and analysis of several types of food and an animal feedstuff. In this 'SAD' method, increments comprising the conventional sample (that is, collected in the fashion prescribed by the standard sampling protocol) are allocated to either of two equal sized 'splits', which are prepared and analysed separately. The absolute difference between the analytical results for the two splits (the split absolute difference, or SAD) is plotted on a one-sided control chart. A non-compliance indicates that the combined uncertainty of sampling or analysis is larger than expected and the result of the measurement (the mean of the two split results) is possibly not fit for purpose. In addition, the SAD results give rise to a rugged estimate the uncertainty associated with the sampling protocol, often a major part of the total measurement uncertainty.

  20. Bulk heterojunction thin film formation by single and dual feed ultrasonic spray method for application in organic solar cells (United States)

    Marathe, D. M.; Tarkas, H. S.; Mahajan, M. S.; Lonkar, G. S.; Tak, S. R.; Sali, J. V.


    We here present a way of preparing the polymer: fullerene BHJ using dual feed method which can lead to formation of pure phases. In this report, we present results of our initial experiments in this direction. The effect of process parameters on the thickness and surface roughness of the active layer has been discussed. The structural and optical properties have been studied using the optical microscope, UV—visible spectroscopy and photoluminescence spectroscopy. Significant PL quenching indicates efficient charge separation in the BHJ formed using this technique. We have also compared the BHJ thin films prepared with this dual feed ultrasonic technique with the single feed spray method. The BHJ formed using this technique has been used as an active layer in OSC. supported by the University Grants Commission, New Delhi, under Faculty Improvement Programme (No. 33-02/12(WRO) Dt.19.03.2013) and the Special Assistance Programme (530/2/DRS/2010(SAP-I)) Phase-II.

  1. Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

    NARCIS (Netherlands)

    Zielinska, K.


    Solid phase microextraction (SPME) is applied in the speciation analysis of the hydrophobic compound triclosan in an aqueous medium containing sorbing SiO2 nanoparticles (NPs). It is found that these NPs, as well as their complexes with triclosan, partition between the bulk medium and the solid

  2. Development and validation of UV-spectrophotometric methods for the determination of sumatriptan succinate in bulk and pharmaceutical dosage form and its degradation behavior under varied stress conditions

    Directory of Open Access Journals (Sweden)

    Kudige Nagaraj Prashanth


    Full Text Available The aim of the present work is to develop sensitive, simple, accurate, precise and cost effective UV-spectrophotometric methods for the determination of sumatriptan succinate (STS, an anti-migraine drug, in bulk and pharmaceutical dosage form; and also to monitor the degradation behavior of the drug under different ICH prescribed stress conditions. Two methods were developed using different solvents, 0.1 M HCl (method A and acetonitrile (method B. The calibration graphs are linear over the range of 0.2–6.0 μg ml−1 in both the methods with a correlation coefficient (r of 0.9999. The apparent molar absorptivity values are 7.59 × 104 and 7.81 × 104 l mol−1 cm−1, for method A and method B, respectively. The other optical characteristics such as Sandell’s sensitivity, limit of detection (LOD and limit of quantification (LOQ values are also reported. The accuracy and precision of the methods were evaluated based on intra-day and inter-day variations. The accuracy of the methods was further confirmed by standard addition procedure. The degradation behavior of the drug was studied by subjecting STS to an acid and alkaline hydrolysis, oxidative, thermal and UV degradation. This study indicated that STS was degraded in alkaline medium and in oxidative condition. The proposed methods were successfully applied to the determination of STS in tablets and the results obtained are comparable with the official method.

  3. Practical Implication of Chromatographic Method for Estimation of Aceclofenac and Pregabalin in Bulk and Pharmaceutical Dosage Forms

    Directory of Open Access Journals (Sweden)

    Hitendrakumar D. Gelani


    Full Text Available Background. Aceclofenac and Pregabalin in combination significantly reduce pain as compared to individual drug in chronic low back pain. Literature reveals that all the reported spectrophotometric methods either need tedious extraction procedures, do not offer high sensitivity, use nonspecific reagent, or recommend the measurement of absorbance in the near UV region where interference most probably occurs that does not offer suitable linearity range. Result. A selective, sensitive, accurate, and precise, high performance liquid chromatographic method with UV detector analysis of Aceclofenac and Pregabalin was investigated. Good chromatographic separation was achieved using an ODS-BP hypersil C18 column (250 mm × 4.6 mm, i.d., 5 μm and a mobile phase consisting of 0.05 M phosphate buffer (KH2PO4 (pH 6.0 : methanol (60 : 40, v/v at a flow rate 1 mL/min. The ultraviolet detector was set at wavelength 218 nm. Retention time for Aceclofenac and Pregabalin was found to be 3.220 and 5.910 min, respectively. Rectilinear relationship with good regression coefficients 0.999 and 0.999 was found over the concentration ranges of 5–25 μg/mL and 3.75–18.75 μg/mL for ACF and PGB, respectively, with detection limits 0.64 and 0.35 μg/mL and quantitation limits 1.95 and 1.06 μg/mL. Conclusion. The mean percentage recoveries were in the range of 98.45–100.08 and 99.69–100.48 for ACF and PGB, respectively. The developed method was successfully applied to the analysis of the drugs in their commercial tablets.

  4. Bulk growth of ninhydrin single crystals by solvent evaporation method and its characterization for SHG and THG applications (United States)

    Vijayan, N.; Philip, J.; Haranath, D.; Rathi, Brijesh; Bhagavannarayana, G.; Halder, S. K.; Roy, N.; Jayalakshmy, M. S.; Verma, Sunil


    Ninhydrin is a well-known compound generally used in amino acid synthesis and also for detecting the latent fingerprints on porous surfaces. Single crystals can be grown by dissolving the compound in double distilled water at ambient temperature, and can be used as a potential material for second and third harmonic generation applications. The grown specimen was subjected to different characterization techniques in order to find out its suitability for device fabrication. Its lattice dimensions have been confirmed by X-ray powder diffraction and its crystalline quality has been assessed by high resolution X-ray diffraction and X-ray topography methods. The presence of functional groups was identified from HETCOR analysis and confirmed the absence of impurities during crystallization. Its optical properties have been examined by photoluminescence and birefringence analyses. Its thermal parameters such as thermal diffusivity, thermal conductivity and specific capacity have been carried out by following photopyroelectric method. Third order nonlinear optical measurements have been carried out using Z-scan technique and its nonlinear optical absorption coefficient has been determined.

  5. Development and validation of a stability-indicating RP–HPLC method for estimation of atazanavir sulfate in bulk

    Directory of Open Access Journals (Sweden)

    S. Dey


    Full Text Available A stability-indicating reverse phase–high performance liquid chromatography (RP–HPLC method was developed and validated for the determination of atazanavir sulfate in tablet dosage forms using C18 column Phenomenix (250 mm×4.6 mm, 5 μm with a mobile phase consisting of 900 mL of HPLC grade methanol and 100 mL of water of HPLC grade. The pH was adjusted to 3.55 with acetic acid. The mobile phase was sonicated for 10 min and filtered through a 0.45 μm membrane filter at a flow rate of 0.5 mL/min. The detection was carried out at 249 nm and retention time of atazanavir sulfate was found to be 8.323 min. Linearity was observed from 10 to 90 μg/mL (coefficient of determination R2 was 0.999 with equation, y=23.427x+37.732. Atazanavir sulfate was subjected to stress conditions including acidic, alkaline, oxidation, photolysis and thermal degradation, and the results showed that it was more sensitive towards acidic degradation. The method was validated as per ICH guidelines.

  6. Creating bulk nanocrystalline metal.

    Energy Technology Data Exchange (ETDEWEB)

    Fredenburg, D. Anthony (Georgia Institute of Technology, Atlanta, GA); Saldana, Christopher J. (Purdue University, West Lafayette, IN); Gill, David D.; Hall, Aaron Christopher; Roemer, Timothy John (Ktech Corporation, Albuquerque, NM); Vogler, Tracy John; Yang, Pin


    Nanocrystalline and nanostructured materials offer unique microstructure-dependent properties that are superior to coarse-grained materials. These materials have been shown to have very high hardness, strength, and wear resistance. However, most current methods of producing nanostructured materials in weapons-relevant materials create powdered metal that must be consolidated into bulk form to be useful. Conventional consolidation methods are not appropriate due to the need to maintain the nanocrystalline structure. This research investigated new ways of creating nanocrystalline material, new methods of consolidating nanocrystalline material, and an analysis of these different methods of creation and consolidation to evaluate their applicability to mesoscale weapons applications where part features are often under 100 {micro}m wide and the material's microstructure must be very small to give homogeneous properties across the feature.

  7. Development and Validation of a Stability-Indicating RP-HPLC Method for the Assay of Pristinamycin in Bulk and Tablet Dosage Form. (United States)

    Mallikarjuna Rao, Nagasarapu; Gowrisankar, Dannana


    Pristinamycin is an antibiotic used mainly in the treatment of Staphylococcus infections. The aim of this study was to develop a rapid and simple stability-indicating RP-HPLC method for the determination of pristinamycin in tablet dosage form. Pristinamycin was eluted on the ACE-5, C18-HL, 250 x 4.6 mm, 5 µm analytical column with a mobile phase consisting of 0.2% orthophosphoric acid and acetonitrile 63:37 v/v, pumped at 1.5 ml/min flow rate. The column was maintained at 40°C and 10 μl of the solutions were injected. UV detection was performed at 206 nm. The procedure separated pristinamycin and its potential degradation products in an overall analysis time of less than 10 min with pristinamycin eluting at about 3 min. The method was validated according to the regulatory guidelines with respect to specificity, precision, accuracy, linearity, and robustness. Forced degradation studies were also performed for pristinamycin bulk drug samples to demonstrate the stability-indicating power of the HPLC method. The % RSD of system precision and method precision was found to be 0.64 and 1.49%, respectively. The procedure provided a linear response over the concentration range 25-150 μg/ml (r = 0.9998). Finally, the applicability of the method was evaluated in the tablet dosage form as well as in stability samples.

  8. Fast growth of n-type 4H-SiC bulk crystal by gas-source method (United States)

    Hoshino, Norihiro; Kamata, Isaho; Tokuda, Yuichiro; Makino, Emi; Kanda, Takahiro; Sugiyama, Naohiro; Kuno, Hironari; Kojima, Jun; Tsuchida, Hidekazu


    Fast growth of n-type 4H-SiC crystals was attempted using a high-temperature gas-source method. High growth rates exceeding 9 mm/h were archived at a seed temperature of 2550 °C, although the formation of macro-step bunching caused doping fluctuation and voids in the grown crystal. We investigated a trade-off between growth-rate enhancement and macro-step formation and how to improve the trade-off. By controlling the growth conditions, the growth of highly nitrogen-doped 4H-SiC crystals without the doping fluctuation and void formation were accomplished under a high growth rate exceeding 3 mm/h, maintaining the density of threading screw dislocations in the same level with the seed crystal. The influence of growth parameters on nitrogen incorporations into grown crystals was also surveyed.

  9. Multi method (STXM, μFT-IR, μXAFS) approach to identify uranium speciation in argillites from the Lodève Basin (France) (United States)

    Michel, P.; Schäfer, T.; Denecke, M. A.; Brendebach, B.; Dardenne, K.; Huber, F.; Rothe, J.


    Spatially resolved spectroscopic investigations with a nanometer to micrometerscale resolution (μ-XRF, μ-XAFS, STXM and μ-FTIR) focused on the U speciation in two clay-rich samples originating from the Autunian shales (Permian Lodève Basin; France) a natural uranium deposit associated with organic matter (bitumen). The goal of this study was to determine the U oxidation state in the samples and to ascertain if any correlation between the U distribution and that of other selected elements present in the clay (K, Ca, Ti, Fe, Zr and C) exists. Identification of uranium associated with organic matter and/or mineral phases (e.g. iron oxides, clay minerals) can potentially give insight into the mechanism of uranium immobilization in this sedimentary formation. μ-XRF and μ-XAFS measured in confocal geometry show that the U is present as U(IV) and its distribution is not correlated to areas with a high Fe content, but rather correlates with the distribution of lighter elements. U L3 μ-EXAFS recorded at areas with high U concentration reveals that U in these hot spots likely present as a nanocrystalline uraninite (UO2) - like phase. Clay fractions of the samples characterized by XRD are mainly composed of chlorite and illite. STXM carbon K-edge, potassium L-edge and iron L-edge investigations conducted on sulphur-embedded microtomes show two types of organic matter present, one positively correlated with the elements K and Fe and another of pure organic composition building fracture infill. The μ-FTIR measurements clearly reveal a direct association of organic matter with clay minerals. From combined results a tentative hypothesis of U immobilization is put forward.

  10. Development and validation of zero and first-order derivative area under curve spectrophotometric methods for the determination of entacapone in bulk material and in tablets. (United States)

    Chalikwar, S S; Shirkhedkar, A A; Bagul, M A; Jain, P S; Surana, S J


    The aim of this work is to establish two simple, economical, and rapid spectrophotometric methods for the quantification of entacapone in bulk material and in tablets. Further, this study is designed to validate the developed methods as per ICH guidelines. In Methods I and II, a stock standard solution was prepared by dissolving 10 mg of entacapone in 100 mL of 10% v/v acetonitrile to obtain a concentration of 100 μg/mL. After suitable dilution, 10 μg/mL of entacapone was prepared and scanned in the UV-visible range 500-200 nm; entacapone showed a maximum absorbance at 384.40 nm. In Method I, area under curve (AUC) of the zero-order spectrum was recorded between 348.00 and 410.20 nm. While, in Method II, zero-order spectra were derivatized into first-order, and the AUC was recorded between 386.40 and 460.20 nm. For a linearity study, series of dilutions were prepared from stock solutions. In Method I, and II, entacapone followed linearity in the concentration range of 2-12 μg/mL and 5-30 μg/mL with (r(2)>0.999). The amounts of entacapone estimated by both these methods were found to be 99.24 ± 0.054 and 98.68 ± 1.04, respectively. The developed methods are simple, precise, rugged, robust, and economical. Both these methods can be used for routine analysis of entacapone from its tablet formulation.

  11. Speciation analysis of 129I in seawater using coprecipitation and accelerator mass spectrometry and its applications

    DEFF Research Database (Denmark)

    Xing, Shan; Hou, Xiaolin; Aldahan, Ala


    Speciation analysis of long-lived 129I in seawater can provide useful information on the source of water masses. This paper presents an improved method for speciation analysis of 129I based on coprecipitation of iodide as AgI with Ag2SO3 and AgCl. By adding a small amount of 127I carrier, the sep...

  12. Speciation of triphenyltin compounds using Moessbauer spectroscopy. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Eng, G.


    Organotin compounds have been used widely as the active agent in antifouling marine paints. Organotin compounds, i.e., tributyltin compounds (TBTs) and triphenyltin compounds (TPTs) have been found to be effective in preventing the unwanted attachment and development of aquatic organisms such as barnacles, sea grass and hydroids on ships, hulls and underwater surfaces. However, these organotin compounds have been found to be toxic to non-targeted marine species as well. While speciation of tributyltins in environmental water systems has received much attention in the literature, little information concerning the speciation of triphenyltins is found. Therefore, it would be important to study the fate of TPTs in the aquatic environment, particularly in sediments, both oxic and anoxic, in order to obtain speciation data. Since marine estuaries consist of areas with varying salinity and pH, it is important to investigate the speciation of these compounds under varying salinity conditions. In addition, evaluation of the speciation of these compounds as a function of pH would give an insight into how these compounds might interact with sediments in waters where industrial chemical run-offs can affect the pH of the estuarine environment. Finally, since organotins are present in both salt and fresh water environments, the speciation of the organotins in seawater and distilled water should also be studied. Moessbauer spectroscopy would provide a preferred method to study the speciation of triphenyltins as they leach from marine paints into the aquatic environment. Compounds used in this study are those triphenyltin compounds that are commonly incorporated into marine paints such as triphenyltin fluoride (TPTF), triphenyltin acetate (TPTOAc), triphenyltin chloride (TPTCl) and triphenyltin hydroxide (TPTOH).

  13. The ecological genetics of homoploid hybrid speciation

    National Research Council Canada - National Science Library

    Gross, B L; Rieseberg, L H


    ... a major role as well. In light of this recent shift, we present an evaluation of ecology's role in homoploid hybrid speciation, with an emphasis on the genetics underlying ecological components of the speciation process...

  14. Speciation through sensory drive in cichlid fish

    NARCIS (Netherlands)

    Seehausen, Ole; Terai, Yohey; Magalhaes, Isabel S.; Carleton, Karen L.; Mrosso, Hillary D. J.; Miyagi, Ryutaro; van der Sluijs, Inke; Schneider, Maria V.; Maan, Martine E.; Tachida, Hidenori; Imai, Hiroo; Okada, Norihiro


    Theoretically, divergent selection on sensory systems can cause speciation through sensory drive. However, empirical evidence is rare and incomplete. Here we demonstrate sensory drive speciation within island populations of cichlid fish. We identify the ecological and molecular basis of divergent

  15. Estimation of the particle size distribution slope with 3 methods: implications for the optical backscattering ratio and the bulk refractive index (United States)

    Karageorgis, A. P.; Drakopoulos, P. G.; Chaikalis, S.; Spyridakis, N.; Psarra, S.


    Within the framework of Perseus and AegeanMarTech projects, multidisciplinary bio-optics experiments were conducted in the optically complex, permanently stratified waters of the NE Aegean Sea. We were able to obtain the particle size distribution (PSD) slope, using different optical sensors: (a) WET Labs ECO-B3B backscattering sensor measuring VSF at three wavelengths (470, 532, and 650 nm); (b) WET Labs C-Star transmissometer (660 nm) and Chelsea ALPHAtracka MKII (470 nm); and (c) Laser In Situ Scattering and Transmissometry - LISST-Deep. Values of the PSD slope estimated by all three methods were found to be within the ranges predicted by Mie theory and the literature. The optical backscattering ratio, bbp, was calculated from bbp(660) and cp(660) and subsequently the bulk index of refraction (np) was estimated as a function of the backscattering ratio and the PSD slope. In July 2014, the values of np varied between 1.01 and >1.24 (mean 1.12+/-0.08), which fall between phytoplankton- and mineral-dominated waters. According to the spatial distribution of np two water layers could be identified, associated with different particle composition: (a) Black Sea water (BSW) and Levantine waters (LW) (from the surface to 65 m depth) that appear to be dominated by material with mean index of refraction 1.13; and (b) the near-bottom layer which exhibited high np, >1.24, the latter attributed to mineral particles with high bulk index of refraction resuspended from the sea floor.

  16. Theoretical analysis and numerical calculation of 3D trapped field distribution of single domain SmBCO bulks by Sm+011 TSIG methods (United States)

    Yang, Wanmin; Yang, Pengtao; Wang, Yanan; Li, Qiang


    The lower critical temperature Tc and critical current density Jc are serious weaknesses of SmBCO bulk superconductors fabricated in air for practical applications, because of the Sm3+/Ba2+ solid solution in Sm1+xBa2-xCu3Oy crystals. In this paper, high quality single domain SmBCO bulk samples S1 (ϕ20 mm) and S2 (ϕ32 mm) have been fabricated in air by a new Sm+011 TSIG method. The trapped field of the samples is 0.8 T and 1.15 T at liquid nitrogen temperature for the samples S1 and S2 respectively, which is the strongest trapped field of the SmBCO samples fabricated in air today. The theoretical formula for 3D trapped field distribution have been derived for a cylindrical model with uniformly distributed critical current density Jc based on the Biot Savart law; the cylindrical sample is divided into a series of concentric rings with the same width and thickness, the trapped field of the samples is the summation of magnetic field produced by all the rings, while the magnetic field generated by each ring was worked out by trapezoidal numerical integration based on the Biot Savart law with the critical current density Jc of the samples. It is found that the calculated field of the samples is well in agreement with the experimental results if the reasonable Jc of the samples is adopted. The theoretical calculation result also indicates that the larger the diameter and the thickness of the samples, the stronger the trapped flux density, but the optimal diameter/thickness ratio should be of a reasonable value around one, and it is not so good to fabricated samples with too larger diameter or thickness for practical applications.

  17. A method for the parameterization of cloud optical properties in bulk and bin microphysical models. Implications for arctic cloudy boundary layers (United States)

    Harrington, Jerry Y.; Olsson, Peter Q.

    Computationally efficient and numerically accurate methods for computing band-averaged cloud optical properties for radiative transfer interactions with various microphysical parameterizations are described. Parameterizations for bulk microphysical models employing generalized gamma distribution representations of the size spectra and binned representations, in which the size spectra fluctuate with time, are discussed. It is shown that simple exponential fits and look-up tables may be used with minimal computational cost and high accuracy for bulk microphysical models. Binned microphysical representations may be parameterized using mean properties for each bin, if averaged appropriately. The implications for the radiative scheme are discussed in comparison with the computed radiative budget of fall/spring season mixed-phase Arctic stratus clouds (ASC). Compared to liquid clouds of the same water path, mixed-phase ASC absorb and reflect less radiation, and transmit more radiation to the surface. This results in greater cooling (warming) of the surface, by up to 60 W m -2, in the infrared (solar) by mixed-phase clouds. The radiative properties of mixed-phase clouds show a significant sensitivity to crystal habit for clouds with ice water paths ≳25 g m -2. Surface net fluxes and cloud absorption may vary by up to 15 W m -2, depending on the ice habit. It is also shown that mixed-phase clouds are more sensitive to the choice of ice effective radius ( re,i) than liquid clouds are to re. Using values of from the literature, it is shown that the surface net fluxes can vary by as much as 50 W m -2 depending on the value of re,i. Furthermore, it is shown that the sign of the surface net flux (i.e. warming or cooling) may be dependent on the value of re,i selected.

  18. High-Performance Liquid Chromatographic and High-Performance Thin-Layer Chromatographic Method for the Quantitative Estimation of Dolutegravir Sodium in Bulk Drug and Pharmaceutical Dosage Form. (United States)

    Bhavar, Girija B; Pekamwar, Sanjay S; Aher, Kiran B; Thorat, Ravindra S; Chaudhari, Sanjay R


    Simple, sensitive, precise, and specific high-performance liquid chromategraphic (HPLC) and high-performance thin-layer chromatographic (HPTLC) methods for the determination of dolutegravir sodium in bulk drug and pharmaceutical dosage form were developed and validated. In the HPLC method, analysis of the drug was carried out on the ODS C18 column (150 × 4.6 mm, 5 μm particle size) using a mixture of acetonitrile: water (pH 7.5) in the ratio of 80:20 v/v as the mobile phase at the flow rate 1 mL/min at 260 nm. This method was found to be linear in the concentration range of 5-35 μg/mL. The peak for dolutegravir sodium was observed at 3.0 ± 0.1 minutes. In the HPTLC method, analysis was performed on aluminum-backed plates pre-coated with silica gel G60 F254 using methanol: chloroform: formic acid in the proportion of 8:2:0.5 v/v/v as the mobile phase. This solvent system was found to give compact spots for dolutegravir sodium with the Rf value 0.77 ± 0.01. Densitometric analysis of dolutegravir sodium was carried out in the absorbance mode at 265 nm. Linear regression analysis showed good linearity with respect to peak area in the concentration range of 200-900 ng/spot. The methods were validated for precision, limit of detection (LOD), limit of quantitation (LOQ), accuracy, and specificity. Statistical analysis showed that both of the methods are repeatable and specific for the estimation of the said drug. The methods can be used for routine quality control analysis of dolutegravir sodium.

  19. Extensive range overlap between heliconiine sister species: evidence for sympatric speciation in butterflies? (United States)

    Rosser, Neil; Kozak, Krzysztof M; Phillimore, Albert B; Mallet, James


    Sympatric speciation is today generally viewed as plausible, and some well-supported examples exist, but its relative contribution to biodiversity remains to be established. We here quantify geographic overlap of sister species of heliconiine butterflies, and use age-range correlations and spatial simulations of the geography of speciation to infer the frequency of sympatric speciation. We also test whether shifts in mimetic wing colour pattern, host plant use and climate niche play a role in speciation, and whether such shifts are associated with sympatry. Approximately a third of all heliconiine sister species pairs exhibit near complete range overlap, and analyses of the observed patterns of range overlap suggest that sympatric speciation contributes 32%-95% of speciation events. Müllerian mimicry colour patterns and host plant choice are highly labile traits that seem to be associated with speciation, but we find no association between shifts in these traits and range overlap. In contrast, climatic niches of sister species are more conserved. Unlike birds and mammals, sister species of heliconiines are often sympatric and our inferences using the most recent comparative methods suggest that sympatric speciation is common. However, if sister species spread rapidly into sympatry (e.g. due to their similar climatic niches), then assumptions underlying our methods would be violated. Furthermore, although we find some evidence for the role of ecology in speciation, ecological shifts did not show the associations with range overlap expected under sympatric speciation. We delimit species of heliconiines in three different ways, based on "strict and " "relaxed" biological species concepts (BSC), as well as on a surrogate for the widely-used "diagnostic" version of the phylogenetic species concept (PSC). We show that one reason why more sympatric speciation is inferred in heliconiines than in birds may be due to a different culture of species delimitation in the two

  20. Stability indicating method development and validation for simultaneous estimation of atorvastatin calcium and celecoxib in bulk and niosomal formulation by RP-HPLC

    Directory of Open Access Journals (Sweden)

    Priyanka S. Jadhav


    Full Text Available The present work describes development and validation of a specific, sensitive, precise and stability-indicating high-performance liquid chromatographic method of analysis of atorvastatin calcium and celecoxib, both as a bulk drug and in niosomal formulation. The analysis has been performed by using Cosmosil-C18 column (4.6 mm´250 mm, 5 m at 25 °C using acetonitrile: ammonium acetate buffer pH 5.0: methanol (50:25:25 v/v/v as mobile phase. The detection was carried out at 277nm with a flow rate of 1.0mL/min. The retention times of Atorvastatin calcium and Celecoxib were 6.195 and 3.989min, respectively. The method was validated according to ICH guidelines, for specificity, precision, linearity, accuracy and robustness. Atorvastatin calcium and Celecoxib were subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The degradation was observed in oxidation and acid hydrolysis. The linearity for atorvastatin calcium and celecoxib were in the range of 100-500 µg/mL. The recovery study of atorvastatin and celecoxib were found to be in the range of 98.96 - 99.92% and 98.90-100%, respectively. The proposed method was validated and successfully applied to the estimation of Atorvastatin calcium and Celecoxib in combined in-house niosomal formulation.

  1. 19 CFR 149.4 - Bulk and break bulk cargo. (United States)


    ... 19 Customs Duties 2 2010-04-01 2010-04-01 false Bulk and break bulk cargo. 149.4 Section 149.4... TREASURY (CONTINUED) IMPORTER SECURITY FILING § 149.4 Bulk and break bulk cargo. (a) Bulk cargo exempted.... (b) Break bulk cargo exempted from time requirement. For break bulk cargo that is exempt from the...

  2. Mineralogy and metals speciation in Mo rich mineral sludges generated at a metal recycling plant. (United States)

    Vemic, M; Bordas, F; Guibaud, G; Joussein, E; Labanowski, J; Lens, P N L; van Hullebusch, E D


    In France, more than 250 million metric tons of sludges need to be treated each year. These sludges are either dumped on the landfills or reused as secondary resources in order to preserve natural resources. A large portions of these sludges are mineral sludges, originating from metal recycling plants. In order to estimate their metal recovery potential, these mineral sludges were characterized. Four types of mineral sludge samples were collected from a metal recycling plant (3 from the recycling plant storage areas (bulk storage, barrel storage and storage shed) and 1 from the collection basin). The sludges were characterized, wherein the Mo, Ni, Cr, Co, Zn and W content and speciation were quantified. The samples had pH values between 5.9 and 10.3 with organic matter contents varying between 6.3% (storage shed) and 29.5% (bulk storage) (loss on ignition at 500 °C). Based on their leaching properties, the four mineral sludge samples (in the case of Mo) and the bulk storage sludge (in the case of Ni and Zn) were classified as potentially hazardous regarding the EN 12457-1 and EN 12457-2 method. Mineralogical results reveal that both bulk storage and the storage shed give the highest contributions to the metal content of the collection basin sample. Sequential extraction of the collection basin samples indicated that Mo is bound to the oxidizable and residual fraction, while Ni, Cr and Co were bound to the residual fraction, and Zn to the soluble acid fraction, respectively. W tends to be equally distributed among all extracted fractions. A strong correlation existed between Mo and Co, as well as between Ni, Zn and Cr, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Bulk derivatization and cation exchange restricted access media-based trap-and-elute liquid chromatography–mass spectrometry method for determination of trace estrogens in serum

    Energy Technology Data Exchange (ETDEWEB)

    Beinhauer, Jana [Department of Biochemistry, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Centre of the Region Haná for Biotechnological and Agricultural Research - Department of Protein Biochemistry and Proteomics, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Bian, Liangqiao [Shimadzu Center for Advanced Analytical Chemistry, The University of Texas at Arlington, Arlington, TX (United States); Shimadzu Institute for Research Technologies, The University of Texas at Arlington, Arlington, TX (United States); Fan, Hui [Department of Chemistry and Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); Šebela, Marek [Department of Biochemistry, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Centre of the Region Haná for Biotechnological and Agricultural Research - Department of Protein Biochemistry and Proteomics, Faculty of Science, Palacký University, Šlechtitelů 11, CZ-783 71 Olomouc (Czech Republic); Kukula, Maciej [Shimadzu Center for Advanced Analytical Chemistry, The University of Texas at Arlington, Arlington, TX (United States); Shimadzu Institute for Research Technologies, The University of Texas at Arlington, Arlington, TX (United States); Barrera, Jose A. [Shimadzu Institute for Research Technologies, The University of Texas at Arlington, Arlington, TX (United States); and others


    Highlights: • Analysis of estrogens in small volume samples at low parts-per-trillion concentration. • Charged bulk derivatization facilitates on-line ion exchange sample preparation. • On-line WCX restricted access media traps analytes, but not proteins and lipids. • Complete preparation and LC–MS/MS analysis completed in 30 min/sample. - Abstract: Estrone (E1), estradiols (α/β-E2), and estriol (E3) are four major metabolically active estrogens exerting strong biological activities at very low circulating concentrations. This paper reports a sensitive and efficient method with automated, on-line clean-up and detection to determine trace estrogens in a small volume of serum samples using liquid chromatography–electrospray ionization–tandem mass spectrometry directly, without off-line liquid–liquid or solid-phase extraction pretreatments. Serum aliquots (charcoal stripped fetal bovine serum, 100 μL) were spiked with four estrogen standards and their corresponding isotope-labeled internal standards, then bulk derivatized with 2-fluoro-1-methyl-pyridium p-toluenesulfonate (2-FMP) to establish the calibration curves and perform method validation. Calibration was established in the concentration ranges of 5–1000 pg mL{sup −1}, and demonstrated good linearity of R{sup 2} from 0.9944 to 0.9997 for the four derivatized estrogens. The lower detection limits obtained were 3–7 pg mL{sup −1}. Good accuracy and precision in the range of 86–112% and 2.3–11.9%, respectively, were observed for the quality control (QC) samples at low, medium, and high concentration levels. The stability tests showed that the derivatized serum samples were stable 8 h after derivatization at room temperature and at least to 48 h if stored at −20 °C. The method was applied to measure trace estrogens in real human and bovine serum samples, and three of four estrogen compounds studied were observed and quantified.

  4. An experimental design approach for optimization of spectrophotometric method for estimation of cefixime trihydrate using ninhydrin as derivatizing reagent in bulk and pharmaceutical formulation

    Directory of Open Access Journals (Sweden)

    Yogita B. Wani


    Full Text Available The aim of the present work is to use experimental design to screen and optimize experimental variables for developing a spectrophotometric method for determining cefixime trihydrate content using ninhydrin as a derivatizing reagent. The method is based on the reaction of the amino group of cefixime with ninhydrin in an alkaline medium to form a yellow-colored derivative (λmax 436 nm. A two-level full factorial design was utilized to screen the effect of ninhydrin reagent concentration (X1, volume of ninhydrin reagent (X2, heating temperature (X3 and heating time (X4 on the formation of the cefixime–ninhydrin complex Y (absorbance. One way ANOVA and Pareto ranking analyses have shown that the ninhydrin reagent concentration (X1, volume of ninhydrin reagent (X2 and heating temperature (X3 were statistically significant factors (P < 0.05 affecting the formation of the cefixime–ninhydrin complex Y (absorbance. A Box-Behnken experimental design with response surface methodology was then utilized to evaluate the main, interaction and quadratic effects of these three factors on the selected response. With the help of a response surface plot and contour plot the optimum values of the selected factors were determined and used for further experiments. These values were a ninhydrin reagent concentration (X1 of 0.2% w/v, volume of ninhydrin reagent (X2 of 1 mL and heating temperature (X3 of 80 °C. The proposed method was validated according to the ICH Q2 (R1 method validation guidelines. The results of the present study have clearly shown that an experimental design concept may be effectively applied to the optimization of a spectrophotometric method for estimating the cefixime trihydrate content in bulk and pharmaceutical formulation with the least number of experimental runs possible.

  5. Validated stability-indicating high performance thin layer chromatographic method for determination of Ivabradine hydrochloride in bulk and marketed formulation: An application to kinetic study

    Directory of Open Access Journals (Sweden)

    Mitesh H. Motisariya


    Full Text Available A sensitive, selective, precise and accurate stability-indicating high-performance thin layer chromatographic method for analysis of Ivabradine hydrochloride (IH an anti anginal agent, both as a bulk drug and in formulations was developed and validated according to ICH guideline. Densitometric analysis of IH was carried out in the absorbance mode at 287 nm using ethyl acetate: 0.389 M ammonium acetate in methanol (1:5, v/v as solvent system. This system was found to give compact spots for IH at an Rf value of 0.36 ± 0.01. Moreover, IH was subjected to acid and alkali hydrolysis, oxidation, accelerated humidity/temperature, wet heat treatment, and photo degradation. The drug undergoes degradation under mainly acidic and basic conditions. Also the degraded products were well resolved from the pure drug with significantly different Rf values. Linearity was found to be in the range of 1200–2800 ng/band. The LOD and LOQ for IH were 255.86 ng/band and 775.33 ng/band, respectively. “Bartlett’s test” and “Lack of fit” applied on peak area for linearity, additionally proved validity of the developed method. Good accuracy and precision were obtained as revealed from %RSD value less than 2. Similarly, no interference was observed from common excipients in tablet formulation as well as degradation product, indicating specificity of the method. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one. Moreover, proposed method was also utilized to investigate the kinetics of acidic degradation process at different temperatures and first order rate constant, half-life, shelf-life and activation energy were calculated.

  6. Application of a Validated Stability-Indicating LC Method for the Simultaneous Estimation of Tapentadol and Its Process-Related Impurities in Bulk and Its Dosage Form

    Directory of Open Access Journals (Sweden)

    Singaram Kathirvel


    Full Text Available Described is a first reported, simple, rapid, selective, and isocratic stability-indicating RP-LC method for the quantitative determination of tapentadol and its related substances in bulk samples and pharmaceutical dosage forms in the presence of its two process-related impurities. Chromatographic separation was achieved on the reversed phase, Enable column (C18 (5-μm, 250 × 4.6 mm, i.d. at ambient temperature using a mobile phase consisting of 0.02 M potassium dihydrogen orthophosphate (adjusted to pH 6 with 1 M KOH and acetonitrile (80 : 20, v/v. Flow rate was 1 mL/min and retention time was found to be 7.7 ± 0.05 min. Quantitation was achieved with UV detection at 215 nm based on peak area with linear calibration curves at concentration range 75–300 μg/mL. Forced degradation studies were performed, in accordance with ICH guidelines, using acidic, alkaline, oxidative, neutral, photolytic, and thermal conditions. The drug was found to be stable under all the conditions. The developed method was validated in terms of precision, robustness, recovery, and limits of detection and quantitation. Regression analysis shows an “r” value (correlation coefficient of greater than 0.999 for tapentadol and two potential impurities.

  7. Comparative analysis of bacterial community composition in bulk tank raw milk by culture-dependent and culture-independent methods using the viability dye propidium monoazide. (United States)

    Weber, Mareike; Geißert, Janina; Kruse, Myriam; Lipski, André


    Microbial diversity of 3 raw milk samples after 72 h of storage at 4 °C in a bulk tank was analyzed by culture-dependent and -independent methods. The culture-dependent approach was based on the isolation of bacteria on complex and selective media, chemotaxonomic differentiation of isolates, and subsequent identification by 16S rRNA gene sequencing. The culture-independent approach included the treatment of raw milk with the dye propidium monoazide before direct DNA extraction by mechanic and enzymatic cell lysis approaches, and cloning and sequencing of the 16S rRNA genes. The selective detection of viable bacteria improved the comparability between bacterial compositions of raw milk based on culture-dependent and -independent methods, which was the major objective of this study. Several bacterial species of the phyla Actinobacteria, Bacteroidetes, Firmicutes, and Proteobacteria were detected by the culture-dependent method, whereas mainly bacteria of the phylum Proteobacteria as well as low proportions of the phyla Bacteroidetes and Actinobacteria were detected by the culture-independent method. This led to the conclusion that the phylum Firmicutes was strongly discriminated by the culture-independent approach. Generally, species richness detected by the culture-dependent method was higher than that detected by the culture-independent method for all samples. However, few taxa could be detected solely by the direct DNA-based method. In conclusion, the combination of culture-dependent and -independent methods led to the detection of the highest bacterial diversity for the raw milk samples analyzed. It was shown that DNA extraction from raw milk as the essential step in culture-independent methods causes the discrimination of taxa by incomplete cell lysis. Treatment of raw milk with the viability dye propidium monoazide was optimized for the application in raw milk without former removal of milk ingredients and proved to be a suitable tool to ensure comparability

  8. Plutonium Speciation in Support of Oxidative-Leaching Demonstration Test

    Energy Technology Data Exchange (ETDEWEB)

    Sinkov, Sergey I.


    Bechtel National, Inc. (BNI) is evaluating the plutonium speciation in caustic solutions that reasonably represent the process streams from the oxidative-leaching demonstration test. Battelle—Pacific Northwest Division (PNWD) was contracted to develop a spectrophotometric method to measure plutonium speciation at submicromolar (< 10-6 M) concentrations in alkaline solutions in the presence of chromate and carbonate. Data obtained from the testing will be used to identify the oxidation state of Pu(IV), Pu(V), and Pu(VI) species, which potentially could exist in caustic leachates. Work was initially conducted under contract number 24590-101-TSA-W000-00004 satisfying the needs defined in Appendix C of the Research and Technology Plan TSS A-219 to evaluate the speciation of chromium, plutonium, and manganese before and after oxidative leaching. In February 2007, the contract mechanism was switched to Pacific Northwest National Laboratory (PNNL) Operating Contract MOA: 24590-QL-HC9-WA49-00001.

  9. Sensory drive in cichlid speciation

    NARCIS (Netherlands)

    Maan, Martine E.; Hofker, Kees D.; van Alphen, Jacques J. M.; Seehausen, Ole

    The role of selection in speciation is a central yet poorly understood problem in evolutionary biology. The rapid radiations of extremely colorful cichlid fish in African lakes have fueled the hypothesis that sexual selection can drive species divergence without geographical isolation. Here we

  10. Development and Validation of a Stability-Indicating RP-UPLC Method for Determination of Cloxacillin Sodium in Its Bulk Form and Formulation. (United States)

    Patel, Nikita; Contractor, Pooja; Keshrala, Rajesh; Patel, Parag R; Shridhar, Bhimagoni


    A simple, linear gradient, rapid, precise and stability-indicating RP-UPLC method was developed for the determination of Cloxacillin Sodium in its bulk form and formulation. Ultra performance liquid chromatography, a most promising advancement in a world of chromatography, reduces analysis time, increases reliability through higher resolution, sensitivity and selectivity as well as used as an economic method due to reducing solvent consumption. A chromatographic separation of a drug as well as its degradants was achieved using Waters acquity BEH, 2.1 × 100 mm, 1.7 μm C18 column with gradient of mobile phase A: phosphate buffer, pH 6.8 and mobile phase B: methanol:acetonitrile (75:25). The drug and degradants were monitored at a detection wavelength of 225 nm with a flow rate of 0.35 mL/min and an injection volume of 10 µL. The temperature of the column and auto sampler compartments was at 30°C and 25°C ± 1°C, respectively. The retention time of the drug was ∼6.9 min. The resolution of the drug and degradant peak was >1.5 in all cases. Force degradation of CLOX SOD was carried under alkaline, acidic, oxidative, thermal, photo degradation conditions and it was analyzed by the proposed method. The drug degrades under alkaline, acidic and oxidative conditions but was stable in temperature and light. A developed method was validated as per ICH guidelines using validation parameters such as precision, linearity and range, limit of quantification, specificity, assay and robustness. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email:

  11. Speciation and migration of 129I in soil profiles

    DEFF Research Database (Denmark)

    Luo, Maoyi; Hou, Xiaolin; Zhou, Weijian


    A method has been developed for speciation analysis of ultra low level 129I in soil using sequential extraction combined with coprecipitation for separation of carrier free iodine and AMS measurement of 129I. Two loess profiles collected from northwest China were analyzed for species of 129I...

  12. Fractionation, characterization and speciation of heavy metals in ...

    African Journals Online (AJOL)

    Speciation of heavy metals in soils determines the availability for metals for plant uptake and potential for contamination of groundwater following application of composts to agricultural lands. Methods used to characterize heavy metals in solid phase of composts and compost amended soils include physical fractionation ...


    Chassis dynamometer emissions testing was conducted to characterize speciated volatile organic compounds (VOCs), including mobile source air toxics (MSATs) and ozone precursors, in exhaust emissions from three modern gasoline direct injection (GDI) light-duty vehicles. Each GDI vehicle tested in this study utilized slightly different fuel injection technology: Vehicle 1 used a 2.4 liter, naturally aspirated, wall-guided GDI; Vehicle 2 used a 1.8 liter, turbocharged GDI engine; Vehicle 3 used a 1.5 liter, turbocharged, spray-guided GDI engine. Vehicle testing was conducted in a temperature controlled chassis dynamometer test cell at 22 °C over the EPA Federal Test Procedure (FTP) and a portion of the Supplemental FTP (SFTP). The FTP was conducted as a three phase cycle with a cold start, hot transient, and warm start phase (also known as the FTP-75 driving cycle). The SFTP consisted of the US06 driving cycle (conducted without the vehicle’s air conditioning on), which provides a more aggressive driving pattern than the FTP. The vehicles operated on 10 percent ethanol blended gasoline (E10). VOC emissions from diluted vehicle exhaust were sampled over each FTP phase and over the Supplemental FTP with SUMMA canisters for EPA Method TO-15 analysis and with DNPH cartridges for carbonyl analysis by EPA Method TO-11A. This presentation will report the impact of driving cycle and GDI technology on speciated MSAT emissions. MSAT emission rates will be compared

  14. Radiopacity of bulk fill flowable resin composite materials | Yildirim ...

    African Journals Online (AJOL)

    Objectives: The purpose of this study was to evaluate the radiopacity of currently marketed bulk fill flowable dental composite materials (Beautifil Bulk Flowable, SDR Flow, Filtek Bulk Fill Flow, and x‑tra Base Bulk Fill). Materials and Methods: Six specimens of each material with a thickness of 1 mm were prepared, and ...


    Energy Technology Data Exchange (ETDEWEB)



    The speciation of Cr(VI) in Cromite Ore Processing Residue was investigated by means of bulk XRD, and a combination of micro-XRF, -XAS and -XRD at the Advanced Light Source (ALS), Berkeley, CA, U.S.A.. Bulk XRD yielded one group of phases that contained explicitly Cr(VI) in their structure, Calcium Aluminum Chromium Oxide Hydrates, accounting for 60% of the total Cr(VI). Micro-analyses at ALS yielded complimentary information, confirming that hydrogarnets and hydrotalcites, two mineral groups that can host Cr(VI) in their structure by substitution, were indeed Cr(VI) sinks. Chromatite (CaCrO4) was also identified by micro-XRD, which was not possible with bulk methods due to its low content. The acquisition of micro-XRF elemental maps enabled not only the identification of Cr(VI)-binding phases, but also the understanding of their location within the matrix. This information is invaluable when designing Cr(VI) treatment, to optimize release and availability for reduction.


    Energy Technology Data Exchange (ETDEWEB)

    Kevin C. Galbreath; Charlene R. Crocker; Carolyn M. Nyberg; Frank E. Huggins; Gerald P. Huffman


    A four-step sequential Ni extraction method, summarized in Table AB-1, was evaluated for identifying and quantifying the Ni species occurring in urban total suspended particulate (TSP) matter and fine particulate matter (<10 {micro}m [PM{sub 10}] and <2.5 {micro}m [PM{sub 2.5}] in aerodynamic diameter). The extraction method was originally developed for quantifying soluble, sulfidic, elemental, and oxidic forms of Ni that may occur in industrial atmospheres. X-ray diffraction (XRD) and x-ray absorption fine structure (XAFS) spectroscopy were used to evaluate the Ni species selectivity of the extraction method. Uncertainties in the chemical speciation of Ni in urban PM{sub 10} and PM{sub 2.5} greatly affect inhalation health risk estimates, primarily because of the large variability in acute, chronic, and cancer-causing effects for different Ni compounds.

  17. Development of anion-exchange/reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry methods for the speciation of bio-available iodine and bromine from edible seaweed. (United States)

    Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio


    Anion exchange high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry has been novelly applied to assess inorganic (iodide and iodate) and organic (3-iodotyrosine - MIT, and 3,5-diiodotyrosine - DIT) iodine species in a single chromatographic run. The optimized operating conditions (Dionex IonPac AS7, gradient elution with 175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase and flow rates within the 0.5-1.5 mL min(-1) range) have also been used to perform inorganic bromine speciation analysis (bromide and bromate). The developed method has been applied for determining the bio-available contents of iodine and bromine species in dialyzates from edible seaweed. Reverse phase high performance liquid chromatography (Zorbax Eclipse XDB-C8, gradient elution with 0.2% (m/m) acetic acid, and 0.2% (m/m) acetic acid in methanol, as mobile phases, and a constant flow rate of 0.75 mL min(-1)) also hyphenated with inductively coupled plasma-mass spectrometry was used to confirm the presence of organic iodine species (MIT and DIT) in the dialyzates. The verification of the presence of iodinated amino acids (MIT and DIT) in the extracts was also performed by reverse phase high performance liquid chromatography-electrospray ionization-mass spectrometry (LTQ Orbitrap). The developed methods have provided good repeatability (RSD values lower than 10% for both anion exchange and reverse phase separations) and analytical recoveries within the 90-105% range for all cases. The in vitro bio-availability method consisted of a simulated gastric and an intestinal digestion/dialysis (10 kDa molecular weight cut-off - MWCO) two-stage procedure. Iodide and MIT were the main bio-available species quantified, whereas bromide was the major bromine species found in the extracts. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. Meiosis and speciation: a study in a speciating Mus terricolor complex

    Indian Academy of Sciences (India)



    –679. Museum of Comparative Zoology,. Cambridge. King M. 1981 Chromosome change and speciation in lizards. In Evolution and speciation (ed. W. R. Atchley and D. S.. Woodruff), pp. 262–285. Cambridge University Press ...

  19. Determination of chemical oxygen demand by a flow injection method based on microwave digestion and chromium speciation coupled to inductively coupled plasma optical emission spectrometry. (United States)

    Almeida, César A; González, Patricia; Mallea, Miguel; Martinez, Luis D; Gil, Raúl A


    The present paper evaluates the applicability of a new FIA system for COD determination. The new system, flow injection microwave solid phase extraction by means of activated carbon (FI-MW-SPE), consists of a digestion circuit, placed in a home MW oven, coupled to an ICP-OES spectrophotometer. Doehlert experimental design was used to speed up the optimization of different experimental variables studied for assisted digestion methods. The method provided a high throughput of about 18 samples h(-1). To assess the accuracy of analytical methods linear regression, elliptic joint confidence region (EJCR) was used. A large linear range of 2.78-850 mg O(2) L(-1) with an excellent detection limit of 0.94 mg O(2) L(-1) was obtained. The interference by high chloride concentration was studied, and values below 3000 mg Cl(-) ions L(-1), allowed the estimation of COD load without any masking agents. COD values for various types of wastewater samples were correlated with those obtained by standard manual methods. Moreover, interferences due to matrix nature are absent; since matrix is washed out of the column before Cr (III) is eluted. This method reduces the time, reagent volume, hazardous emission, external contamination, with a good reproducibility and accuracy. Copyright © 2012. Published by Elsevier B.V.

  20. Speciation of Pb in industrially polluted soils

    DEFF Research Database (Denmark)

    Jensen, Pernille Erland; Ottosen, Lisbeth M.; Pedersen, Anne Juul


    This study was aimed at elucidating the importance of original Pb-speciation versus soil-characteristics to mobility and distribution of Pb in industrially polluted soils. Ten industrially polluted Danish surface soils were characterized and Pb speciation was evaluated through SEM-EDX studies......, examination of pH-dependent desorption, distribution in grain-size fractions and sequential extraction. Our results show that the first factors determining the speciation of Pb in soil are: (1) the stability of the original speciation and (2) the contamination level, while soil characteristics...

  1. Reconstructing the History of Selection during Homoploid Hybrid Speciation (United States)

    Karrenberg, Sophie; Lexer, Christian; Rieseberg, Loren H.


    This study aims to identify selection pressures during the historical process of homoploid hybrid speciation in three Helianthus (sunflower) hybrid species. If selection against intrinsic genetic incompatibilities (fertility selection) or for important morphological/ecological traits (phenotypic selection) were important in hybrid speciation, we would expect this selection to have influenced the parentage of molecular markers or chromosomal segments in the hybrid species’ genomes. To infer past selection, we compared the parentage of molecular markers in high-density maps of the three hybrid species with predicted marker parentage from an analysis of fertility selection in artificial hybrids and from the directions of quantitative trait loci effects with respect to the phenotypes of the hybrid species. Multiple logistic regression models were consistent with both fertility and phenotypic selection in all three species. To further investigate traits under selection, we used a permutation test to determine whether marker parentage predicted from groups of functionally related traits differed from neutral expectations. Our results suggest that trait groups associated with ecological divergence were under selection during hybrid speciation. This study presents a new method to test for selection and supports earlier claims that fertility selection and phenotypic selection on ecologically relevant traits have operated simultaneously during sunflower hybrid speciation. PMID:17479459

  2. Microfabricated Bulk Piezoelectric Transformers (United States)

    Barham, Oliver M.

    Piezoelectric voltage transformers (PTs) can be used to transform an input voltage into a different, required output voltage needed in electronic and electro- mechanical systems, among other varied uses. On the macro scale, they have been commercialized in electronics powering consumer laptop liquid crystal displays, and compete with an older, more prevalent technology, inductive electromagnetic volt- age transformers (EMTs). The present work investigates PTs on smaller size scales that are currently in the academic research sphere, with an eye towards applications including micro-robotics and other small-scale electronic and electromechanical sys- tems. PTs and EMTs are compared on the basis of power and energy density, with PTs trending towards higher values of power and energy density, comparatively, indicating their suitability for small-scale systems. Among PT topologies, bulk disc-type PTs, operating in their fundamental radial extension mode, and free-free beam PTs, operating in their fundamental length extensional mode, are good can- didates for microfabrication and are considered here. Analytical modeling based on the Extended Hamilton Method is used to predict device performance and integrate mechanical tethering as a boundary condition. This model differs from previous PT models in that the electric enthalpy is used to derive constituent equations of motion with Hamilton's Method, and therefore this approach is also more generally applica- ble to other piezoelectric systems outside of the present work. Prototype devices are microfabricated using a two mask process consisting of traditional photolithography combined with micropowder blasting, and are tested with various output electri- cal loads. 4mm diameter tethered disc PTs on the order of .002cm. 3 , two orders smaller than the bulk PT literature, had the followingperformance: a prototype with electrode area ratio (input area / output area) = 1 had peak gain of 2.3 (+/- 0.1), efficiency of 33 (+/- 0

  3. Ion-pair chromatography coupled to inductively coupled plasma-mass spectrometry (IPC-ICP-MS) as a method for thiomolybdate speciation in natural waters. (United States)

    Lohmayer, Regina; Reithmaier, Gloria Maria Susanne; Bura-Nakić, Elvira; Planer-Friedrich, Britta


    Molybdenum precipitates preferentially under reducing conditions; therefore, its occurrence in sediment records is used as an indicator of paleoredox conditions. Although thiomolybdates (MoO4-xSx(2-) with x = 1-4) supposedly are necessary intermediates in the process of molybdenum precipitation under anoxic conditions, there is no information about their abundance in natural environments, because of a lack of element-specific methods with sufficiently low detection limits. Here, we optimized ion-pair chromatographic separation for coupling to an inductively coupled plasma-mass spectrometry detector (IPC-ICP-MS). 2-Propanol (10%-25% gradient) replaced the previously used acetonitrile (25%-75%) as the solvent, to reduce the carbon load into the plasma. In synthetic solutions, formation of thiomolybdates was found to occur spontaneously in the presence of excess sulfide and the degree of thiolation was highest at pH 7. Excess hydroxyl led to a transformation of thiomolybdates to molybdate. Under acidic to neutral conditions, precipitation of molybdenum and hydrolysis of tetrathiomolybdate were observed. Flash-freezing was found to be suitable to stabilize tetrathiomolybdate, with 2 mM) negatively affected the detection of molybdate, which eluted mainly in the dead volume, but had no negative effect on higher thiolated molybdates. Detection limits were ∼10 nM. With the newly developed IPC-ICP-MS method, thiomolybdates were found to form spontaneously in euxinic marine waters after adding a molybdate spike and occur naturally in sulfidic geothermal waters.

  4. Speciation analysis of 129I in seawater using coprecipitation and accelerator mass spectrometry and its applications

    DEFF Research Database (Denmark)

    Xing, Shan; Hou, Xiaolin; Aldahan, Ala


    Speciation analysis of long-lived 129I in seawater can provide useful information on the source of water masses. This paper presents an improved method for speciation analysis of 129I based on coprecipitation of iodide as AgI with Ag2SO3 and AgCl. By adding a small amount of 127I carrier, the sep...

  5. Kinetic studies of nickel speciation in model solutions of a well-characterized humic acid using the competing ligand exchange method

    Energy Technology Data Exchange (ETDEWEB)

    Guthrie, J.W.; Mandal, R.; Salam, M.S.A.; Hassan, N.M.; Murimboh, J.; Chakrabarti, C.L.; Back, M.H.; Gregoire, D.C


    Publications on the binding characteristics of metals with humic acid (HA) are sparse. Here we investigated the release of nickel from Ni(II)-HA complexes using model solutions of three different [Ni(II)]/[HA] mole ratios at three different pH values; we also compared the results with those of [Ni(II)]/[FA] complexes from previous work in this laboratory. Ligand exchange kinetics using the competing ligand exchange method (CLEM) were studied using two different techniques: graphite furnace atomic absorption spectrometry (GFAAS) with Chelex 100 resin as the competing ligand, and adsorptive cathodic stripping voltammetry (AdCSV) with dimethylglyoxime as the competing ligand to measure the rate of dissociation of Ni(II)-HA complexes. The results of the kinetic studies showed that as the [Ni(II)]/[HA] mole ratio was decreased, the rate of dissociation of Ni(II)-HA complexes decreased, and the proportion of free Ni{sup 2+} ions plus very labile nickel complexes decreased while the proportion of the less labile kinetically distinguishable components increased. Generally, the rate of dissociation of Ni(II)-HA complexes was slower than that of Ni(II)-FA complexes. Studies on the validity of the kinetic model showed that the concentrations of chemical species varied in a reasonable way with pH and the [Ni(II)]/[HA] mole ratios, indicating that the kinetically distinguishable components have chemical significance and the kinetic model is valid.

  6. Arsenic speciation in edible mushrooms. (United States)

    Nearing, Michelle M; Koch, Iris; Reimer, Kenneth J


    The fruiting bodies, or mushrooms, of terrestrial fungi have been found to contain a high proportion of the nontoxic arsenic compound arsenobetaine (AB), but data gaps include a limited phylogenetic diversity of the fungi for which arsenic speciation is available, a focus on mushrooms with higher total arsenic concentrations, and the unknown formation and role of AB in mushrooms. To address these, the mushrooms of 46 different fungus species (73 samples) over a diverse range of phylogenetic groups were collected from Canadian grocery stores and background and arsenic-contaminated areas. Total arsenic was determined using ICP-MS, and arsenic speciation was determined using HPLC-ICP-MS and complementary X-ray absorption spectroscopy (XAS). The major arsenic compounds in mushrooms were found to be similar among phylogenetic groups, and AB was found to be the major compound in the Lycoperdaceae and Agaricaceae families but generally absent in log-growing mushrooms, suggesting the microbial community may influence arsenic speciation in mushrooms. The high proportion of AB in mushrooms with puffball or gilled morphologies may suggest that AB acts as an osmolyte in certain mushrooms to help maintain fruiting body structure. The presence of an As(III)-sulfur compound, for the first time in mushrooms, was identified in the XAS analysis. Except for Agaricus sp. (with predominantly AB), inorganic arsenic predominated in most of the store-bought mushrooms (albeit with low total arsenic concentrations). Should inorganic arsenic predominate in these mushrooms from contaminated areas, the risk to consumers under these circumstances should be considered.

  7. Trace element analytical speciation in biological systems: importance, challenges and trends (United States)

    Sanz-Medel, Alfredo


    Speciation of trace elements is a relatively new field and it was in toxicology that the relationship between the chemical form of a metal and its harmful effects was first recognized. The present need for chemical speciation information in biochemistry bioinorganic and clinical chemistry is documented in an attempt to justify the present demand for innovative chemical speciation strategies and analytical technologies. The challenge and complexity of speciation is stressed and three different categories of analytical speciation of increasing analytical difficulty are proposed. Analytical strategies developed so far to try to tackle speciation problems (computational approaches, direct species-specific and hybrid techniques) are reviewed and critically assessed for biological materials. It is indisputable these days that in most cases of real-life analytical speciation we have to resort to the development and use of hybrid techniques combining an adequate separation technique for the species physical separation and an element specific detector such as those based in atomic spectrometry. Examples of such strategies, as developed mainly in the author's laboratory and including chromatographic and non-chromatographic type hybrid strategies coupled to flame, plasma and electrothermal vaporization atomic detectors, are discussed in more detail. Finally, in light of the latest trends observed in this new field, the author attempts to cast a forward look into the foreseeable future of analytical speciation research in biological and biomedical sciences. The urgent plea for quality assurance in non-routine analysis and the concept of using complementary analytical techniques and definitive methods to attack the complexity of chemical speciation in biological systems are particularly highlighted.

  8. Estimating the duration of speciation from phylogenies

    NARCIS (Netherlands)

    Etienne, Rampal S.; Morlon, Helene; Lambert, Amaury

    Speciation is not instantaneous but takes time. The protracted birth-death diversification model incorporates this fact and predicts the often observed slowdown of lineage accumulation toward the present. The mathematical complexity of the protracted speciation model has barred estimation of its

  9. Adaptive speciation theory : A conceptual review

    NARCIS (Netherlands)

    Weissing, Franz J.; Edelaar, Pim; van Doorn, G. Sander

    Speciation-the origin of new species-is the source of the diversity of life. A theory of speciation is essential to link poorly understood macro-evolutionary processes, such as the origin of biodiversity and adaptive radiation, to well understood micro-evolutionary processes, such as allele

  10. A tipping point in parapatric speciation. (United States)

    Yamaguchi, Ryo; Iwasa, Yoh


    More than two loci are involved in reproductive isolation in most cases of putative recent speciation. We study the speciation between two geographically isolated populations connected by infrequent migration, in which incompatibility is controlled by quantitative loci. Incompatibility genetic distance is defined as the fraction of compatibility controlling loci that are different between individuals. Speciation is established when genetic distance reaches a threshold level in spite of occasional migration and subsequent hybridization that reduce genetic distance. With stochastic analysis, we investigate how the time to speciation depends on the manner in which the magnitude of incompatibility increases with genetic distance. Results are: (1) The time to speciation is short if the migration rate is smaller than the mutation rate, or if intermediate levels of genetic distance cause mild incompatibility, making migrants less effective in reducing genetic distance. (2) Genetic distance may fluctuate around a positive quasi-equilibrium level for a long time, and suddenly show a quick passage to speciation when it goes beyond a "tipping point." Notably a gradual increase in incompatibility can result in a sudden and rapid formation of a new species. (3) Speciation becomes very slow if incompatibility is effective for individuals differing at only one locus. These findings provide testable predictions on reproductive traits controlled by specific incompatibility accumulation forms that facilitate the speciation process. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Speciation of heavy metals in River Rhine

    NARCIS (Netherlands)

    Vega, F.A.; Weng, L.


    Chemical speciation of Zn, Cu, Ni, Cd and Pb in River Rhine was studied by measuring free ion concentration and distribution in nanoparticles, and by comparing the measurement with speciation modeling. Concentrations of free metal ions were determined in situ using Donnan Membrane Technique (DMT).

  12. Advances in Ecological Speciation: an integrative approach. (United States)

    Faria, Rui; Renaut, Sebastien; Galindo, Juan; Pinho, Catarina; Melo-Ferreira, José; Melo, Martim; Jones, Felicity; Salzburger, Walter; Schluter, Dolph; Butlin, Roger


    The role of natural selection in promoting reproductive isolation has received substantial renewed interest within the last two decades. As a consequence, the study of ecological speciation has become an extremely productive research area in modern evolutionary biology. Recent innovations in sequencing technologies offer an unprecedented opportunity to study the mechanisms involved in ecological speciation. Genome scans provide significant insights but have some important limitations; efforts are needed to integrate them with other approaches to make full use of the sequencing data deluge. An international conference 'Advances in Ecological Speciation' organized by the University of Porto (Portugal) aimed to review current progress in ecological speciation. Using some of the examples presented at the conference, we highlight the benefits of integrating ecological and genomic data and discuss different mechanisms of parallel evolution. Finally, future avenues of research are suggested to advance our knowledge concerning the role of natural selection in the establishment of reproductive isolation during ecological speciation. © 2013 John Wiley & Sons Ltd.

  13. A two-locus model of speciation. (United States)

    Gregorius, H R


    Speciation is considered as the evolution of partial or complete cross-incompatibility between the carriers of genes (at a locus called "object locus") that distinguish the prospective species populations. The mating relations at the object locus are modified by the alleles at a second mating modifier locus. Based on a widely applicable concept of fitness and mating preference, it is shown that heterozygote disadvantage in fitness at the object locus is necessary for speciation, which corroborates Wallace's hypothesis. It is pointed out that the difference between sympatric and parapatric speciation essentially lies in the mechanisms stabilizing the polymorphism required at the object locus as a prerequisite for speciation. In the presence of recombination between the object and mating modifier locus speciation may be prevented by forces maintaining gametic phase imbalance between these loci such as can result from unidirectional gene flow between parapatric populations.

  14. Rapid parapatric speciation on holey adaptive landscapes

    CERN Document Server

    Gavrilets, S; Vose, M D; Gavrilets, Sergey; Li, Hai; Vose, Michael D.


    A classical view of speciation is that reproductive isolation arises as a by-product of genetic divergence. Here, individual-based simulations are used to evaluate whether the mechanisms implied by this view may result in rapid speciation if the only source of genetic divergence are mutation and random genetic drift. Distinctive features of the simulations are the consideration of the complete process of speciation (from initiation until completion), and of a large number of loci, which was only one order of magnitude smaller than that of bacteria. It is demonstrated that rapid speciation on the time scale of hundreds of generations is plausible without the need for extreme founder events, complete geographic isolation, the existence of distinct adaptive peaks or selection for local adaptation. The plausibility of speciation is enhanced by population subdivision. Simultaneous emergence of more than two new species from a subdivided population is highly probable. Numerical examples relevant to the theory of ce...

  15. A microchannel confocal examination of arsenic speciation and distribution in Bufo americanus (United States)

    Nearing, Michelle M.; Koch, Iris; Gordon, Robert A.; Reimer, Kenneth J.


    We have used confocal methods to examine the distribution and speciation of arsenic within amphibian tissue (Bufo americanus) from a contaminated mine site. The use of new microchannel technology permits a confocal, and energy-independent, examination of a given voxel within the amphibian tissue without the need for sectioning. We observe differences in arsenic concentration and speciation depending on tissue type, with the Eberth- Katschenko layer in particular containing Mn, Fe, Cu and Zn in addition to Ca and pentavalent arsenic.

  16. A validated spectrofluorimetric method for the determination of citalopram in bulk and pharmaceutical preparations based on the measurement of the silver nanoparticles-enhanced fluorescence of citalopram/terbium complexes. (United States)

    Khan, Muhammad Naeem; Shah, Jasmin; Jan, Muhammad Rasul; Lee, Sang Hak


    A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02-14 μg mL(-1), with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15 × 10(-6) μg mL(-1) and 2.38 × 10(-5) μg mL(-1) respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66% (n = 6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98% to 100.97% for bulk powder and from 96.57% to 101.77% for pharmaceutical preparations.

  17. Cosmological Brane World Solutions with Bulk Scalar Fields


    Davis, Stephen C.


    Cosmological brane world solutions are found for five-dimensional bulk spacetimes with a scalar field. A supergravity inspired method for obtaining static solutions is combined with a method for finding brane cosmologies with constant bulk energies. This provides a way to generate full (bulk and brane) cosmological solutions to brane worlds with bulk scalar fields. Examples of these solutions, and their cosmological evolution, are discussed.

  18. Surveying selenium speciation from soil to cell - forms and transformations

    Energy Technology Data Exchange (ETDEWEB)

    Gammelgaard, Bente; Gabel-Jensen, Charlotte [University of Copenhagen, Department of Pharmaceutics and Analytical Chemistry, Faculty of Pharmaceutical Sciences, Copenhagen (Denmark); Jackson, Matthew I. [Grand Forks Human Nutrition Research Center, Agricultural Research Service, United States Department of Agriculture, Grand Forks, ND (United States)


    The aim of this review is to present and evaluate the present knowledge of which selenium species are available to the general population in the form of food and common supplements and how these species are metabolized in mammals. The overview of the selenium sources takes a horizontal approach, which encompasses identification of new metabolites in yeast and food of plant and animal origin, whereas the survey of the mammalian metabolism takes a horizontal as well as a vertical approach. The vertical approach encompasses studies on dynamic conversions of selenium compounds within cells, tissues or whole organisms. New and improved sample preparation, separation and detection methods are evaluated from an analytical chemical perspective to cover the progress in horizontal speciation, whereas the analytical methods for the vertical speciation and the interpretations of the results are evaluated from a biological angle as well. (orig.)

  19. Sexual selection and diversification: reexamining the correlation between dichromatism and speciation rate in birds. (United States)

    Huang, Huateng; Rabosky, Daniel L


    Theory predicts that sexual selection can serve as an important driver of speciation, but phylogenetic comparative analyses have failed to demonstrate a consistent effect of sexual selection on species richness at macroevolutionary scales. Sexual dichromatism in birds is an example of a phenotypic trait that is hypothesized to reflect the intensity of sexual selection, yet previous studies have reached ambiguous conclusions regarding its role in promoting species diversification. Here, we revisit this problem by pairing published spectrophotometer estimates of plumage dichromatism in the bird-visible range with a newly developed method for modeling speciation rates on phylogenetic trees that explicitly accounts for diversification rate variation through time and among clades. We find little evidence linking dichromatism to speciation across birds, using several measures of dichromatism and macroevolutionary diversification. These results suggest that sexual dichromatism plays a limited role in determining speciation rates at macroevolutionary scales in birds.

  20. Heat transport in bulk/nanoporous/bulk silicon devices

    Energy Technology Data Exchange (ETDEWEB)

    Criado-Sancho, M. [Departamento de Ciencias y Técnicas Físicoquimicas, Facultad de Ciencias, UNED, Senda del Rey 9, 20040 Madrid (Spain); Jou, D., E-mail: [Departament de Física, Universitat Autònoma de Barcelona, 08193 Bellaterra, Catalonia (Spain); Institut d' Estudis Catalans, Carme 47, 08001 Barcelona, Catalonia (Spain)


    We study heat transport in bulk/nanoporous/bulk silicon devices; we show that, despite bulk/nanoporous devices may act as thermal rectifiers, the non-linear aspects of their joint thermal conductance are not strong enough to lead to a negative differential thermal resistance, necessary to allow bulk/nanoporous/bulk Si devices to act as thermal transistors. Furthermore, we explicitly study the effective thermal conductivity of the mentioned devices for several temperatures, geometries, porosities, and pore size.

  1. Contributions of surface and bulk heterogeneities to the NO oxidation activities of ceria-zirconia catalysts with composition Ce(0.76)Zr(0.24)O(2) prepared by different methods. (United States)

    Atribak, Idriss; Bueno-López, Agustín; García-García, Avelina; Azambre, Bruno


    The study of the catalytic activity towards NO oxidation to NO(2) was approached by using ceria-zirconia mixed oxides with the same nominal composition (Ce(0.76)Zr(0.24)O(2)) but prepared by different routes of synthesis: coprecipitation, solid combustion synthesis with urea, citrate complexation route, reversed microemulsion and template synthesis. The characterisation of the catalysts was performed by N(2) adsorption at -196 °C, XRD, Raman Spectroscopy, H(2)-TPR and XPS in order to ascertain the relationships between their catalytic activities and their bulk and surface properties. The results showed that the preparation method is critical for the physico-chemical properties of the mixed oxides, exhibiting very different BET surface areas, crystalline phase/s contributions and bulk oxygen mobility. The distribution of Ce and Zr on the surface with regard to the bulk is very much influenced by the preparation method as well. The NO(2) production from NO oxidation was shown to be mostly correlated with the Ce/Zr surface atomic ratio and the proportion of Ce(4+) (presumably in a doped cubic phase) in the uppermost layers.

  2. "Understanding" cosmological bulk viscosity


    Zimdahl, Winfried


    A universe consisting of two interacting perfect fluids with the same 4-velocity is considered. A heuristic mean free time argument is used to show that the system as a whole cannot be perfect as well but neccessarily implies a nonvanishing bulk viscosity. A new formula for the latter is derived and compared with corresponding results of radiative hydrodynamics.

  3. Bulk chemicals from biomass

    NARCIS (Netherlands)

    Haveren, van J.; Scott, E.L.; Sanders, J.P.M.


    Given the current robust forces driving sustainable production, and available biomass conversion technologies, biomass-based routes are expected to make a significant impact on the production of bulk chemicals within 10 years, and a huge impact within 20-30 years. In the Port of Rotterdam there is a

  4. Tipping points in the dynamics of speciation. (United States)

    Nosil, Patrik; Feder, Jeffrey L; Flaxman, Samuel M; Gompert, Zachariah


    Speciation can be gradual or sudden and involve few or many genetic changes. Inferring the processes generating such patterns is difficult, and may require consideration of emergent and non-linear properties of speciation, such as when small changes at tipping points have large effects on differentiation. Tipping points involve positive feedback and indirect selection stemming from associations between genomic regions, bi-stability due to effects of initial conditions and evolutionary history, and dependence on modularity of system components. These features are associated with sudden 'regime shifts' in other cellular, ecological, and societal systems. Thus, tools used to understand other complex systems could be fruitfully applied in speciation research.

  5. Speciation gradients and the distribution of biodiversity. (United States)

    Schluter, Dolph; Pennell, Matthew W


    Global patterns of biodiversity are influenced by spatial and environmental variations in the rate at which new species form. We relate variations in speciation rates to six key patterns of biodiversity worldwide, including the species-area relationship, latitudinal gradients in species and genetic diversity, and between-habitat differences in species richness. Although they sometimes mirror biodiversity patterns, recent rates of speciation, at the tip of the tree of life, are often highest where species richness is low. Speciation gradients therefore shape, but are also shaped by, biodiversity gradients and are often more useful for predicting future patterns of biodiversity than for interpreting the past.

  6. Mercury speciation in seafood using isotope dilution analysis: a review. (United States)

    Clémens, Stéphanie; Monperrus, Mathilde; Donard, Olivier F X; Amouroux, David; Guérin, Thierry


    Mercury is a toxic compound that can contaminate humans through food and especially via fish consumption. Mercury's toxicity depends on the species, with methylmercury being the most hazardous form for humans. Hg speciation analysis has been and remains a widely studied subject because of the potential difficulty of preserving the initial distribution of mercury species in the analysed sample. Accordingly, many analytical methods have been developed and most of them incur significant loss and/or cross-species transformations during sample preparation. Therefore, to monitor and correct artefact formations, quantification by isotope dilution is increasingly used and provides significant added value for analytical quality assurance and quality control. This review presents and discusses the two different modes of application of isotope dilution analysis for elemental speciation (i.e. species-unspecific isotope dilution analysis and species-specific isotope dilution analysis) and the different quantification techniques (i.e. classical and multiple spike isotope dilution analyses). Isotope tracers are thus used at different stages of sample preparation to determine the extent of inter-species transformations and correct such analytical artefacts. Finally, a synthesis of the principal methods used for mercury speciation in seafood using isotope dilution analysis is presented. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Trace metal characterization and speciation in geothermal effluent by multiple scanning anodic stripping voltammetry and atomic absorption analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kowalski, B.R.


    Recent studies have shown geothermal power plants to have a significant environmental impact on the ground water of the area. The heavy metals arsenic and mercury are special problems, as both are concentrated by flora and fauna exposed to the effluent waters. Because the toxicity of these and other metallic pollutants present in geothermal effluent depends on the chemical form, or speciation, of the particular metal, any serious study of the environmental impact of a geothermal development should include studies of trace metal speciation, in addition to trace metal concentration. This proposal details a method for determining metal speciation in dilute waters. The method is based on ion-exchange and backed by atomic absorption spectrometry and multiple scanning anodic stripping voltammetry. Special laboratory studies will be performed on mercury, arsenic and selenium speciation in synthetic geothermal water. The method will be applied to three known geothermal areas in Washington and Oregon, with emphasis on the speciation of mercury, arsenic and selenium in these waters. The computer controlled electrochemical instrumentation was built and tested. Using this instrumentation, a new experimental procedure was developed to determine the chemical form (speciation) of metal ions in very dilute solutions (ng/ml). This method was tested on model systems including Pb, Cd, and As with C1/sup -/, CO/sub 3//sup 2 -/ and glycine ligands. Finally, the speciation of lead in a geothermal water was examined and the PbC1/sup +/ complex was observed and quantified.

  8. Speciation and distribution of arsenic and localization of nutrients in rice grains

    Energy Technology Data Exchange (ETDEWEB)

    Lombi, E.; Scheckel, K.G.; Pallon, J.; Carey, A.M.; Zhu, Y.G.; Meharg, A.A. (EPA); (UCopenhagen); (Aberdeen); (Lund); (Chinese Aca. Sci.)


    Arsenic (As) contamination of rice grains and the generally low concentration of micronutrients in rice have been recognized as a major concern for human health. Here, we investigated the speciation and localization of As and the distribution of (micro)nutrients in rice grains because these are key factors controlling bioavailability of nutrients and contaminants. Bulk total and speciation analyses using high-pressure liquid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) and X-ray absorption near-edge spectroscopy (XANES) was complemented by spatially resolved microspectroscopic techniques ({mu}-XANES, {mu}-X-ray fluorescence ({mu}-XRF) and particle induced X-ray emission (PIXE)) to investigate both speciation and distribution of As and localization of nutrients in situ. The distribution of As and micronutrients varied between the various parts of the grains (husk, bran and endosperm) and was characterized by element-specific distribution patterns. The speciation of As in bran and endosperm was dominated by As(III)-thiol complexes. The results indicate that the translocation from the maternal to filial tissues may be a bottleneck for As accumulation in the grain. Strong similarities between the distribution of iron (Fe), manganese (Mn) and phosphorus (P) and between zinc (Zn) and sulphur (S) may be indicative of complexation mechanisms in rice grains.

  9. Evolution: sympatric speciation the eusocial way

    DEFF Research Database (Denmark)

    Boomsma, Jacobus Jan; Nash, David Richard


    Sympatric speciation normally requires particular conditions of ecological niche differentiation. However, ant social parasites have been suspected to arise sympatrically, because (dis)loyalty to eusocial kin-structures induces disruptive selection for dispersal and inbreeding. A new study...

  10. Aerosol Chemical Speciation Monitor (ACSM) Instrument Handbook

    Energy Technology Data Exchange (ETDEWEB)

    Watson, Thomas B. [Brookhaven National Lab. (BNL), Upton, NY (United States)


    The Aerodyne Aerosol Chemical Speciation Monitor (ACSM) measures particle mass loading and chemical composition in real time for non-refractory sub-micron aerosol particles. The ACSM is designed for long-term unattended deployment and routine monitoring applications.

  11. Dearborn GC-MS organic speciation data (United States)

    U.S. Environmental Protection Agency — Ambient particulate matter organic speciation data from July - August, 2011. This dataset is associated with the following publication: Lynam, M., T. Dvonch, J....

  12. Pb speciation results in amended soils (United States)

    U.S. Environmental Protection Agency — The dataset shows the distribution of Pb phases resulting from various amendments to change Pb speciation. This dataset is associated with the following publication:...

  13. Mistletoes as parasites: Host specificity and speciation. (United States)

    Norton, D A; Carpenter, M A


    Recent research on parasite evolution has highlighted the importance of host specialization in speciation, either through host-switching or cospeciation. Many parasites show common patterns of host specificity, with higher host specificity where host abundance is high and reliable, phylogenetically conservative host specificity, and formation of races on or in different host species. Recent advances in our understanding of host specificity and speciation patterns in a variety of animal parasites provides valuable insights into the evolutionary biology of mistletoes.

  14. Electrochemical metal speciation in colloidal dispersions


    Wonders, J.H.A.M.


    The term "heavy metals" is connected with toxicity. They form strong complexes with enzymes, other proteins and DNA in living organisms, which causes dysfunctioning and hence poisoning. In combination with the uptake mechanism of the organism, speciation of heavy metal determines the bio-availability of heavy metals. In the environment, heavy metals are complexed by soil particles or molecules of organic and inorganic origin. This thesis deals with the speciation and the binding char...

  15. Diffusion or bulk flow

    DEFF Research Database (Denmark)

    Schulz, Alexander


    symplasmic pathway from mesophyll to sieve elements. Crucial for the driving force is the question where water enters the pre-phloem pathway. Surprisingly, the role of PD in water movement has not been addressed so far appropriately. Modeling of assimilate and water fluxes indicates that in symplasmic...... the concentration gradient or bulk flow along a pressure gradient. The driving force seems to depend on the mode of phloem loading. In a majority of plant species phloem loading is a thermodynamically active process, involving the activity of membrane transporters in the sieve-element companion cell complex. Since...... is currently matter of discussion, called passive symplasmic loading. Based on the limited material available, this review compares the different loading modes and suggests that diffusion is the driving force in apoplasmic loaders, while bulk flow plays an increasing role in plants having a continuous...

  16. Diffusion or bulk flow

    DEFF Research Database (Denmark)

    Schulz, Alexander


    is currently matter of discussion, called passive symplasmic loading. Based on the limited material available, this review compares the different loading modes and suggests that diffusion is the driving force in apoplasmic loaders, while bulk flow plays an increasing role in plants having a continuous...... the concentration gradient or bulk flow along a pressure gradient. The driving force seems to depend on the mode of phloem loading. In a majority of plant species phloem loading is a thermodynamically active process, involving the activity of membrane transporters in the sieve-element companion cell complex. Since...... assimilate movement includes an apoplasmic step, this mode is called apoplasmic loading. Well established is also the polymer-trap loading mode, where the phloem-transport sugars are raffinose-family oligomers in herbaceous plants. Also this mode depends on the investment of energy, here for sugar...

  17. Micromegas in a bulk

    CERN Document Server

    Giomataris, Ioanis; Andriamonje, Samuel A; Aune, S; Charpak, Georges; Colas, P; Giganon, Arnaud; Rebourgeard, P C; Salin, P; Rebourgeard, Ph.


    In this paper we present a novel way to manufacture the bulk Micromegas detector. A simple process based on the PCB (Printed Circuit Board) technology is employed to produce the entire sensitive detector. Such fabrication process could be extended to very large area detectors made by the industry. The low cost fabrication together with the robustness of the electrode materials will make it extremely attractive for several applications ranging from particle physics and astrophysics to medicine

  18. Micromegas in a bulk

    Energy Technology Data Exchange (ETDEWEB)

    Giomataris, I. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France)]. E-mail:; De Oliveira, R. [CERN, Geneva (Switzerland); Andriamonje, S. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France); Aune, S. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France); Charpak, G. [CERN, Geneva (Switzerland); Colas, P. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France); Fanourakis, G. [Institute of Nuclear Physcis, NCSR Demokritos, Aghia Paraskevi 15310 (Greece); Ferrer, E. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France); Giganon, A. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France); Rebourgeard, Ph. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France); Salin, P. [DAPNIA, CEA Saclay, F91191 Gif sur Yvette CEDEX (France)


    In this paper, we present a novel way to manufacture the bulk Micromegas detector. A simple process based on the Printed Circuit Board (PCB) technology is employed to produce the entire sensitive detector. Such a fabrication process could be extended to very large area detectors made by the industry. The low cost fabrication together with the robustness of the electrode materials will make it attractive for several applications ranging from particle physics and astrophysics to medicine.

  19. Speciation, in the nuclear fuel cycle by spectroscopic techniques

    Energy Technology Data Exchange (ETDEWEB)

    Colette, S.; Plancque, G.; Allain, F.; Lamouroux, C.; Steiner, V.; Amekraz, B.; Moulin, C. [CEA/Saclay, Dept, des Procedes d' Enrichissement (DPE), 91 - Gif-sur-Yvette (France)


    New analytical techniques allowing to perform speciation in the framework of the nuclear fuel cycle are more and more needed. They have to be selective (since matrix encountered are very complex), sensitive (in order to work at representative concentration and below solubility limit), as well as non intrusive (in order to keep the image of the real solution). Among them, laser-based analytical techniques present these advantages together with the possibility to perform remote measurements via fiber optics. Hence, Time-Resolved Laser-Induced Fluorescence (TRLIF) has been used for actinides/lanthanides interaction and speciation studies in inorganic and organic matrices from the reprocessing to waste storage. Moreover, new ion detection methods such as Electro-Spray - Mass Spectrometry (ES-MS) seems promising for speciation studies. Hence, it is the first time that it is possible to directly couple a liquid at atmospheric pressure to a mass detection working at reduced pressure with a soft mode of ionisation that should allow to give informations on chemical species present. Principle, advantages and limitations as well as results obtained with the use of TRLIF and ES-MS on different systems of interest including actinides, lanthanides, fission products in interaction with simple organic molecules to very complex structure will be presented and discussed. (authors)

  20. Chemical speciation of vanadium in coal bottom Ash

    Energy Technology Data Exchange (ETDEWEB)

    Aydin, Firat; Aydin, Isil; Hamamci, Candan [Science Faculty, Chemistry Department, Dicle University, Diyarbakir (Turkey); Saydut, Abdurrahman [Engineering Faculty, Mining Engineering Department, Dicle University, Diyarbakir (Turkey); Gunduz, Beniz [Science Faculty, Chemistry Department, Selcuk University, Konya (Turkey)


    Chemical speciation of vanadium is important to understand the true nature of this element in the environment as well as its biochemical pathways. Sample pretreatment, preparation, and chemical speciation methods were applied for vanadium in coal bottom ash here. Two-stage microwave acid digestion was used to preparation of samples. Determination of vanadium was performed using inductively coupled plasma-optical emission spectrometry (ICP-OES). Speciation of vanadium was carried out using a seven-step sequential extraction procedure of the coal bottom ash each releasing species of vanadium: Water soluble, exchangeable, carbonate, reducible, oxidizable, sulfide, and residual fractions. Total vanadium concentration in the coal bottom ash is 701 mg kg{sup -1} d.w. The most abundant form of vanadium in coal bottom ash is residual fraction of vanadium (196 mg kg{sup -1} d.w.). Relative abundances of the remaining vanadium fractions in coal bottom ash are as follows: Reducible (176 mg kg{sup -1} d.w.) > sulfide (176 mg kg{sup -1} d.w.) > carbonate (85 mg kg{sup -1} d.w.) > oxidizable (50 mg kg{sup -1} d.w.) > water soluble (10.6 mg kg{sup -1} d.w.) > exchangeable (9.0 mg kg{sup -1} d.w.). (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  1. Magnetic property and microstructure of Nd-Fe-B-M (M = Si, C) bulk nanocomposite magnets prepared by spark plasma sintering method

    Energy Technology Data Exchange (ETDEWEB)

    Fukuzaki, T; Tamura, R [Polyscale Technology Research Center, Tokyo University of Science (Japan); Tanaka, K; Nishimoto, K; Nishio, K [Department of Materials Science and Technology, Tokyo University of Science (Japan); Muro, Y [Department of Physics, Tokyo University of Science 2641 Yamazaki, Noda, Chiba, 278-8510 (Japan)], E-mail:


    We have prepared Nd{sub 2}Fe{sub 14}B/(a-Fe or Fe{sub 3}B) bulk nanocomposite magnets at the compositions of Nd{sub 4}Fe{sub 77.5}B{sub 18.5-x}M{sub x} (M = Si, C) by substituting other elements M for B. In the case of the Si substitution, the saturation magnetization is found to increase while the coercivity remains the same at 1 at.%Si. In the case of the C substitution, the magnetic behavior becomes drastically softer for more than 1at.%C, which is attributed to the suppression of the Nd{sub 2}Fe{sub 14}B hard phase. Finally, the grain sizes of the Nd{sub 2}Fe{sub 14}B and the Fe{sub 3}B phases are found to depend on the ramp-up time, and the reduction of the grain size results in an increase of the coercivity.

  2. Bulk density of small meteoroids (United States)

    Kikwaya, J.-B.; Campbell-Brown, M.; Brown, P. G.


    Aims: Here we report on precise metric and photometric observations of 107 optical meteors, which were simultaneously recorded at multiple stations using three different intensified video camera systems. The purpose is to estimate bulk meteoroid density, link small meteoroids to their parent bodies based on dynamical and physical density values expected for different small body populations, to better understand and explain the dynamical evolution of meteoroids after release from their parent bodies. Methods: The video systems used had image sizes ranging from 640 × 480 to 1360 × 1036 pixels, with pixel scales from 0.01° per pixel to 0.05° per pixel, and limiting meteor magnitudes ranging from Mv = +2.5 to +6.0. We find that 78% of our sample show noticeable deceleration, allowing more robust constraints to be placed on density estimates. The density of each meteoroid is estimated by simultaneously fitting the observed deceleration and lightcurve using a model based on thermal fragmentation, conservation of energy and momentum. The entire phase space of the model free parameters is explored for each event to find ranges of parameters which fit the observations within the measurement uncertainty. Results: (a) We have analysed our data by first associating each of our events with one of the five meteoroid classes. The average density of meteoroids whose orbits are asteroidal and chondritic (AC) is 4200 kg m-3 suggesting an asteroidal parentage, possibly related to the high-iron content population. Meteoroids with orbits belonging to Jupiter family comets (JFCs) have an average density of 3100 ± 300 kg m-3. This high density is found for all meteoroids with JFC-like orbits and supports the notion that the refractory material reported from the Stardust measurements of 81P/Wild 2 dust is common among the broader JFC population. This high density is also the average bulk density for the 4 meteoroids with orbits belonging to the Ecliptic shower-type class (ES) also

  3. Polysulfide speciation and reactivity in chromate-contaminated soil. (United States)

    Chrysochoou, Maria; Johnston, Chad P


    Calcium polysulfide (CPS) has been observed to maintain a reducing capacity for prolonged time periods when used to treat Cr(VI)-contaminated soils. This study utilized bulk and micro-X-ray absorption near edge structure (XANES) spectroscopy to investigate sulfur speciation in soil samples treated with CPS in batch and column studies and to determine the source of the reducing potential. Bulk XANES spectra indicated the presence of two dominant sulfur species: elemental sulfur, which is the product of the sulfide-chromate redox reaction, and thiosulfate (S2O3(2-)). Micro-XANES analyses confirmed these findings and showed that elemental sulfur precipitated as large particles, while thiosulfate was diffused within the soil grains and thus available to react with chromate that leached from slowly dissolving PbCrO4. Micro-X-ray fluorescence (μXRF) analyses indicated a close association of Pb and thiosulfate, so that PbS2O3 is a likely sink for thiosulfate, accounting for up to 20% of the total S added. Sorption of thiosulfate on iron oxides below pH 8 is a second retention mechanism for thiosulfate in the solid. Given that thiosulfate cannot reduce chromate but can reduce solid-bound Fe(III) under neutral pH conditions, it is hypothesized that ferrous iron production is an additional mechanism to maintain reductive conditions in CPS-treated soils. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Speciation of arsenic, selenium, and chromium in wildfire impacted soils and ashes (United States)

    Wolf, Ruth E.; Hoefen, Todd M.; Hageman, Philip L.; Morman, Suzette A.; Plumlee, Geoffrey S.


    In 2007-09, California experienced several large wildfires that damaged large areas of forest and destroyed many homes and buildings. The U.S. Geological Survey collected samples from the Harris, Witch, Grass Valley, Ammo, Santiago, Canyon, Jesusita, and Station fires for testing to identify any possible characteristics of the ashes and soils from burned areas that may be of concern for their impact on water quality, human health, and endangered species. The samples were subjected to analysis for bulk chemical composition for 44 elements by inductively coupled plasma mass spectrometry (ICP-MS) after acid digestion and de-ionized water leach tests for pH, alkalinity, conductivity, and anions. Water leach tests generated solutions ranging from pH 10-12, suggesting that ashes can generate caustic alkalinity in contact with rainwater or body fluids (for example, sweat and fluids in the respiratory tract). Samples from burned residential areas in the 2007 fires had elevated levels for several metals, including: As, Pb, Sb, Cu, Zn, and Cr. In some cases, the levels found were above the U.S. Environmental Protection Agency (USEPA) preliminary remediation goals (PRG) for soils. Speciation analyses were conducted on de-ionized water and simulated lung fluid leachates for As(III), As(V), Se(IV), Se(VI), Cr(III), and Cr(VI). All species were determined in the same analytical run using an ion-pairing HPLC-ICP-MS method. For leachates containing high levels of total Cr, the majority of the chromium was present in the hexavalent, Cr(VI), form. Higher total and hexavalent chromium levels were observed for samples collected from burned residential areas. Arsenic was also generally present in the more oxidized, As(V), form. Selenium (IV) and (VI) were present, but typically at levels below 2 ppb for most samples. Stability studies of leachate solutions under different storage conditions were performed and the suitability of different sample preservation methods for speciation

  5. Chemical Speciation of Long-lived Radionuclide Technetium-99 and its Environmental Behaviour

    DEFF Research Database (Denmark)

    Shi, Keliang

    Because of the high fission yield, high mobility and long half-life, technetium-99 is considered to be one of the most important radionuclides in environmental trace application as well as nuclear waste management. The study on the determination of technetium and its speciation is therefore a key...... issue for understanding its fate and behaviour in ecosystem. This thesis aims to develop series of analytical methods for rapid and accurate determination of total 99Tc in environmental samples (e.g., seaweed, soil, and seawater), as well as speciation analysis of 99Tc in seaweeds. The application of 99...... limit of 1.5 mBq for 99Tc was obtained by ICP-MS measurement. The analytical methods were proved to be reliable and have been successfully applied for the determination of 99Tc in environmental samples. An analytical method for chemical speciation of 99Tc in natural seaweed has been developed. Different...

  6. Bulk Moisture and Salinity Sensor (United States)

    Nurge, Mark; Monje, Oscar; Prenger, Jessica; Catechis, John


    Measurement and feedback control of nutrient solutions in plant root zones is critical to the development of healthy plants in both terrestrial and reduced-gravity environments. In addition to the water content, the amount of fertilizer in the nutrient solution is important to plant health. This typically requires a separate set of sensors to accomplish. A combination bulk moisture and salinity sensor has been designed, built, and tested with different nutrient solutions in several substrates. The substrates include glass beads, a clay-like substrate, and a nutrient-enriched substrate with the presence of plant roots. By measuring two key parameters, the sensor is able to monitor both the volumetric water content and salinity of the nutrient solution in bulk media. Many commercially available moisture sensors are point sensors, making localized measurements over a small volume at the point of insertion. Consequently, they are more prone to suffer from interferences with air bubbles, contact area of media, and root growth. This makes it difficult to get an accurate representation of true moisture content and distribution in the bulk media. Additionally, a network of point sensors is required, increasing the cabling, data acquisition, and calibration requirements. measure the dielectric properties of a material in the annular space of the vessel. Because the pore water in the media often has high salinity, a method to measure the media moisture content and salinity simultaneously was devised. Characterization of the frequency response for capacitance and conductance across the electrodes was completed for 2-mm glass bead media, 1- to 2-mm Turface (a clay like media), and 1- to 2-mm fertilized Turface with the presence of root mass. These measurements were then used to find empirical relationships among capacitance (C), the dissipation factor (D), the volumetric water content, and the pore water salinity.

  7. Quantitative estimation of diacerein in bulk and in capsule formulation using hydrotropic solubilizing agents by UV-spectrophotometry and the first order derivative using the area under curve method. (United States)

    Pandey, Ramchandra; Patil, Pravin O; Patil, Manohar U; Deshmukh, Prashant K; Bari, Sanjay B


    This study was designed to develop and validate two simple, rapid, and economical UV-spectrophotometric and the first-order derivative methods using the area under curve method for estimation of diacerein in bulk and in capsule formulation. In this study, hydrotrophic solution of 8 M urea and 0.5 M potassium citrate were employed as the solubilizing agent to solubilize a poorly water-soluble drug, diacerein. In the UV-spectrophotometry method, two wavelengths 252.0 nm and 266.2 nm and in the first-order derivative spectrophotometric methods two wavelengths 259.4 nm and 274.2 nm in 8 M urea and two wavelengths 247.8 nm and 267.4 nm in the UV-spectrophotometry method and in the first-order derivative spectrophotometric methods two wavelengths 259.2 nm and 274.2 nm in 0.5 M potassium citrate were selected for determination of areas. Hydrotrophic agents used did not interfere in spectrophotometric analysis of diacerein. Diacerein followed linearity in the concentration range of 2-12 μg/mL with a coefficient correlation of 0.999 for both methods. The amount of drugs estimated by both proposed methods are in good accord with label claim. The % RSD value in recovery, precision, and ruggedness studies are found to be less than 2 indicate that the method is accurate, precise, and rugged.

  8. A phylogenetic test of sympatric speciation in the Hydrobatinae (Aves: Procellariiformes). (United States)

    Wallace, S J; Morris-Pocock, J A; González-Solís, J; Quillfeldt, P; Friesen, V L


    Phylogenetic relationships among species can provide insight into how new species arise. For example, careful consideration of both the phylogenetic and geographic distributions of species in a group can reveal the geographic models of speciation within the group. One such model, sympatric speciation, may be more common than previously thought. The Hydrobatinae (Aves: Procellariformes) is a diverse subfamily of Northern Hemisphere storm-petrels for which the taxonomy is unclear. Previous studies showed that Hydrobates (formally Oceanodroma) castro breeding in the Azores during the cool season is sister species to H. monteiroi, a hot season breeder at the same locations, which suggests sympatric speciation by allochrony. To test whether other species within the subfamily arose via sympatric speciation by allochrony, we sequenced the cytochrome b gene and five nuclear introns to estimate a phylogenetic tree using multispecies coalescent methods, and to test whether species breeding in the same geographic area are monophyletic. We found that speciation within the Hydrobatinae appears to have followed several geographic modes of divergence. Sympatric seasonal species in Japan likely did not arise through sympatric speciation, but allochrony may have played a role in the divergence of H. matsudairae, a cool season breeder, and H. monorhis, a hot season breeder. No other potential cases of sympatric speciation were discovered within the subfamily. Despite breeding in the same geographic area, hydrobatine storm-petrels breeding in Baja California (H. microsoma and H. melania) are each sister to a species breeding off the coast of Peru (H. tethys and H. markhami, respectively). In fact, antitropical sister species appear to have diverged at multiple times, suggesting allochronic divergence might be common. In addition, allopatry has likely played a role in divergence of H. furcata, a north Pacific breeder, and H. pelagius, a north Atlantic breeder. This study demonstrates

  9. Cobalt toxicity in anaerobic granular sludge: influence of chemical speciation

    NARCIS (Netherlands)

    Bartacek, J.; Fermoso, F.G.; Baldo-Urrutia, A.M.; Hullebusch, van E.D.; Lens, P.N.L.


    The influence of cobalt speciation on the toxicity of cobalt to methylotrophic methanogenesis in anaerobic granular sludge was investigated. The cobalt speciation was studied with three different media that contained varying concentrations of complexing ligands [carbonates, phosphates and

  10. Novel kinetic spectrophotometric method for estimation of certain biologically active phenolic sympathomimetic drugs in their bulk powders and different pharmaceutical formulations. (United States)

    Omar, Mahmoud A; Badr El-Din, Khalid M; Salem, Hesham; Abdelmageed, Osama H


    A simple, selective and sensitive kinetic spectrophotometric method was described for estimation of four phenolic sympathomimetic drugs namely; terbutaline sulfate, fenoterol hydrobromide, isoxsuprine hydrochloride and etilefrine hydrochloride. This method is depended on the oxidation of the phenolic drugs with Folin-Ciocalteu reagent in presence of sodium carbonate. The rate of color development at 747-760nm was measured spectrophotometrically. The experimental parameters controlling the color development were fully studied and optimized. The reaction mechanism for color development was proposed. The calibration graphs for both the initial rate and fixed time methods were constructed, where linear correlations were found in the general concentration ranges of 3.65×10-6-2.19×10-5molL-1 and 2-24.0μgmL-1 with correlation coefficients in the following range 0.9992-0.9999, 0.9991-0.9998 respectively. The limits of detection and quantitation for the initial rate and fixed time methods were found to be in general concentration range 0.109-0.273, 0.363-0.910 and 0.210-0.483, 0.700-1.611μgmL-1 respectively. The developed method was validated according to ICH and USP 30 -NF 25 guidelines. The suggested method was successfully implemented to the estimation of these drugs in their commercial pharmaceutical formulations and the recovery percentages obtained were ranged from 97.63%±1.37 to 100.17%±0.95 and 97.29%±0.74 to 100.14±0.81 for initial rate and fixed time methods respectively. The data obtained from the analysis of dosage forms were compared with those obtained by reported methods. Statistical analysis of these results indicated no significant variation in the accuracy and precision of both the proposed and reported methods. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. [XANES study of lead speciation in duckweed]. (United States)

    Chu, Bin-Bin; Luo, Li-Qiang; Xu, Tao; Yuan, Jing; Sun, Jian-Ling; Zeng, Yuan; Ma, Yan-Hong; Yi, Shan


    Qixiashan lead-zinc mine of Nanjing was one of the largest lead zinc deposits in East China Its exploitation has been over 50 years, and the environmental pollution has also been increasing. The lead concentration in the local environment was high, but lead migration and toxic mechanism has not been clear. Therefore, biogeochemistry research of the lead zinc mine was carried out. Using ICP-MS and Pb-L III edge XANES, lead concentration and speciation were analyzed respectively, and duckweed which can tolerate and enriched heavy metals was found in the pollution area. The results showed that the lead concentration of duckweed was 39.4 mg x kg(-1). XANES analysis and linear combination fit indicated that lead stearate and lead sulfide accounted for 65% and 36.9% respectively in the lead speciation of duckweed, suggesting that the main lead speciation of duckweed was sulfur-containing lead-organic acid.

  12. Vanadium speciation by chromatographic separation of V(IV) and V ...

    African Journals Online (AJOL)

    A new method for vanadium speciation has been developed. The method is based on chromatographic separation of vanadium(IV) and vanadium(V) in acidic medium followed by the determination with ICP-OES. Vanadium species exist in acidic solution (pH < 3) as VO2+ for vanadium(IV) and VO2 + for vanadium(V).

  13. Optimization of parameters for the synthesis of Y{sub 2}Cu{sub 2}O{sub 5} nanoparticles by Taguchi method and comparison of their magnetic and optical properties with their bulk counterpart

    Energy Technology Data Exchange (ETDEWEB)

    Farbod, Mansoor, E-mail:; Rafati, Zahra; Shoushtari, Morteza Zargar


    Y{sub 2}Cu{sub 2}O{sub 5} nanoparticles were synthesized by sol–gel combustion method and effects of different factors on the size of nanoparticles were investigated. In order to reduce the experimental stages, Taguchi robust design method was employed. Acid citric:Cu{sup +2} M ratio, pH, sintering temperature and time were chosen as the parameters for optimization. Among these factors the solution pH had the most influence and the others had nearly the same influence on the nanoparticles sizes. Based on the predicted conditions by Taguchi design, the sample with a minimum particle size of 47 nm was prepared. The magnetic behavior of Y{sub 2}Cu{sub 2}O{sub 5} nanoparticles were measured and found that at low fields they are soft ferromagnetic but at high fields they behave paramagnetically. The magnetic behavior of nanoparticles were compared to their bulk counterparts and found that the M{sub r} of the samples was slightly different, but the H{sub c} of the nanoparticles was 76% of the bulk sample. The maximum absorbance peak of UV–vis spectrum showed a blue shift for the smaller particles. - Highlights: • Y{sub 2}Cu{sub 2}O{sub 5} nanoparticles (Y202) were synthesized by sol–gel combustion method. • To optimize the synthesis parameters Taguchi statistical method was used. • The solution pH had the most influence and the others had nearly the same effect. • The hysteresis loop of (Y202) nanoparticles showed a soft ferromagnetic behavior. • UV maximum absorbance peak showed a blue shift for the nanoparticle.

  14. Development of superconductor bulk for superconductor bearing

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Chan Joong; Jun, Byung Hyuk; Park, Soon Dong (and others)


    Current carrying capacity is one of the most important issues in the consideration of superconductor bulk materials for engineering applications. There are numerous applications of Y-Ba-Cu-O (YBCO) bulk superconductors e.g. magnetic levitation train, flywheel energy storage system, levitation transportation, lunar telescope, centrifugal device, magnetic shielding materials, bulk magnets etc. Accordingly, to obtain YBCO materials in the form of large, single crystals without weak-link problem is necessary. A top seeded melt growth (TSMG) process was used to fabricate single crystal YBCO bulk superconductors. The seeded and infiltration growth (IG) technique was also very promising method for the synthesis of large, single-grain YBCO bulk superconductors with good superconducting properties. 5 wt.% Ag doped Y211 green compacts were sintered at 900 .deg. C {approx} 1200 .deg.C and then a single crystal YBCO was fabricated by an infiltration method. A refinement and uniform distribution of the Y211 particles in the Y123 matrix were achieved by sintering the Ag-doped samples. This enhancement of the critical current density was ascribable to a fine dispersion of the Y211 particles, a low porosity and the presence of Ag particles. In addition, we have designed and manufactured large YBCO single domain with levitation force of 10-13 kg/cm{sup 2} using TSMG processing technique.

  15. An experimental design approach for optimization of spectrophotometric method for estimation of cefixime trihydrate using ninhydrin as derivatizing reagent in bulk and pharmaceutical formulation


    Yogita B. Wani; Dipak D. Patil


    The aim of the present work is to use experimental design to screen and optimize experimental variables for developing a spectrophotometric method for determining cefixime trihydrate content using ninhydrin as a derivatizing reagent. The method is based on the reaction of the amino group of cefixime with ninhydrin in an alkaline medium to form a yellow-colored derivative (λmax 436 nm). A two-level full factorial design was utilized to screen the effect of ninhydrin reagent concentration (X1),...

  16. Development and Validation of a Stability-Indicating HPTLC Method for Analysis of Rasagiline Mesylate in the Bulk Drug and Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    Singaram Kathirvel


    Full Text Available A simple and sensitive thin-layer chromatographic method has been established for analysis of rasagiline mesylate in pharmaceutical dosage form. Chromatography on silica gel 60 F254 plates with 6 : 1 : 2(v/v/v butanol-methanol water as mobile phase furnished compact spots at Rf  0.76±0.01. Densitometric analysis was performed at 254 nm. To show the specificity of the method, rasagiline mesylate was subjected to acid, base, neutral hydrolysis, oxidation, photolysis, and thermal decomposition, and the peaks of degradation products were well resolved from that of the pure drug. Linear regression analysis revealed a good linear relationship between peak area and amount of rasagiline mesylate in the range of 100–350 ng/band. The minimum amount of rasagiline mesylate that could be authentically detected and quantified was 11.12 and 37.21 ng/band, respectively. The method was validated, in accordance with ICH guidelines for precision, accuracy, and robustness. Since the method could effectively separate the drug from its degradation products, it can be regarded as stability indicating.

  17. RP-HPLC Method Development and Validation for the Determination and Stability Indicative Studies of Montelukast in Bulk and its Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    A. Patnaik


    Full Text Available A simple, precise, accurate, economical and reproducible HPLC method for estimation of montelukast in tablet dosage form has been developed. Quantitative HPLC was performed with Shimadzu LC2010c HT with Winchrom Software with UV-Visible detector (SPD-IOA, PUMP (LC-IOAT and (LC-IOATvp. Phenomenex C8, 5 μm, 25 cm × 4.6 mm i.d. column was used in the study. The mobile phase of ACN: Acetate buffer= 6.5:3.5 of pH 3 were used in this study. The conditions optimized were: flow rate (1 mL/minute, wavelength (222 nm and run time was 20 min. Retention time was found to be 3.08 min. The linearity was found to be in the concentration range of 10-100 μg/mL. The developed method was evaluated in the assay of commercially available tablet moni containing 10 mg of montelukast. The amount of drug in tablet was found to be 10.34 mg/tab for the brand. Results of analysis were validated statistically and by recovery studies. The recovery studies 99.67% was indicative of the accuracy of proposed method. The precision was calculated as repeatability, inter and intraday variation (%RSD for the drug. By using the method, stability of the drug has been studied.

  18. Factors Controlling Redox Speciation of Plutonium and Neptunium in Extraction Separation Processes

    Energy Technology Data Exchange (ETDEWEB)

    Paulenova, Alena [Principal Investigator; Vandegrift, III, George F. [Collaborator


    The objective of the project was to examine the factors controlling redox speciation of plutonium and neptunium in UREX+ extraction in terms of redox potentials, redox mechanism, kinetics and thermodynamics. Researchers employed redox-speciation extractions schemes in parallel to the spectroscopic experiments. The resulting distribution of redox species w studied uring spectroscopic, electrochemical, and spectro-electrochemical methods. This work reulted in collection of data on redox stability and distribution of redox couples in the nitric acid/nitrate electrolyte and the development of redox buffers to stabilize the desired oxidation state of separated radionuclides. The effects of temperature and concentrations on the redox behavior of neptunium were evaluated.

  19. A review on speciation of iodine-129 in the environmental and biological samples

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Hansen, Violeta; Aldahan, Ala


    plants, the I-129/I-127 ratios have being reached to values of 10(-10) to 10(-4) in the environment from 10(-12) in the pre-nuclear era. In this article, we review the occurrence, sources, inventory, and concentration level of I-129 in environment and the method for speciation analysis of I-129...... in the environment. Measurement techniques for the determination of I-129 are presented and compared. An overview of applications of I-129 speciation in various scientific disciplines such as radiation protection, waste depository, and environmental sciences is given. In addition, the bioavailability and radiation...

  20. Magic cues versus magic preferences in speciation

    NARCIS (Netherlands)

    Maan, Martine E.; Seehausen, Ole

    Question: How does divergent natural selection lead to divergence in mating traits and the evolution of reproductive isolation? Background: Ecological speciation of non-allopatric taxa usually requires the evolution of an association between selective mating and the traits underlying ecological

  1. Behavioural reproductive isolation and speciation in Drosophila

    Indian Academy of Sciences (India)

    The origin of premating reproductive isolation continues to help elucidate the process of speciation and is the central event in the evolution of biological species. Therefore, during the process of species formation the diverging populations must acquire some means of reproductive isolation so that the genes from one gene ...

  2. Characterization of Technetium Speciation in Cast Stone

    Energy Technology Data Exchange (ETDEWEB)

    Um, Wooyong; Jung, Hun Bok; Wang, Guohui; Westsik, Joseph H.; Peterson, Reid A.


    This report describes the results from laboratory tests performed at Pacific Northwest National Laboratory (PNNL) for the U.S. Department of Energy (DOE) EM-31 Support Program (EMSP) subtask, “Production and Long-Term Performance of Low Temperature Waste Forms” to provide additional information on technetium (Tc) speciation characterization in the Cast Stone waste form. To support the use of Cast Stone as an alternative to vitrification for solidifying low-activity waste (LAW) and as the current baseline waste form for secondary waste streams at the Hanford Site, additional understanding of Tc speciation in Cast Stone is needed to predict the long-term Tc leachability from Cast Stone and to meet the regulatory disposal-facility performance requirements for the Integrated Disposal Facility (IDF). Characterizations of the Tc speciation within the Cast Stone after leaching under various conditions provide insights into how the Tc is retained and released. The data generated by the laboratory tests described in this report provide both empirical and more scientific information to increase our understanding of Tc speciation in Cast Stone and its release mechanism under relevant leaching processes for the purpose of filling data gaps and to support the long-term risk and performance assessments of Cast Stone in the IDF at the Hanford Site.

  3. Electrochemical metal speciation in colloidal dispersions

    NARCIS (Netherlands)

    Wonders, J.H.A.M.


    The term "heavy metals" is connected with toxicity. They form strong complexes with enzymes, other proteins and DNA in living organisms, which causes dysfunctioning and hence poisoning. In combination with the uptake mechanism of the organism, speciation of heavy metal determines the

  4. Biogeochemical speciation of Fe in ocean water

    NARCIS (Netherlands)

    Hiemstra, T.; Riemsdijk, van W.H.


    The biogeochemical speciation of Fe in seawater has been evaluated using the consistent Non-Ideal Competitive Adsorption model (NICA¿Donnan model). Two types of data sets were used, i.e. Fe-hydroxide solubility data and competitive ligand equilibration/cathodic stripping voltammetry (CLE/CSV) Fe

  5. Behavioural reproductive isolation and speciation in Drosophila

    Indian Academy of Sciences (India)


    Mar 29, 2012 ... somes, DNA sequence and hybrid sterility showed that. D. simulans and D. mauritiana are more closely .... DNA including microsatellites) to study population ge- netic structure and incipient speciation in this ...... in the grasshopper Chorthippus parallelus. Evolution 54. 1687–1698. Trickett AJ and Butlin RK ...

  6. Integration of bulk piezoelectric materials into microsystems (United States)

    Aktakka, Ethem Erkan

    Bulk piezoelectric ceramics, compared to deposited piezoelectric thin-films, provide greater electromechanical coupling and charge capacity, which are highly desirable in many MEMS applications. In this thesis, a technology platform is developed for wafer-level integration of bulk piezoelectric substrates on silicon, with a final film thickness of 5-100microm. The characterized processes include reliable low-temperature (200°C) AuIn diffusion bonding and parylene bonding of bulk-PZT on silicon, wafer-level lapping of bulk-PZT with high-uniformity (+/-0.5microm), and low-damage micro-machining of PZT films via dicing-saw patterning, laser ablation, and wet-etching. Preservation of ferroelectric and piezoelectric properties is confirmed with hysteresis and piezo-response measurements. The introduced technology offers higher material quality and unique advantages in fabrication flexibility over existing piezoelectric film deposition methods. In order to confirm the preserved bulk properties in the final film, diaphragm and cantilever beam actuators operating in the transverse-mode are designed, fabricated and tested. The diaphragm structure and electrode shapes/sizes are optimized for maximum deflection through finite-element simulations. During tests of fabricated devices, greater than 12microm PP displacement is obtained by actuation of a 1mm2 diaphragm at 111kHz with sleep-mode (simulated). Under lg vibration at 155Hz, a 70mF ultra-capacitor is charged from OV to 1.85V in 50 minutes.

  7. Selenium Metabolism in Cancer Cells: The Combined Application of XAS and XFM Techniques to the Problem of Selenium Speciation in Biological Systems

    Directory of Open Access Journals (Sweden)

    Hugh H. Harris


    Full Text Available Determining the speciation of selenium in vivo is crucial to understanding the biological activity of this essential element, which is a popular dietary supplement due to its anti-cancer properties. Hyphenated techniques that combine separation and detection methods are traditionally and effectively used in selenium speciation analysis, but require extensive sample preparation that may affect speciation. Synchrotron-based X-ray absorption and fluorescence techniques offer an alternative approach to selenium speciation analysis that requires minimal sample preparation. We present a brief summary of some key HPLC-ICP-MS and ESI-MS/MS studies of the speciation of selenium in cells and rat tissues. We review the results of a top-down approach to selenium speciation in human lung cancer cells that aims to link the speciation and distribution of selenium to its biological activity using a combination of X-ray absorption spectroscopy (XAS and X-ray fluorescence microscopy (XFM. The results of this approach highlight the distinct fates of selenomethionine, methylselenocysteine and selenite in terms of their speciation and distribution within cells: organic selenium metabolites were widely distributed throughout the cells, whereas inorganic selenium metabolites were compartmentalized and associated with copper. New data from the XFM mapping of electrophoretically-separated cell lysates show the distribution of selenium in the proteins of selenomethionine-treated cells. Future applications of this top-down approach are discussed.

  8. Speciation analysis of 129I and its applications in environmental research

    DEFF Research Database (Denmark)

    Zhang, Luyuan; Hou, Xiaolin


    been reported for speciation analysis of 129I in a variety of environmental samples. These methods have been applied in many researches, including conversion processes of iodine species in marine and terrestrial systems, migration and retention of iodine in soil and sediment, geochemical cycling...

  9. Introduction to the EU-network on trace element speciation: preparing for the 21(st) century

    DEFF Research Database (Denmark)

    Cornelis, R.; Camara, C.; Ebdon, L.


    The main objective of the EU-network is to bring together scientists with a background in analytical chemistry interested in speciation method development with potential users from industry and representatives from legislative bodies. The network started on 1/10/1997 for a duration of 2 years. A ...

  10. Foliar or root exposures to smelter particles: Consequences for lead compartmentalization and speciation in plant leaves

    Energy Technology Data Exchange (ETDEWEB)

    Schreck, Eva [Université de Toulouse, INP, UPS, EcoLab (Laboratoire Ecologie Fonctionnelle et Environnement), ENSAT, Avenue de l' Agrobiopole, 31326 Castanet-Tolosan (France); CNRS, EcoLab, 31326 Castanet-Tolosan (France); Géosciences Environnement Toulouse (GET), Observatoire Midi Pyrénées, Université de Toulouse, CNRS, IRD, 14 Avenue E. Belin, F-31400 Toulouse (France); Dappe, Vincent [LASIR (UMR CNRS 8516), Université de Lille 1, Bât. C5, 59655 Villeneuve d' Ascq Cedex (France); Sarret, Géraldine [ISTerre, UMR 5275, Université Grenoble I, CNRS, F-38041 Grenoble (France); Sobanska, Sophie [LASIR (UMR CNRS 8516), Université de Lille 1, Bât. C5, 59655 Villeneuve d' Ascq Cedex (France); Nowak, Dorota; Nowak, Jakub; Stefaniak, Elżbieta Anna [Department of Chemistry, John Paul II Catholic University of Lublin, Al. Kraśnicka 102, 20-718 Lublin (Poland); Magnin, Valérie [ISTerre, UMR 5275, Université Grenoble I, CNRS, F-38041 Grenoble (France); Ranieri, Vincent [CEA-INAC, 17 rue des Martyrs, 38054 Grenoble Cedex 9 (France); Dumat, Camille, E-mail: [Université de Toulouse, INP, UPS, EcoLab (Laboratoire Ecologie Fonctionnelle et Environnement), ENSAT, Avenue de l' Agrobiopole, 31326 Castanet-Tolosan (France); CNRS, EcoLab, 31326 Castanet-Tolosan (France)


    In urban areas with high fallout of airborne particles, metal uptake by plants mainly occurs by foliar pathways and can strongly impact crop quality. However, there is a lack of knowledge on metal localization and speciation in plants after pollution exposure, especially in the case of foliar uptake. In this study, two contrasting crops, lettuce (Lactuca sativa L.) and rye-grass (Lolium perenne L.), were exposed to Pb-rich particles emitted by a Pb-recycling factory via either atmospheric or soil application. Pb accumulation in plant leaves was observed for both ways of exposure. The mechanisms involved in Pb uptake were investigated using a combination of microscopic and spectroscopic techniques (electron microscopy, laser ablation, Raman microspectroscopy, and X-ray absorption spectroscopy). The results show that Pb localization and speciation are strongly influenced by the type of exposure (root or shoot pathway) and the plant species. Foliar exposure is the main pathway of uptake, involving the highest concentrations in plant tissues. Under atmospheric fallouts, Pb-rich particles were strongly adsorbed on the leaf surface of both plant species. In lettuce, stomata contained Pb-rich particles in their apertures, with some deformations of guard cells. In addition to PbO and PbSO{sub 4}, chemical forms that were also observed in pristine particles, new species were identified: organic compounds (minimum 20%) and hexagonal platy crystals of PbCO{sub 3}. In rye-grass, the changes in Pb speciation were even more egregious: Pb–cell wall and Pb–organic acid complexes were the major species observed. For root exposure, identified here as a minor pathway of Pb transfer compared to foliar uptake, another secondary species, pyromorphite, was identified in rye-grass leaves. Finally, combining bulk and spatially resolved spectroscopic techniques permitted both the overall speciation and the minor but possibly highly reactive lead species to be determined in order to

  11. Speciation of Cu in a Contaminated Agricultural Soil Measured By XAFS, Mu-XAFS, And Mu-XRF

    Energy Technology Data Exchange (ETDEWEB)

    Strawn, D.G.; Baker, L.L.


    Contamination of agricultural soils with Cu as a result of fungicide application and spills threatens environmental quality and reduces soil quality for crop growth. In this paper advanced spectroscopic and microscopic methods were used to elucidate the Cu speciation in a calcareous soil contaminated since the 1940s. Microscopically focused synchrotron-based XRF ({mu}-SXRF) was used to map the elemental distribution in the soils. Results indicated that most of the Cu was not associated with metal oxides, silicates, phosphates, or carbonates. Bulk and microscopically focused X-absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectra indicated that the Cu in the soil was predominantly Cu adsorbed on soil organic matter (SOM). Interpretation of the fitting results suggests that the Cu is complexed to SOM via bidentate inner-sphere coordination with carboxyl or amine ligands. Results presented in this paper provide detailed information on the molecular coordination of Cu in a contaminated soil. Such information is critical for understanding the long-term fate and best management practices for Cu in the environment.

  12. Lineage divergence and speciation in the Web-toed Salamanders (Plethodontidae: Hydromantes) of the Sierra Nevada, California. (United States)

    Rovito, Sean M


    Peripatric speciation and the importance of founder effects have long been controversial, and multilocus sequence data and coalescent methods now allow hypotheses of peripatric speciation to be tested in a rigorous manner. Using a multilocus phylogeographical data set for two species of salamanders (genus Hydromantes) from the Sierra Nevada of California, hypotheses of recent divergence by peripatric speciation and older, allopatric divergence were tested. Phylogeographical analysis revealed two divergent lineages within Hydromantes platycephalus, which were estimated to have diverged in the Pliocene. By contrast, a low-elevation species, Hydromantes brunus, diverged from within the northern lineage of H. platycephalus much more recently (mid-Pleistocene), during a time of major climatic change in the Sierra Nevada. Multilocus species tree estimation and coalescent estimates of divergence time, migration rate, and growth rate reject a scenario of ancient speciation of H. brunus with subsequent gene flow and introgression from H. platycephalus, instead supporting a more recent divergence with population expansion. Although the small, peripheral distribution of H. brunus suggests the possibility of peripatric speciation, the estimated founding population size of the species was too large to have allowed founder effects to be important in its divergence. These results provide evidence for both recent speciation, most likely tied to the climatic changes of the Pleistocene, and older lineage divergence, possibly due to geological events, and add to evidence that Pleistocene glacial cycles were an important driver of diversification in the Sierra Nevada. © 2010 Blackwell Publishing Ltd.

  13. Polonium bulk and surface vibrational dynamics

    Energy Technology Data Exchange (ETDEWEB)

    Tigrine, Rachid; Bourahla, Boualem [Laboratoire de Physique PEC UMR 6087, Universite du Maine, Le Mans (France); Laboratoire de Physique et Chimie Quantique, Universite de Tizi Ouzou (Algeria); Khater, Antoine


    Calculations are presented for the bulk phonons and for surface Rayleigh phonons and resonances for Polonium, the only element known to form in the simple cubic lattice. The static stability of this lattice has been confirmed recently by ab initio simulations which yield two bulk elastic constants, c{sub 11} and c{sub 12}. Constitutive equations are derived for the isotropic cubic lattice based upon the Fuchs's method. This permits effectively a numerical evaluation of central potential force constants for Polonium from the ab initio results. Numerical calculations are then made for the material vibration dynamics in the force constant model with the use of the matching method. The numerical applications yield for Polonium the bulk phonon branches along[100],[110], and [111], and the Rayleigh phonons and surface resonances along the[010] direction in an unreconstructed (001) surface. The local vibration densities of states are calculated for bulk and surface sites for this element. (copyright 2009 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  14. Simulation-integrated Design of Dry Bulk Terminals

    NARCIS (Netherlands)

    Van Vianen, T.A.


    To meet the expected increase of seaborne trade flows for coal and iron ore dry bulk terminals need to be designed or expanded. A comprehensive design method for dry bulk terminals is missing. Designs are currently based on rules-of-thumb, practical experiences and average values for specific design

  15. Bulk modulus of metals according to structureless pseudopotential ...

    African Journals Online (AJOL)

    structureless pseudopotential model was fully developed. The developed method was used to calculate the bulk modulus and kinetic energy contribution to the bulk modulus of 46 elemental metals. The results obtained were compared with experimental values and their variation with electron density parameter was studied ...

  16. Sulfur and iron speciation in gas-rich impact-melt glasses from basaltic shergottites determined by microXANES

    Energy Technology Data Exchange (ETDEWEB)

    Sutton, S.R.; Rao, M.N.; Nyquist, L.E. (UofC); (Johnson Space Center)


    Sulfur and iron K XANES measurements were made on GRIM glasses from EET 79001. Iron is in the ferrous state. Sulfur speciation is predominately sulfide coordination but is Fe coordinated in Lith B and, most likely, Ca coordinated in Lith A. Sulfur is abundantly present as sulfate near Martian surface based on chemical and mineralogical investigations on soils and rocks in Viking, Pathfinder and MER missions. Jarosite is identified by Moessbauer studies on rocks at Meridian and Gusev, whereas MgSO{sub 4} is deduced from MgO-SO{sub 3} correlations in Pathfinder MER and Viking soils. Other sulfate minerals such as gypsum and alunogen/S-rich aluminosilicates and halides are detected only in martian meteorites such as shergottites and nakhlites using SEM/FE-SEM and EMPA techniques. Because sulfur has the capacity to occur in multiple valence states, determination of sulfur speciation (sulfide/sulfate) in secondary mineral assemblages in soils and rocks near Mars surface may help us understand whether the fluid-rock interactions occurred under oxidizing or reducing conditions. On Earth, volcanic rocks contain measurable quantities of sulfur present as both sulfide and sulfate. Carroll and Rutherford showed that oxidized forms of sulfur may comprise a significant fraction of total dissolved sulfur, if the oxidation state is higher than {approx}2 log fO{sub 2} units relative to the QFM buffer. Terrestrial samples containing sulfates up to {approx}25% in fresh basalts from the Galapagos Rift on one hand and high sulfide contents present in oceanic basalts on the other indicate that the relative abundance of sulfide and sulfate varies depending on the oxygen fugacity of the system. Basaltic shergottites (bulk) such as Shergotty, EET79001 and Zagami usually contain small amounts of sulfur ({approx}0.5%) as pyrrhotite. But, in isolated glass pockets containing secondary salts (known as GRIM glasses) in these meteorites, sulfur is present in high abundance ({approx}1-12%). To

  17. Radiation effects in bulk silicon (United States)

    Claeys, Cor; Vanhellemont, Jan


    This paper highlights important aspects related to irradiation effects in bulk silicon. Some basic principles related to the interaction of radiation with material, i.e. ionization and atomic displacement, are briefly reviewed. A physical understanding of radiation effects strongly depends on the availability of appropriate analytical tools. These tools are critically accessed from a silicon bulk viewpoint. More detailed information, related to the properties of the bulk damage and some dedicated application aspects, is given for both electron and proton irradiations. Emphasis is placed on radiation environments encountered during space missions and on their influence on the electrical performance of devices such as memories and image sensors.

  18. Speciation of Sulfur in Biochar Produced from Pyrolysis and Gasification of Oak and Corn Stover (United States)


    The effects of feedstock type and biomass conversion conditions on the speciation of sulfur in biochars are not well-known. In this study, the sulfur content and speciation in biochars generated from pyrolysis and gasification of oak and corn stover were determined. We found the primary determinant of the total sulfur content of biomass to be the feedstock from which the biochar is generated, with oak and corn stover biochars containing 160 and 600–800 ppm sulfur, respectively. In contrast, for sulfur speciation, we found the primary determinant to be the temperature combined with the thermochemical conversion method. The speciation of sulfur in biochars was determined using X-ray absorption near-edge structure (XANES), ASTM method D2492, and scanning electron microscopy–energy-dispersive spectroscopy (SEM–EDS). Biochars produced under pyrolysis conditions at 500–600 °C contain sulfate, organosulfur, and sulfide. In some cases, the sulfate contents are up to 77–100%. Biochars produced in gasification conditions at 850 °C contain 73–100% organosulfur. The increase of the organosulfur content as the temperature of biochar production increases suggests a similar sulfur transformation mechanism as that in coal, where inorganic sulfur reacts with hydrocarbon and/or H2 to form organosulfur when the coal is heated. EDS mapping of a biochar produced from corn stover pyrolysis shows individual sulfur-containing mineral particles in addition to the sulfur that is distributed throughout the organic matrix. PMID:25003702

  19. The genetics of speciation by reinforcement.

    Directory of Open Access Journals (Sweden)

    Daniel Ortiz-Barrientos


    Full Text Available Reinforcement occurs when natural selection strengthens behavioral discrimination to prevent costly interspecies matings, such as when matings produce sterile hybrids. This evolutionary process can complete speciation, thereby providing a direct link between Darwin's theory of natural selection and the origin of new species. Here, by examining a case of speciation by reinforcement in Drosophila,we present the first high-resolution genetic study of variation within species for female mating discrimination that is enhanced by natural selection. We show that reinforced mating discrimination is inherited as a dominant trait, exhibits variability within species, and may be influenced by a known set of candidate genes involved in olfaction. Our results show that the genetics of reinforced mating discrimination is different from the genetics of mating discrimination between species, suggesting that overall mating discrimination might be a composite phenomenon, which in Drosophila could involve both auditory and olfactory cues. Examining the genetics of reinforcement provides a unique opportunity for both understanding the origin of new species in the face of gene flow and identifying the genetic basis of adaptive female species preferences, two major gaps in our understanding of speciation.

  20. Arsenic speciation and sorption in natural environments (United States)

    Campbell, Kate M.; Nordstrom, D. Kirk


    Aqueous arsenic speciation, or the chemical forms in which arsenic exists in water, is a challenging, interesting, and complicated aspect of environmental arsenic geochemistry. Arsenic has the ability to form a wide range of chemical bonds with carbon, oxygen, hydrogen, and sulfur, resulting in a large variety of compounds that exhibit a host of chemical and biochemical properties. Besides the intriguing chemical diversity, arsenic also has the rare capacity to capture our imaginations in a way that few elements can duplicate: it invokes images of foul play that range from sinister to comedic (e.g., “inheritance powder” and arsenic-spiked elderberry wine). However, the emergence of serious large-scale human health problems from chronic arsenic exposure in drinking water has placed a high priority on understanding environmental arsenic mobility, toxicity, and bioavailability, and chemical speciation is key to these important questions. Ultimately, the purpose of arsenic speciation research is to predict future occurrences, mitigate contamination, and provide successful management of water resources.

  1. Silicon Bulk Micromachined Vibratory Gyroscope (United States)

    Tang, T. K.; Gutierrez, R. C.; Wilcox, J. Z.; Stell, C.; Vorperian, V.; Calvet, R.; Li, W. J.; Charkaborty, I.; Bartman, R.; Kaiser, W. J.


    This paper reports on design, modeling, fabrication, and characterization of a novel silicon bulk micromachined vibratory rate gyroscope designed for microspacecraft applications. The new microgyroscope consists of a silicon four leaf cloverstructure with a post attached to the center.

  2. Proceedings of BulkTrans '89

    Energy Technology Data Exchange (ETDEWEB)


    Papers were presented on bulk commodity demand; steel industry bulk trades; grains and the world food economy; steam coal and cement demand; shipping profitability; bulk carrier design and economics; bulk ports and terminals; ship unloading; computers in bulk terminals; and conveyors and stockyard equipment.

  3. Combatting bulking sludge with ultrasound

    Energy Technology Data Exchange (ETDEWEB)

    Wuensch, B.; Heine, W.; Neis, U. [Technische Univ. Hamburg-Harburg, Hamburg (Germany). Dept. of Sanitary and Environmental Engineering


    Bulking and floating sludge cause great problems in many waste water treatment plants with biological nutrient removal. The purification as well as the sludge digestion process can be affected. These problems are due to the interlaced structure of filamentous microorganisms, which have an impact on the sludge's settling behaviour. Foam is able to build up a stable layer, which does not settle in the secondary clarifier. Foam in digestion causes a reduction of the degree of stabilisation and of the biogas production. We use low-frequency ultrasound to combat filamentous organisms in bulking sludge. Low-frequency ultrasound is suitable to create high local shear stresses, which are capable of breaking the filamentous structures of the sludge. After preliminary lab-scale tests now a full-scale new ultrasound equipment is operating at Reinfeld sewage treatment plant, Germany. The objective of this study is to explore the best ultrasound configuration to destroy the filamentous structure of bulking and foaming sludge in a substainable way. Later this study will also look into the effects of ultrasound treated bulking sludge on the anaerobic digestion process. Up to now results show that the settling behaviour of bulking sludge is improved. The minimal ultrasound energy input for destruction of bulking structure was determined. (orig.)

  4. Chromium speciation in solid matrices and regulation: a review

    Energy Technology Data Exchange (ETDEWEB)

    Unceta, N. [University of the Basque Country, Department of Analytical Chemistry, Faculty of Pharmacy, Vitoria-Gasteiz (Spain); Seby, F. [Ultra Traces Analyses Aquitaine (UT2A), Helioparc Pau-Pyrenees, Pau (France); Malherbe, J.; Donard, O.F.X. [Universite de Pau et des Pays de l' Adour, Helioparc Pau-Pyrenees, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, IPREM, UMR CNRS 5254, Pau (France)


    In recent years, the extensive use of chromium in industrial processes has led to the promotion of several directives and recommendations by the European Union, that try to limit and regulate the presence of Cr(VI) in the environment and to protect industrial workers using chromium and end-users of manufactured products. As a consequence, new standard methods and analytical procedures have been published at the EU level for Cr(VI) determination in soil, sludge, sediment, and similar waste materials, workplace atmospheres, cement, packaging materials, industrially produced samples, and corrosion-protection layers on some components of vehicles and electrical and electronic equipment. The objective of this article is to summarize the different directives and recommendations and to critically review the currently existing standard methods and the methods published in the literature for chromium speciation in the above mentioned solid matrices, putting the emphasis on the different extraction procedures which have been developed for each matrix. Particular attention has been paid to Cr(III) and Cr(VI) inter-conversions that can occur during extraction and efforts to minimize these unwanted reactions. Although the use of NaOH-Na{sub 2}CO{sub 3} solutions with hot plate extraction seems to be the more widespread procedure, species transformation can still occur and several studies suggest that speciated isotope-dilution mass spectrometry (SIDMS) could be a suitable tool for correction of these interconversions. Besides, recent studies have proved the role of Cr(III) in chromium toxicology. As a consequence, the authors suggest an update of standard methods in the near future. (orig.)

  5. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt


    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination...... of 1300 W. The limit of detection achieved under these conditions was 1 mu g L-1 (100 mu L injections). The HPLC-ICP-MS system was used for selenium speciation of selenite and selenate in aqueous solutions during a BCR certification exercise and for selenium speciation in the certified reference material...

  6. Method and Apparatus of Measuring Velocity and Sound Attenuation Coefficient in Bulk Materials Based on the Analysis of the Structure of Sound-Insulation Materials on the Basis of Perlite (United States)

    Kapranov, B. I.; Mashanov, A. P.


    This paper presents the results of research and describes the apparatus for measuring the acoustic characteristics of bulk materials. Ultrasound, it has passed through a layer of bulk material, is further passes through an air gap. The presence of air gap prevents from measuring tract mechanical contacts, but complicates the measurement technology Studies were conducted on the example of measuring the acoustic characteristics of the widely used perlite-based sound-proofing material.

  7. Speciation of organic aerosols in the Saharan Air Layer and in the free troposphere westerlies

    Directory of Open Access Journals (Sweden)

    M. I. García


    Full Text Available We focused this research on the composition of the organic aerosols transported in the two main airflows of the subtropical North Atlantic free troposphere: (i the Saharan Air Layer – the warm, dry and dusty airstream that expands from North Africa to the Americas at subtropical and tropical latitudes – and (ii the westerlies, which flow from North America over the North Atlantic at mid- and subtropical latitudes. We determined the inorganic compounds (secondary inorganic species and elemental composition, elemental carbon and the organic fraction (bulk organic carbon and organic speciation present in the aerosol collected at Izaña Observatory,  ∼  2400 m a.s.l. on the island of Tenerife. The concentrations of all inorganic and almost all organic compounds were higher in the Saharan Air Layer than in the westerlies, with bulk organic matter concentrations within the range 0.02–4.0 µg m−3. In the Saharan Air Layer, the total aerosol population was by far dominated by dust (93 % of bulk mass, which was mixed with secondary inorganic pollutants ( <  5 % and organic matter ( ∼  1.5 %. The chemical speciation of the organic aerosols (levoglucosan, dicarboxylic acids, saccharides, n-alkanes, hopanes, polycyclic aromatic hydrocarbons and those formed after oxidation of α-pinene and isoprene, determined by gas chromatography coupled with mass spectrometry accounted for 15 % of the bulk organic matter (determined by the thermo-optical transmission technique; the most abundant organic compounds were saccharides (associated with surface soils, secondary organic aerosols linked to oxidation of biogenic isoprene (SOA ISO and dicarboxylic acids (linked to several primary sources and SOA. When the Saharan Air Layer shifted southward, Izaña was within the westerlies stream and organic matter accounted for  ∼  28 % of the bulk mass of aerosols. In the westerlies, the organic aerosol species determined

  8. Modelling of bulk superconductor magnetization (United States)

    Ainslie, M. D.; Fujishiro, H.


    This paper presents a topical review of the current state of the art in modelling the magnetization of bulk superconductors, including both (RE)BCO (where RE = rare earth or Y) and MgB2 materials. Such modelling is a powerful tool to understand the physical mechanisms of their magnetization, to assist in interpretation of experimental results, and to predict the performance of practical bulk superconductor-based devices, which is particularly important as many superconducting applications head towards the commercialization stage of their development in the coming years. In addition to the analytical and numerical techniques currently used by researchers for modelling such materials, the commonly used practical techniques to magnetize bulk superconductors are summarized with a particular focus on pulsed field magnetization (PFM), which is promising as a compact, mobile and relatively inexpensive magnetizing technique. A number of numerical models developed to analyse the issues related to PFM and optimise the technique are described in detail, including understanding the dynamics of the magnetic flux penetration and the influence of material inhomogeneities, thermal properties, pulse duration, magnitude and shape, and the shape of the magnetization coil(s). The effect of externally applied magnetic fields in different configurations on the attenuation of the trapped field is also discussed. A number of novel and hybrid bulk superconductor structures are described, including improved thermal conductivity structures and ferromagnet-superconductor structures, which have been designed to overcome some of the issues related to bulk superconductors and their magnetization and enhance the intrinsic properties of bulk superconductors acting as trapped field magnets. Finally, the use of hollow bulk cylinders/tubes for shielding is analysed.

  9. Kinetic and thermodynamic determinants of trace metal partitioning at biointerphases: the role of intracellular speciation dynamics. (United States)

    Duval, Jérôme F L; Présent, Romain M; Rotureau, Elise


    There is a large body of work evidencing the necessity to evaluate chemical speciation dynamics of trace metals in solution for an accurate definition of their bioavailability to microorganisms. In contrast, the integration of intracellular metal speciation dynamics in biouptake formalisms is still in its early stages. Accordingly, we elaborate here a rationale for the interplay between chemodynamics of intracellular metal complexes and dynamics of processes governing metal biouptake under non-complexing outer medium conditions. These processes include the conductive diffusion of metal ions to the charged soft biointerphase, metal internalisation, excretion of intracellular free metal species and metal depletion from bulk solution. The theory is formulated from Nernst-Planck equations corrected for electrostatic and reaction kinetic terms applied at the biosurface and in the intracellular volume. Computational illustrations demonstrate how biointerfacial metal distribution dynamics inherently reflects the chemodynamic properties of intracellular complexes. In the practical limits of high and weak metal affinity to biosurface internalisation sites, the metal concentration profile is explicitly solved under conditions of strong intracellular complexing agents. Exact analytical expression is further developed for metal partitioning at equilibrium. This provides a way to evaluate the metal biopartition coefficient from refined analysis of bulk metal depletion measured at various cell concentrations. Depending on here-defined dimensionless parameters involving rates of metal internalisation-excretion and complex formation, the formalism defines the nature of the different kinetic regimes governing bulk metal depletion and biouptake. In particular, the conditions leading to an internalisation flux limited by diffusion as a result of demanding intracellular metal complexation are identified.

  10. Phylogenies reveal new interpretation of speciation and the Red Queen. (United States)

    Venditti, Chris; Meade, Andrew; Pagel, Mark


    The Red Queen describes a view of nature in which species continually evolve but do not become better adapted. It is one of the more distinctive metaphors of evolutionary biology, but no test of its claim that speciation occurs at a constant rate has ever been made against competing models that can predict virtually identical outcomes, nor has any mechanism been proposed that could cause the constant-rate phenomenon. Here we use 101 phylogenies of animal, plant and fungal taxa to test the constant-rate claim against four competing models. Phylogenetic branch lengths record the amount of time or evolutionary change between successive events of speciation. The models predict the distribution of these lengths by specifying how factors combine to bring about speciation, or by describing how rates of speciation vary throughout a tree. We find that the hypotheses that speciation follows the accumulation of many small events that act either multiplicatively or additively found support in 8% and none of the trees, respectively. A further 8% of trees hinted that the probability of speciation changes according to the amount of divergence from the ancestral species, and 6% suggested speciation rates vary among taxa. By comparison, 78% of the trees fit the simplest model in which new species emerge from single events, each rare but individually sufficient to cause speciation. This model predicts a constant rate of speciation, and provides a new interpretation of the Red Queen: the metaphor of species losing a race against a deteriorating environment is replaced by a view linking speciation to rare stochastic events that cause reproductive isolation. Attempts to understand species-radiations or why some groups have more or fewer species should look to the size of the catalogue of potential causes of speciation shared by a group of closely related organisms rather than to how those causes combine.

  11. Bulk metallic glass for low noise fluxgate Project (United States)

    National Aeronautics and Space Administration — The team of Prime Photonics, Virginia Tech, and Utron Kinetics propose to demonstrate a method for fabrication of a bulk, amorphous, cobalt-rich material that...

  12. Arsenic speciation in solids using X-ray absorption spectroscopy (United States)

    Foster, Andrea L.; Kim, Chris S.


    Synchrotron-based X-ray absorption spectroscopy (XAS) is an in situ, minimally-destructive, element-specific, molecular-scale structural probe that has been employed to study the chemical forms (species) of arsenic (As) in solid and aqueous phases (including rocks, soils, sediment, synthetic compounds, and numerous types of biota including humans) for more than 20 years. Although several excellent reviews of As geochemistry and As speciation in the environment have been published previously (including recent contributions in this volume), the explosion of As-XAS studies over the past decade (especially studies employing microfocused X-ray beams) warrants this new review of the literature and of data analysis methods.

  13. Finding genes and lineages under selection in speciation. (United States)

    Hart, Michael W; Guerra, Vanessa


    What are the genes and traits that respond to selection and cause prezygotic reproductive isolation between species? This question has been hard to answer because genomes are large, the targets of selection may be scattered across the genome (Sabeti et al., ) and different genes may respond to the same selective pressure in different populations (Scheinfeldt et al., ). In this issue of Molecular Ecology, Weber et al. () use a clever comparative approach and leading-edge transcriptomic methods to identify the species and genes under positive selection for divergence between brittle stars (the echinoderm class Ophiuroidea) in the Ophioderma longicauda species complex. They found convincing evidence of positive or diversifying selection acting on two genes encoding ion channels that form part of the signal transduction cascade within the sperm in response to pheromones. Evidence for selection was concentrated in genes from one species (called C5, with internal fertilization and female parental care of brooded juveniles and not in the other species (called C3, with more conventional broadcast spawning and planktonic development of embryos and larvae). That analysis greatly extends the range of taxa, life history traits and molecules that are associated with positive selection in speciation. It also illustrates some of the current limitations on the application of RNAseq methods in the search for the targets of selection in nonmodel organisms like brittle stars. From both points of view, the new work by Weber et al. () has important implications for our understanding of speciation in the ocean. © 2017 John Wiley & Sons Ltd.

  14. Bulk viscosity of accretion disks around non rotating black holes (United States)

    Moeen Moghaddas, M.


    In this paper, we study the Keplerian, relativistic accretion disks around the non rotating black holes with the bulk viscosity. Many of authors studied the relativistic accretion disks around the black holes, but they ignored the bulk viscosity. We introduce a simple method to calculate the bulk in these disks. We use the simple form for the radial component of the four velocity in the Schwarzschild metric, then the other components of the four velocity and the components of the shear and the bulk tensor are calculated. Also all components of the bulk viscosity, the shear viscosity and stress tensor are calculated. It is seen that some components of the bulk tensor are comparable with the shear tensor. We calculate some of the thermodynamic quantities of the relativistic disks. Comparison of thermodynamic quantities shows that in some states influences of the bulk viscosity are important, especially in the inner radiuses. All calculations are done analytically and we do not use the boundary conditions. Finally, we find that in the relativistic disks around the black holes, the bulk viscosity is non-negligible in all the states.

  15. Comparative Studies of the Speciation Patterns of Nickel and ...

    African Journals Online (AJOL)



    Jan 31, 2005 ... ABSTRACT. Results of speciation studies of nickel and chromium in wastewater, surface and groundwater systems using flame atomic .... atomic absorption spectrometer (Varian, Australia) using air- acetylene fuel system ..... it is expected that, overall, the changes in speciation as a result of sample dilution ...

  16. Chemical Speciation of Some metal ions in Groundwaters of Yola ...

    African Journals Online (AJOL)

    Chemical speciation of some metal ions in groundwaters of Yola area using geochemical model were carried out to determine the water quality of the area using the PHREEQC speciation model. The study findings based on model calculations indicated that free Na+, Ca2+, Mg2+ and K+ ions are present and the ...

  17. What do we need to know about speciation?

    NARCIS (Netherlands)

    Butlin, Roger; Debelle, Allan; Kerth, Claudius; Snook, Rhonda R.; Beukeboom, Leo W.; Castillo Cajas, Ruth; Diao, Wenwen; Maan, Martine E.; Paolucci, Silvia; Weissing, Franz J.; van de Zande, Louis; Hoikkala, Anneli; Geuverink, Elzemiek; Jennings, Jackson; Kankare, Maaria; Knott, K. Emily; Tyukmaeva, Venera I.; Zoumadakis, Christos; Ritchie, Michael G.; Barker, Daniel; Immonen, Elina; Kirkpatrick, Mark; Noor, Mohamed; Macias Garcia, Constantino; Schmitt, Thomas; Schilthuizen, Menno

    Speciation has been a major focus of evolutionary biology research in recent years, with many important advances. However, some of the traditional organising principles of the subject area no longer provide a satisfactory framework, such as the classification of speciation mechanisms by geographical

  18. Sympatric speciation by sexual selection : A critical reevaluation

    NARCIS (Netherlands)

    van Doorn, G.S.; Dieckmann, U.; Weissing, F.J.

    Several empirical studies put forward sexual selection as an important driving force of sympatric speciation. This idea agrees with recent models suggesting that speciation may proceed by means of divergent Fisherian runaway processes within a single population. Notwithstanding this, the models so

  19. Self-consistent approach for neutral community models with speciation

    NARCIS (Netherlands)

    Haegeman, Bart; Etienne, Rampal S.

    Hubbell's neutral model provides a rich theoretical framework to study ecological communities. By incorporating both ecological and evolutionary time scales, it allows us to investigate how communities are shaped by speciation processes. The speciation model in the basic neutral model is

  20. The neutral theory of biodiversity with random fission speciation

    NARCIS (Netherlands)

    Etienne, Rampal S.; Haegeman, Bart

    The neutral theory of biodiversity and biogeography emphasizes the importance of dispersal and speciation to macro-ecological diversity patterns. While the influence of dispersal has been studied quite extensively, the effect of speciation has not received much attention, even though it was already

  1. Dynamic speciation analysis and bioavailability of metals in aquatic systems

    NARCIS (Netherlands)

    Leeuwen, van H.P.; Town, R.M.; Buffle, J.; Cleven, R.F.M.J.; Davison, W.; Puy, J.; Riemsdijk, van W.H.; Sigg, L.


    Dynamic metal speciation analysis in aquatic ecosystems is emerging as a powerful basis for development of predictions of bioavailability and reliable risk assessment strategies. A given speciation sensor is characterized by an effective time scale or kinetic window that defines the measurable metal

  2. On the dependence of speciation rates on species abundance and ...

    Indian Academy of Sciences (India)

    The question of the potential importance for speciation of large/small population sizes remains open. We compare speciation rates in twelve major taxonomic groups that differ by twenty orders of magnitude in characteristic species abundance (global population number). It is observed that the twenty orders of magnitude's ...

  3. Sympatric speciation and extinction driven by environment dependent sexual selection

    NARCIS (Netherlands)

    Van Doorn, G.S.; Noest, A.J.; Hogeweg, P.


    A theoretical model is studied to investigate the possibility of sympatric speciation driven by sexual selection and ecological diversification. In particular, we focus on the rock-dwelling haplochromine cichlid species in Lake Victoria. The high speciation rate in these cichlids has been explained

  4. Speciation of arsenic and mercury in feed: why and how?

    DEFF Research Database (Denmark)

    Hedegaard, Rikke Susanne Vingborg; Sloth, Jens Jørgen


    The understanding of the mechanisms of biological activities and biotransformation of trace elements such as arsenic and mercury has improved during recent years with the help of chemical speciation studies. However, the most important practical application of elemental speciation is in the area ...

  5. Parasites Promote and When Might They Constrain Ecological Speciation?

    Directory of Open Access Journals (Sweden)

    Anssi Karvonen


    Full Text Available Research on speciation and adaptive radiation has flourished during the past decades, yet factors underlying initiation of reproductive isolation often remain unknown. Parasites represent important selective agents and have received renewed attention in speciation research. We review the literature on parasite-mediated divergent selection in context of ecological speciation and present empirical evidence for three nonexclusive mechanisms by which parasites might facilitate speciation: reduced viability or fecundity of immigrants and hybrids, assortative mating as a pleiotropic by-product of host adaptation, and ecologically-based sexual selection. We emphasise the lack of research on speciation continuums, which is why no study has yet made a convincing case for parasite driven divergent evolution to initiate the emergence of reproductive isolation. We also point interest towards selection imposed by single versus multiple parasite species, conceptually linking this to strength and multifariousness of selection. Moreover, we discuss how parasites, by manipulating behaviour or impairing sensory abilities of hosts, may change the form of selection that underlies speciation. We conclude that future studies should consider host populations at variable stages of the speciation process, and explore recurrent patterns of parasitism and resistance that could pinpoint the role of parasites in imposing the divergent selection that initiates ecological speciation.

  6. Sample treatment in chromatography-based speciation of organometallic pollutants. (United States)

    Gómez-Riza, J L; Morales, E; Giráldez, I; Sánchez-Rodas, D; Velasco, A


    Speciation analysis is nowadays performed routinely in many laboratories to control the quality of the environment, food and health. Chemical speciation analyses generally include the study of different oxidation state of elements or individual organometallic compounds. The determination of the different chemical forms of elements is still an analytical challenge, since they are often unstable and concentrations in different matrices of interest are in the microg l(-1) or even in the ng l(-1) range (e.g., estuarine waters) or ng g(-1) in sediments and biological tissues. For this reason, sensitive and selective analytical atomic techniques are being used as available detectors for speciation, generally coupled with chromatography for the time-resolved introduction of analytes into the atomic spectrometer. The complexity of these instrumental couplings has a straightforward consequence on the duration of the analysis, but sample preparation to separate and transfer the chemical species present in the sample into a solution to be accepted readily by a chromatographic column is the more critical step of total analysis, and demands considerable operator skills and time cost. Traditionally, liquid-liquid extraction has been employed for sample treatment with serious disadvantages, such as consumption, disposal and long-term exposure to organic solvent. In addition, they are usually cumbersome and time-consuming. Therefore, the introduction of new reagents such as sodium tetraethylborate for the simultaneous derivatization of several elements has been proposed. Other possibilities are based in the implementation of techniques for efficient and accelerated isolation of species from the sample matrix. This is the case for microwave-assisted extraction, solid-phase extraction and microextraction, supercritical fluid extraction or pressurized liquid extraction, which offer new possibilities in species treatment, and the advantages of a drastic reduction of the extraction

  7. Importance of ICPMS for speciation analysis is changing: future trends for targeted and non-targeted element speciation analysis. (United States)

    Feldmann, Joerg; Raab, Andrea; Krupp, Eva M


    This article is aimed at researchers interested in organic molecules which contain a heteroatom but who have never considered using inductively coupled plasma mass spectrometry (ICPMS) or who have used ICPMS for years and developed numerous methods for analysis of target elemental species. We try to illustrate (1) that ICPMS has been very useful for speciation analysis of metal(loid) target species and that there is now a trend to replace the costly detector with cheaper detection systems for routine target analysis, and (2) that ICPMS has been used and will be used even more in the future for non-targeted analysis of elements which are not normally associated with ICPMS analysis, such as non-metals such as sulfur, phosphorus, chlorine and fluorine. Graphical Abstract Starting with HPLC-ICPMS for non-targeted analysis of heteroatom containing molecules, once target molecule is identified alternative detectors can be used for routine measurements.

  8. Quantitative HPLC-ICP-MS analysis of antimony redox speciation in complex sample matrices: new insights into the Sb-chemistry causing poor chromatographic recoveries


    Hansen, Claus; Schmidt, Bjørn; Larsen, Erik Huusfeldt; Gammelgaard, Bente; Stürup, Stefan; Hansen, Helle Rüsz


    In solution antimony exists either in the pentavalent or trivalent oxidation state. As Sb(III) is more toxic than Sb(V), it is important to be able to perform a quantitative speciation analysis of Sb’s oxidation state. The most commonly applied chromatographic methods used for this redox speciation analysis do, however, often show a low chromatographic Sb recovery when samples of environmental or biological origin are analysed. In this study we explored basal chemistry of antimony and found t...

  9. Speciation in experimental C-O-H fluids produced by the thermal dissociation of oxalic acid dihydrate (United States)

    Morgan, G. B., VI; Chou, I.-Ming; Pasteris, J. D.


    Fluid speciations and their related reaction pathways were studied in C-O-H-system fluids produced by the thermal dissociation of oxalic acid dihydrate (OAD: H 2C 2O 4 · 2H 2O) sealed in silica glass capsules. Experiments were conducted in the temperature range 230-750°C, with bulk fluid densities in the range 0.01-0.53 g/cm 3. Pressure was controlled by temperature and density in the isochoric systems. The quenched products of dissociation experiments were an aqueous liquid and one (supercritical fluid) or, rarely, two (vapor plus liquid) carbonic phase (s). In-situ Raman microanalyses were performed on the quenched carbonic phases at room temperature, at which fluid pressures ranged from about 50 to 340 bars. Bulk fluid speciations were reconstructed from the Raman analyses via mass balance constraints, and appear to monitor the true fluid speciations at run conditions. In experiments from the lowtemperature range (230-350°C), fluid speciations record the dissociation of OAD according to the reaction OAD = CO2 + CO + 3 H2O. A process of the form CO + H2O = CO2 + H2 is driven to the right with increasing temperature. The hydrogen gas produced tends to escape from the sample systems via diffusion into/through the silica glass capsules, shifting bulk compositions toward equimolar binary H 2O-CO 2 mixtures. The speciations of fluids in experiments with minimal hydrogen loss show poor agreement with speciations calculated for equilibrium fluids by the corresponding-states model of SAXENA and FEI (1988). Such disagreement suggests that the formations of CH 4 and graphite are metastably inhibited in the current experiments, which correlates with their absence or trivial abundances in experimental products. Moreover, calculations in which the stabilities of methane and graphite are suppressed suggest that such metastable equilibrium is approached only in experiments at temperatures greater than about 600-650°C. These results have applications to fluid processes in

  10. Analytical aspects of technetium speciation in spinach plants

    Energy Technology Data Exchange (ETDEWEB)

    Harms, A.V


    Spinach (Spinacea oleracea L.) is used as a model plant for terrestrial systems, because of its relation to the human food chain, its ability to accumulate heavy metals, and certain experimental advantages, e.g., the relative ease of cultivation of the seedlings and the relative ease of maceration of its leaves. The role of technetium in this research with its chemical, environmental and analytical aspects is discussed in Chapter 2. Chapters 3, 4, and 5, are dedicated to a closer look at the design of a reliable speciation method using size-exclusion chromatography (SEC). Chapter 3 illustrates the role which a `protective` compound, i.e., 2-mercaptoethanol (2-ME), an inhibitor of polyphenol oxidase, might play in plant-Tc speciation studies. The reactivity of TcO{sub 4}{sup {sup -}} and two Tc model species, i.e., anionic Tc-DTPA and cationic Tc-cyclam, with 2-ME is discussed. The Tc species are separated with low- pressure SEC, using Sephadex as stationary phase. It is shown that Tc-DTPA does react with 2-ME, presumably resulting in the formation of a Tc-complex. In Chapter 4 the development of a `mild` high-performance SEC method for separation of Tc compounds is described. It is shown that non-size effects enhance the separation characteristics of this technique resulting in the separation of TcO{sub 4}{sup {sup -}}, Tc-DTPA, and Tc-cyclam. Moreover, it is shown that the extent of these non-size effects has a close relation with the nature of the Tc species, temperature, ionic strength of the mobile phase, and nature of the stationary phase. One of the stationary phases, i.e., a copolymer of 2-hydroxyethyl methacrylate and ethylene dimethacrylate (HEMA), is also used in Chapter 5 to separate TcO{sub 4}{sup {sup -}} from plant-induced Tc species (TcX). Chapter 5 is dedicated to the development of an analytical procedure for Tc speciation in spinach plants using a dual Tc radiotracer technique. Chapters 6 and 7 are dedicated to a further investigation of the

  11. Longitudinal bulk acoustic mass sensor

    DEFF Research Database (Denmark)

    Hales, Jan Harry; Teva, Jordi; Boisen, Anja


    A polycrystalline silicon longitudinal bulk acoustic cantilever is fabricated and operated in air at 51 MHz. A mass sensitivity of 100 Hz/fg (1 fg=10(-15) g) is obtained from the preliminary experiments where a minute mass is deposited on the device by means of focused ion beam. The total noise...

  12. Bulk fields with brane terms

    Energy Technology Data Exchange (ETDEWEB)

    Aguila, F. del [Departamento de Fisica Teorica y del Cosmos and Centro Andaluz de Fisica de Particulas Elementales (CAFPE), Universidad de Granada, E-18071 Granada (Spain); Perez-Victoria, M. [Dipartimento di Fisica ' ' G. Galilei' ' , Universita di Padova and INFN, Sezione di Padova, Via Marzolo 8, I-35131 Padua (Italy); Santiago, J. [Institute for Particle Physics Phenomenology, University of Durham, South Road, Durham DH1 3LE (United Kingdom)


    In theories with branes, bulk fields get in general divergent corrections localized on these defects. Hence, the corresponding brane terms are renormalized and should be included in the effective theory from the very beginning. We review the phenomenology associated to brane kinetic terms for different spins and backgrounds, and point out that renormalization is required already at the classical level. (orig.)

  13. Selenium speciation in acidic environmental samples: application to acid rain-soil interaction at Mount Etna volcano. (United States)

    Floor, Geerke H; Iglesías, Mònica; Román-Ross, Gabriela; Corvini, Philippe F X; Lenz, Markus


    Speciation plays a crucial role in elemental mobility. However, trace level selenium (Se) speciation analyses in aqueous samples from acidic environments are hampered due to adsorption of the analytes (i.e. selenate, selenite) on precipitates. Such solid phases can form during pH adaptation up till now necessary for chromatographic separation. Thermodynamic calculations in this study predicted that a pHvolcano was developed. With a mobile phase containing 20mM ammonium citrate at pH 3, selenate and selenite could be separated in different acidic media (spiked water, rain, soil leachates) in volcano demonstrated the dominance of selenate over selenite in leachates from samples collected close to the volcanic craters. This suggests that competitive behavior with sulfate present in acid rain might be a key factor in Se mobilization. The developed speciation method can significantly contribute to understand Se cycling in acidic, Al/Fe rich environments. Copyright © 2011 Elsevier Ltd. All rights reserved.

  14. Electrodialytic removal of heavy metals from different fly ashes. Influence of heavy metal speciation in the ashes

    DEFF Research Database (Denmark)

    Pedersen, Anne Juul; Ottosen, Lisbeth M.; Villumsen, Arne


    in lab scale, and the results were discussed in relation to the expected heavy metal speciation in the ashes. In initial leaching experiments the pH-dependent desorption characteristics of the heavy metals Cd, Pb, Zn and Cu were analogous in the two MSWI ashes, and thus it was expected...... that the speciation of these metals was similar in the two ashes. On the other hand, the leaching behaviour (and concentration) of Cr was diverse. The apparent similar speciation of Cd, Pb, Zn and Cu was only partly confirmed in the following electrodialytic remediation experiments. Significant differences in re......Electrodialytic Remediation has recently been suggested as a potential method for removal of heavy metals from fly ashes. In this work electrodialytic remediation of three different fly ashes, i.e. two municipal solid waste incinerator (MSWI) fly ashes and one wood combustion fly ash was studied...

  15. Arsenic speciation by hydride generation-quartz furnace atomic absorption spectrometry. Optimization of analytical parameters and application to environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Molenat, N.; Astruc, A.; Holeman, M.; Pinel, R. [Laboratoire de Chimie Analytique Bioinorganique et Environnement, Dept. de Chimie, Faculte des Sciences et Techniques, 64 - Pau (France); Maury, G. [Montpellier-2 Univ., 34 (France). Dept. de Chimie Organique Fine


    Analytical parameters of hydride generation, trapping, gas chromatography and atomic absorption spectrometry detection in a quartz cell furnace (HG/GC/QFAAS) device have been optimized in order to develop an efficient and sensitive method for arsenic compounds speciation. Good performances were obtained with absolute detection limits in the range of 0.1 - 0.5 ng for arsenite, arsenate, mono-methyl-arsonic acid (MMAA), dimethyl-arsinic acid (DMAA) and trimethyl-arsine oxide (TMAO). A pH selective reduction for inorganic arsenic speciation was successfully reported. Application to the accurate determination of arsenic compounds in different environmental samples was performed. (authors)

  16. Surface barrier and bulk pinning in MgB$_2$ superconductor


    Pissas, M.; Moraitakis, E.; Stamopoulos, D.; Papavassiliou, G.; Psycharis, V.; Koutandos, S.


    We present a modified method of preparation of the new superconductor MgB$_2$. The polycrystalline samples were characterized using x-ray and magnetic measurements. The surface barriers control the isothermal magnetization loops in powder samples. In bulk as prepared samples we always observed symmetric magnetization loops indicative of the presence of a bulk pinning mechanism. Magnetic relaxation measurements in the bulk sample reveal a crossover of surface barrier to bulk pinning.

  17. Metallic speciation in environmental samples. La especiacion metalica en muestras medioambientales

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez Uria, J.E.


    A review about chemical speciation in environmental samples was developed. Starting from definition of speciation, characteristic techniques and squemes for speciation more adequate for the characterization of the several organic/inorganic metal-species was considered. Finally, the possible future tendences of speciation techniques was also considered. (Author) 27 refs.

  18. Application of Hyphenated Techniques in Speciation Analysis of Arsenic, Antimony, and Thallium (United States)

    Michalski, Rajmund; Szopa, Sebastian; Jabłońska, Magdalena; Łyko, Aleksandra


    Due to the fact that metals and metalloids have a strong impact on the environment, the methods of their determination and speciation have received special attention in recent years. Arsenic, antimony, and thallium are important examples of such toxic elements. Their speciation is especially important in the environmental and biomedical fields because of their toxicity, bioavailability, and reactivity. Recently, speciation analytics has been playing a unique role in the studies of biogeochemical cycles of chemical compounds, determination of toxicity and ecotoxicity of selected elements, quality control of food products, control of medicines and pharmaceutical products, technological process control, research on the impact of technological installation on the environment, examination of occupational exposure, and clinical analysis. Conventional methods are usually labor intensive, time consuming, and susceptible to interferences. The hyphenated techniques, in which separation method is coupled with multidimensional detectors, have become useful alternatives. The main advantages of those techniques consist in extremely low detection and quantification limits, insignificant interference, influence as well as high precision and repeatability of the determinations. In view of their importance, the present work overviews and discusses different hyphenated techniques used for arsenic, antimony, and thallium species analysis, in different clinical, environmental and food matrices. PMID:22654649

  19. Testing gradual and speciational models of evolution in extant taxa: the example of ratites. (United States)

    Laurin, M; Gussekloo, S W S; Marjanović, D; Legendre, L; Cubo, J


    Ever since Eldredge and Gould proposed their model of punctuated equilibria, evolutionary biologists have debated how often this model is the best description of nature and how important it is compared to the more gradual models of evolution expected from natural selection and the neo-Darwinian paradigm. Recently, Cubo proposed a method to test whether morphological data in extant ratites are more compatible with a gradual or with a speciational model (close to the punctuated equilibrium model). As shown by our simulations, a new method to test the mode of evolution of characters (involving regression of standardized contrasts on their expected standard deviation) is easier to implement and more powerful than the previously proposed method, but the Mesquite module comet (aimed at investigating evolutionary models using comparative data) performs better still. Uncertainties in branch length estimates are probably the largest source of potential error. Cubo hypothesized that heterochronic mechanisms may underlie morphological changes in bone shape during the evolution of ratites. He predicted that the outcome of these changes may be consistent with a speciational model of character evolution because heterochronic changes can be instantaneous in terms of geological time. Analysis of a more extensive data set confirms his prediction despite branch length uncertainties: evolution in ratites has been mostly speciational for shape-related characters. However, it has been mostly gradual for size-related ones. © 2011 The Authors. Journal of Evolutionary Biology © 2011 European Society For Evolutionary Biology.

  20. Genomic islands of speciation in Anopheles gambiae.

    Directory of Open Access Journals (Sweden)


    Full Text Available The African malaria mosquito, Anopheles gambiae sensu stricto (A. gambiae, provides a unique opportunity to study the evolution of reproductive isolation because it is divided into two sympatric, partially isolated subtaxa known as M form and S form. With the annotated genome of this species now available, high-throughput techniques can be applied to locate and characterize the genomic regions contributing to reproductive isolation. In order to quantify patterns of differentiation within A. gambiae, we hybridized population samples of genomic DNA from each form to Affymetrix GeneChip microarrays. We found that three regions, together encompassing less than 2.8 Mb, are the only locations where the M and S forms are significantly differentiated. Two of these regions are adjacent to centromeres, on Chromosomes 2L and X, and contain 50 and 12 predicted genes, respectively. Sequenced loci in these regions contain fixed differences between forms and no shared polymorphisms, while no fixed differences were found at nearby control loci. The third region, on Chromosome 2R, contains only five predicted genes; fixed differences in this region were also verified by direct sequencing. These "speciation islands" remain differentiated despite considerable gene flow, and are therefore expected to contain the genes responsible for reproductive isolation. Much effort has recently been applied to locating the genes and genetic changes responsible for reproductive isolation between species. Though much can be inferred about speciation by studying taxa that have diverged for millions of years, studying differentiation between taxa that are in the early stages of isolation will lead to a clearer view of the number and size of regions involved in the genetics of speciation. Despite appreciable levels of gene flow between the M and S forms of A. gambiae, we were able to isolate three small regions of differentiation where genes responsible for ecological and behavioral

  1. Towards bulk based preconditioning for quantum dotcomputations

    Energy Technology Data Exchange (ETDEWEB)

    Dongarra, Jack; Langou, Julien; Tomov, Stanimire; Channing,Andrew; Marques, Osni; Vomel, Christof; Wang, Lin-Wang


    This article describes how to accelerate the convergence of Preconditioned Conjugate Gradient (PCG) type eigensolvers for the computation of several states around the band gap of colloidal quantum dots. Our new approach uses the Hamiltonian from the bulk materials constituent for the quantum dot to design an efficient preconditioner for the folded spectrum PCG method. The technique described shows promising results when applied to CdSe quantum dot model problems. We show a decrease in the number of iteration steps by at least a factor of 4 compared to the previously used diagonal preconditioner.

  2. Tailoring Magnetic Properties in Bulk Nanostructured Solids (United States)

    Morales, Jason Rolando

    Important magnetic properties and behaviors such as coercivity, remanence, susceptibility, energy product, and exchange coupling can be tailored by controlling the grain size, composition, and density of bulk magnetic materials. At nanometric length scales the grain size plays an increasingly important role since magnetic domain behavior and grain boundary concentration determine bulk magnetic behavior. This has spurred a significant amount of work devoted to developing magnetic materials with nanometric features (thickness, grain/crystallite size, inclusions or shells) in 0D (powder), 1D (wires), and 2D (thin films) materials. Large 3D nanocrystalline materials are more suitable for many applications such as permanent magnets, magneto-optical Faraday isolators etc. Yet there are relatively few successful demonstrations of 3D magnetic materials with nanoscale influenced properties available in the literature. Making dense 3D bulk materials with magnetic nanocrystalline microstructures is a challenge because many traditional densification techniques (HIP, pressureless sintering, etc.) move the microstructure out of the "nano" regime during densification. This dissertation shows that the Current Activated Pressure Assisted Densification (CAPAD) method, also known as spark plasma sintering, can be used to create dense, bulk, magnetic, nanocrystalline solids with varied compositions suited to fit many applications. The results of my research will first show important implications for the use of CAPAD for the production of exchange-coupled nanocomposite magnets. Decreases in grain size were shown to have a significant role in increasing the magnitude of exchange bias. Second, preferentially ordered bulk magnetic materials were produced with highly anisotropic material properties. The ordered microstructure resulted in changing magnetic property magnitudes (ex. change in coercivity by almost 10x) depending on the relative orientation (0° vs. 90°) of an externally

  3. Contribution of analytical techniques coupled to the knowledge of the uranium speciation in natural conditions; Apports des techniques analytiques couplees a la connaissance de la speciation de l'uranium en conditions naturelles

    Energy Technology Data Exchange (ETDEWEB)

    Petit, J.


    To understand the transport mechanisms and the radionuclides behaviour in the bio-geosphere is necessary to evaluate healthy and environmental risks of nuclear industry. These mechanisms are monitored by radioelements speciation, namely the distribution between their different physico-chemical forms in the environment. From this perspective, this PhD thesis deals with uranium speciation in a natural background. A detailed summary of uranium biogeochemistry has been written, which enables to restrict the PhD issue to uranium complexation with oxalic acid, a hydrophilic organic acid with good binding properties, ubiquitous in soil waters. Analytical conditions have been established by means of speciation diagrams. The speciation diagrams building by means of literature stability constants has allowed to define the analytical conditions of complex formation. The chosen analytical technique is the hyphenation of a separative technique (liquid chromatography LC or capillary electrophoresis CE) with mass spectrometry (ICPMS). The studied complexes presence in the synthetic samples has been confirmed with UV/visible spectrophotometry. LC-ICPMS analyses have proved the lability of the uranyl-organic acid complexes, namely their tendency to dissociate during analysis, which prevents from studying uranium speciation. CE-ICPMS study of labile complexes from a metal-ligand system has been made possible by employing affinity capillary electrophoresis, which enables to determine stability constants and electrophoretic mobilities. This PhD thesis has allowed to compare the different mathematical treatments of binding isotherm and to take into account ionic strength and real ligand concentration. Affinity CE has been applied successfully to lanthanum-oxalate (model system) and uranium-oxalate systems. The obtained results have been applied to a real system (situated in Le Bouchet). This shows the contribution of the developed method to the modelling of uranium speciation. (author)

  4. Chemical state speciation by resonant Raman scattering

    CERN Document Server

    Karydas, A G; Zarkadas, C; Paradelis, T; Kallithrakas-Kontos, N


    In the resonant Raman scattering (RRS) process the emitted photon exhibits a continuous energy distribution with a high energy cutoff limit. This cutoff energy depends on the chemical state of the element under examination. In the present work, the possibility of identifying the chemical state of V atoms by employing RRS spectroscopy with a semiconductor Si(Li) detector is investigated. A proton induced Cr K alpha x-ray beam was used as the incident radiation, having a fixed energy lower than the V K-absorption edge. The net RRS distributions extracted from the energy dispersive spectra of metallic V and its compound targets were simulated by an appropriate theoretical model. The results showed the possibility of employing RRS spectroscopy with a semiconductor detector for chemical speciation studies.

  5. Carbon speciation and surface tension of fog (United States)

    Capel, P.D.; Gunde, R.; Zurcher, F.; Giger, W.


    The speciation of carbon (dissolved/particulate, organic/inorganic) and surface tension of a number of radiation fogs from the urban area of Zurich, Switzerland, were measured. The carbon species were dominated by "dissolved" organic carbon (DOC; i.e., the fraction that passes through a filter), which was typically present at levels of 40-200 mg/L. Less than 10% of the DOC was identified as specific individual organic compounds. Particulate organic carbon (POC) accounted for 26-41% of the mass of the particles, but usually less than 10% of the total organic carbon mass. Inorganic carbon species were relatively minor. The surface tensions of all the measured samples were less than pure water and were correlated with their DOC concentrations. The combination of high DOC and POC and low surface tension suggests a mechanism for the concentration of hydrophobic organic contaminants in the fog droplet, which have been observed by numerous investigators. ?? 1990 American Chemical Society.

  6. Horizontal Gene Transfer, Dispersal and Haloarchaeal Speciation (United States)

    Papke, R. Thane; Corral, Paulina; Ram-Mohan, Nikhil; de la Haba, Rafael R.; Sánchez-Porro, Cristina; Makkay, Andrea; Ventosa, Antonio


    The Halobacteria are a well-studied archaeal class and numerous investigations are showing how their diversity is distributed amongst genomes and geographic locations. Evidence indicates that recombination between species continuously facilitates the arrival of new genes, and within species, it is frequent enough to spread acquired genes amongst all individuals in the population. To create permanent independent diversity and generate new species, barriers to recombination are probably required. The data support an interpretation that rates of evolution (e.g., horizontal gene transfer and mutation) are faster at creating geographically localized variation than dispersal and invasion are at homogenizing genetic differences between locations. Therefore, we suggest that recurrent episodes of dispersal followed by variable periods of endemism break the homogenizing forces of intrapopulation recombination and that this process might be the principal stimulus leading to divergence and speciation in Halobacteria. PMID:25997110

  7. Horizontal Gene Transfer, Dispersal and Haloarchaeal Speciation

    Directory of Open Access Journals (Sweden)

    R. Thane Papke


    Full Text Available The Halobacteria are a well-studied archaeal class and numerous investigations are showing how their diversity is distributed amongst genomes and geographic locations. Evidence indicates that recombination between species continuously facilitates the arrival of new genes, and within species, it is frequent enough to spread acquired genes amongst all individuals in the population. To create permanent independent diversity and generate new species, barriers to recombination are probably required. The data support an interpretation that rates of evolution (e.g., horizontal gene transfer and mutation are faster at creating geographically localized variation than dispersal and invasion are at homogenizing genetic differences between locations. Therefore, we suggest that recurrent episodes of dispersal followed by variable periods of endemism break the homogenizing forces of intrapopulation recombination and that this process might be the principal stimulus leading to divergence and speciation in Halobacteria.

  8. Horizontal gene transfer, dispersal and haloarchaeal speciation. (United States)

    Papke, R Thane; Corral, Paulina; Ram-Mohan, Nikhil; Haba, Rafael R de la; Sánchez-Porro, Cristina; Makkay, Andrea; Ventosa, Antonio


    The Halobacteria are a well-studied archaeal class and numerous investigations are showing how their diversity is distributed amongst genomes and geographic locations. Evidence indicates that recombination between species continuously facilitates the arrival of new genes, and within species, it is frequent enough to spread acquired genes amongst all individuals in the population. To create permanent independent diversity and generate new species, barriers to recombination are probably required. The data support an interpretation that rates of evolution (e.g., horizontal gene transfer and mutation) are faster at creating geographically localized variation than dispersal and invasion are at homogenizing genetic differences between locations. Therefore, we suggest that recurrent episodes of dispersal followed by variable periods of endemism break the homogenizing forces of intrapopulation recombination and that this process might be the principal stimulus leading to divergence and speciation in Halobacteria.

  9. Topography-driven isolation, speciation and a global increase of endemism with elevation

    DEFF Research Database (Denmark)

    Steinbauer, Manuel; Field, R.; Grytnes, John-Arvid


    with elevation, globally. This was independent of richness–elevation relationships, which had varying shapes but decreased with elevation at high elevations. The endemism-elevation relationships were consistent with isolation-related predictions, but inconsistent with hypotheses related to area, richness...... and temperature. Main conclusions: Higher per-species speciation rates caused by increasing isolation with elevation are the most plausible and parsimonious explanation for the globally consistent pattern of higher endemism at higher elevations that we identify. We suggest that topography-driven isolation...... hypotheses invoking higher speciation with area, temperature and species richness. Location: 32 insular and 18 continental elevational gradients from around the world. Methods: We compiled entire floras with elevation-specific occurrence information, and calculated the proportion of native species...

  10. Genetic structure and bio-climatic modeling support allopatric over parapatric speciation along a latitudinal gradient

    Directory of Open Access Journals (Sweden)

    Rossetto Maurizio


    Full Text Available Abstract Background Four of the five species of Telopea (Proteaceae are distributed in a latitudinal replacement pattern on the south-eastern Australian mainland. In similar circumstances, a simple allopatric speciation model that identifies the origins of genetic isolation within temporal geographic separation is considered as the default model. However, secondary contact between differentiated lineages can result in similar distributional patterns to those arising from a process of parapatric speciation (where gene flow between lineages remains uninterrupted during differentiation. Our aim was to use the characteristic distributional patterns in Telopea to test whether it reflected the evolutionary models of allopatric or parapatric speciation. Using a combination of genetic evidence and environmental niche modelling, we focused on three main questions: do currently described geographic borders coincide with genetic and environmental boundaries; are there hybrid zones in areas of secondary contact between closely related species; did species distributions contract during the last glacial maximum resulting in distributional gaps even where overlap and hybridisation currently occur? Results Total genomic DNA was extracted from 619 individuals sampled from 36 populations representing the four species. Seven nuclear microsatellites (nSSR and six chloroplast microsatellites (cpSSR were amplified across all populations. Genetic structure and the signature of admixture in overlap zones was described using the Bayesian clustering methods implemented in STUCTURE and NewHybrids respectively. Relationships between chlorotypes were reconstructed as a median-joining network. Environmental niche models were produced for all species using environmental parameters from both the present day and the last glacial maximum (LGM. The nSSR loci amplified a total of 154 alleles, while data for the cpSSR loci produced a network of six chlorotypes. STRUCTURE revealed

  11. Genetic structure and bio-climatic modeling support allopatric over parapatric speciation along a latitudinal gradient. (United States)

    Rossetto, Maurizio; Allen, Chris B; Thurlby, Katie A G; Weston, Peter H; Milner, Melita L


    Four of the five species of Telopea (Proteaceae) are distributed in a latitudinal replacement pattern on the south-eastern Australian mainland. In similar circumstances, a simple allopatric speciation model that identifies the origins of genetic isolation within temporal geographic separation is considered as the default model. However, secondary contact between differentiated lineages can result in similar distributional patterns to those arising from a process of parapatric speciation (where gene flow between lineages remains uninterrupted during differentiation). Our aim was to use the characteristic distributional patterns in Telopea to test whether it reflected the evolutionary models of allopatric or parapatric speciation. Using a combination of genetic evidence and environmental niche modelling, we focused on three main questions: do currently described geographic borders coincide with genetic and environmental boundaries; are there hybrid zones in areas of secondary contact between closely related species; did species distributions contract during the last glacial maximum resulting in distributional gaps even where overlap and hybridisation currently occur? Total genomic DNA was extracted from 619 individuals sampled from 36 populations representing the four species. Seven nuclear microsatellites (nSSR) and six chloroplast microsatellites (cpSSR) were amplified across all populations. Genetic structure and the signature of admixture in overlap zones was described using the Bayesian clustering methods implemented in STUCTURE and NewHybrids respectively. Relationships between chlorotypes were reconstructed as a median-joining network. Environmental niche models were produced for all species using environmental parameters from both the present day and the last glacial maximum (LGM).The nSSR loci amplified a total of 154 alleles, while data for the cpSSR loci produced a network of six chlorotypes. STRUCTURE revealed an optimum number of five clusters

  12. Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review. (United States)

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


    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.

  13. Recombination rate variation and speciation: theoretical predictions and empirical results from rabbits and mice. (United States)

    Nachman, Michael W; Payseur, Bret A


    Recently diverged taxa may continue to exchange genes. A number of models of speciation with gene flow propose that the frequency of gene exchange will be lower in genomic regions of low recombination and that these regions will therefore be more differentiated. However, several population-genetic models that focus on selection at linked sites also predict greater differentiation in regions of low recombination simply as a result of faster sorting of ancestral alleles even in the absence of gene flow. Moreover, identifying the actual amount of gene flow from patterns of genetic variation is tricky, because both ancestral polymorphism and migration lead to shared variation between recently diverged taxa. New analytic methods have been developed to help distinguish ancestral polymorphism from migration. Along with a growing number of datasets of multi-locus DNA sequence variation, these methods have spawned a renewed interest in speciation models with gene flow. Here, we review both speciation and population-genetic models that make explicit predictions about how the rate of recombination influences patterns of genetic variation within and between species. We then compare those predictions with empirical data of DNA sequence variation in rabbits and mice. We find strong support for the prediction that genomic regions experiencing low levels of recombination are more differentiated. In most cases, reduced gene flow appears to contribute to the pattern, although disentangling the relative contribution of reduced gene flow and selection at linked sites remains a challenge. We suggest fruitful areas of research that might help distinguish between different models.

  14. Chemical speciation and bioavailability of rare earth elements (REEs) in the ecosystem: a review. (United States)

    Khan, Aysha Masood; Bakar, Nor Kartini Abu; Bakar, Ahmad Farid Abu; Ashraf, Muhammad Aqeel


    Rare earths (RE), chemically uniform group of elements due to similar physicochemical behavior, are termed as lanthanides. Natural occurrence depends on the geological circumstances and has been of long interest for geologist as tools for further scientific research into the region of ores, rocks, and oceanic water. The review paper mainly focuses to provide scientific literature about rare earth elements (REEs) with potential environmental and health effects in understanding the research. This is the initial review of RE speciation and bioavailability with current initiative toward development needs and research perceptive. In this paper, we have also discussed mineralogy, extraction, geochemistry, analytical methods of rare earth elements. In this study, REEs with their transformation and vertical distribution in different environments such as fresh and seawater, sediments, soil, weathering, transport, and solubility have been reported with most recent literature along key methods of findings. Speciation and bioavailability have been discussed in detail with special emphasis on soil, plant, and aquatic ecosystems and their impacts on the environment. This review shows that REE gained more importance in last few years due to their detrimental effects on living organisms, so their speciation, bioavailability, and composition are much more important to evaluate their health risks and are discussed thoroughly as well.

  15. Foliar or root exposures to smelter particles: consequences for lead compartmentalization and speciation in plant leaves. (United States)

    Schreck, Eva; Dappe, Vincent; Sarret, Géraldine; Sobanska, Sophie; Nowak, Dorota; Nowak, Jakub; Stefaniak, Elżbieta Anna; Magnin, Valérie; Ranieri, Vincent; Dumat, Camille


    In urban areas with high fallout of airborne particles, metal uptake by plants mainly occurs by foliar pathways and can strongly impact crop quality. However, there is a lack of knowledge on metal localization and speciation in plants after pollution exposure, especially in the case of foliar uptake. In this study, two contrasting crops, lettuce (Lactuca sativa L.) and rye-grass (Lolium perenne L.), were exposed to Pb-rich particles emitted by a Pb-recycling factory via either atmospheric or soil application. Pb accumulation in plant leaves was observed for both ways of exposure. The mechanisms involved in Pb uptake were investigated using a combination of microscopic and spectroscopic techniques (electron microscopy, laser ablation, Raman microspectroscopy, and X-ray absorption spectroscopy). The results show that Pb localization and speciation are strongly influenced by the type of exposure (root or shoot pathway) and the plant species. Foliar exposure is the main pathway of uptake, involving the highest concentrations in plant tissues. Under atmospheric fallouts, Pb-rich particles were strongly adsorbed on the leaf surface of both plant species. In lettuce, stomata contained Pb-rich particles in their apertures, with some deformations of guard cells. In addition to PbO and PbSO4, chemical forms that were also observed in pristine particles, new species were identified: organic compounds (minimum 20%) and hexagonal platy crystals of PbCO3. In rye-grass, the changes in Pb speciation were even more egregious: Pb-cell wall and Pb-organic acid complexes were the major species observed. For root exposure, identified here as a minor pathway of Pb transfer compared to foliar uptake, another secondary species, pyromorphite, was identified in rye-grass leaves. Finally, combining bulk and spatially resolved spectroscopic techniques permitted both the overall speciation and the minor but possibly highly reactive lead species to be determined in order to better assess the

  16. Equilibrium Measurements of the NH3-CO2-H2O System: Speciation Based on Raman Spectroscopy and Multivariate Modeling

    Directory of Open Access Journals (Sweden)

    Maths Halstensen


    Full Text Available Liquid speciation is important for reliable process design and optimization of gas-liquid absorption process. Liquid-phase speciation methods are currently available, although they involve tedious and time-consuming laboratory work. Raman spectroscopy is well suited for in situ monitoring of aqueous chemical reactions. Here, we report on the development of a method for speciation of the CO2-NH3-H2O equilibrium using Raman spectroscopy and PLS-R modeling. The quantification methodology presented here offers a novel approach to provide rapid and reliable predictions of the carbon distribution of the CO2-NH3-H2O system, which may be used for process control and optimization. Validation of the reported speciation method which is based on independent, known, NH3-CO2-H2O solutions shows estimated prediction uncertainties for carbonate, bicarbonate, and carbamate of 6.45 mmol/kg H2O, 34.39 mmol/kg H2O, and 100.9 mmol/kg H2O, respectively.

  17. Extraction techniques in speciation analysis of environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Morabito, R. [ENEA Casaccia, Rome (Italy). Environmental Dept.


    One of the main problems in speciation analysis is that the different species of metals are present in complex matrices at very low concentration levels. Thus it is almost always necessary to separate the analytes of concern from the matrix and to concentrate them up to detectable concentration levels. Special care should be paid during extraction in order to avoid any contamination of samples, losses and changes in speciation of analytes of concern. The most common extraction techniques for speciation analysis of Pb, Sn, Hg, Cr, As, Se and Sb in liquid and solid samples are presented and briefly discussed. Due to the large quantity of material to be covered, speciation of alkyl, aryl, and macromolecular compounds (porphyrines, thioneines, etc.) has not been taken into account. (orig.)

  18. Speciation and Persistence of Dimethoate in the Aquatic Environment

    African Journals Online (AJOL)

    Speciation and Persistence of Dimethoate in the Aquatic Environment: Characterization in Terms of a Rate Model that Takes Into Account Hydrolysis, Photolysis, Microbial Degradation and Adsorption of the Pesticide by Colloidal and Sediment Particles.


    Chassis dynamometer emissions testing was conducted to characterize speciated volatile organic compounds (VOCs), including mobile source air toxics (MSATs) and ozone precursors, in exhaust emissions from three modern gasoline direct injection (GDI) light-duty vehicles. Each GDI v...

  20. Pb Speciation Data to Estimate Lead Bioavailability to Quail (United States)

    U.S. Environmental Protection Agency — Linear combination fitting data for lead speciation of soil samples evaluated through an in-vivo/in-vitro correlation for quail exposure. This dataset is associated...

  1. Cobalamin Concentrations in Fetal Liver Show Gender Differences: A Result from Using a High-Pressure Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry as an Ultratrace Cobalt Speciation Method. (United States)

    Bosle, Janine; Goetz, Sven; Raab, Andrea; Krupp, Eva M; Scheckel, Kirk G; Lombi, Enzo; Meharg, Andrew A; Fowler, Paul A; Feldmann, Jörg


    Maternal diet and lifestyle choices may affect placental transfer of cobalamin (Cbl) to the fetus. Fetal liver concentration of Cbl reflects nutritional status with regards to vitamin B12, but at these low concentration current Cbl measurement methods lack robustness. An analytical method based on enzymatic extraction with subsequent reversed-phase-high-pressure liquid chromatography (RP-HPLC) separation and parallel ICPMS and electrospray ionization (ESI)-Orbitrap-MS to determine specifically Cbl species in liver samples of only 10-50 mg was developed using 14 pig livers. Subsequently 55 human fetal livers were analyzed. HPLC-ICPMS analysis for cobalt (Co) and Cbl gave detection limits of 0.18 ng/g and 0.88 ng/g d.m. in liver samples, respectively, with a recovery of >95%. Total Co (Cot) concentration did not reflect the amount of Cbl or vitamin B12 in the liver. Cbl bound Co contributes only 45 ± 15% to Cot. XRF mapping and μXANES analysis confirmed the occurrence of non-Cbl cobalt in pig liver hot spots indicating particular Co. No correlations of total cobalt nor Cbl with fetal weight or weeks of gestation were found for the human fetal livers. Although no gender difference could be identified for total Co concentration, female livers were significantly higher in Cbl concentration (24.1 ± 7.8 ng/g) than those from male fetuses (19.8 ± 7.1 ng/g) (p = 0.04). This HPLC-ICPMS method was able to quantify total Cot and Cbl in fetus liver, and it was sensitive and precise enough to identify this gender difference.

  2. How humans drive speciation as well as extinction

    DEFF Research Database (Denmark)

    Bull, Joseph William; Maron, M.


    influence upon divergence in microorganisms. Even if human activities resulted in no net loss of species diversity by balancing speciation and extinction rates, this would probably be deemed unacceptable. We discuss why, based upon ‘no net loss’ conservation literature— considering phylogenetic diversity...... and other metrics, risk aversion, taboo trade-offs and spatial heterogeneity. We conclude that evaluating speciation alongside extinction could result in more nuanced understanding of biosphere trends, clarifying what it is we actually value about biodiversity....

  3. Gold based bulk metallic glass


    Schroers, Jan; Lohwongwatana, Boonrat; Johnson, William L.; Peker, Atakan


    Gold-based bulk metallic glass alloys based on Au-Cu-Si are introduced. The alloys exhibit a gold content comparable to 18-karat gold. They show very low liquidus temperature, large supercooled liquid region, and good processibility. The maximum casting thickness exceeds 5 mm in the best glassformer. Au49Ag5.5Pd2.3Cu26.9Si16.3 has a liquidus temperature of 644 K, a glass transition temperature of 401 K, and a supercooled liquid region of 58 K. The Vickers hardness of the alloys in this system...

  4. Can environmental change affect host/parasite-mediated speciation? (United States)

    Brunner, Franziska S; Eizaguirre, Christophe


    Parasitism can be a driver of species divergence and thereby significantly alter species formation processes. While we still need to better understand how parasite-mediated speciation functions, it is even less clear how this process is affected by environmental change. Both rapid and gradual changes of the environment can modify host immune responses, parasite virulence and the specificity of their interactions. They will thereby change host-parasite evolutionary trajectories and the potential for speciation in both hosts and parasites. Here, we summarise mechanisms of host-parasite interactions affecting speciation and subsequently consider their susceptibility to environmental changes. We mainly focus on the effects of temperature change and nutrient input to ecosystems as they are major environmental stressors. There is evidence for both disruptive and accelerating effects of those pressures on speciation that seem to be context-dependent. A prerequisite for parasite-driven host speciation is that parasites significantly alter the host's Darwinian fitness. This can rapidly lead to divergent selection and genetic adaptation; however, it is likely preceded by more short-term plastic and transgenerational effects. Here, we also consider how these first responses and their susceptibility to environmental changes could lead to alterations of the species formation process and may provide alternative pathways to speciation. Copyright © 2016 The Authors. Published by Elsevier GmbH.. All rights reserved.

  5. Development of speciation analysis for selenium in nutritional supplements by the determination of the seleno-methionine; Developpement de l'analyse de speciation du selenium dans des complements alimentaires par la determination de la selenomethionine

    Energy Technology Data Exchange (ETDEWEB)

    Sannac, S.; Labarraque, G.; Fisicaro, P. [Laboratoire National de Metrologie et d' Essai (LNE), 75 - Paris (France); Sannac, S.; Pannier, F.; Potin-Gautier, M. [Pau Univ. et des Pays de l' Adour, CNRS/UMR 5254, Lab. de Chimie Analytique, Bio-Inorganique et Environnement (IPREM), 64 (France)


    The development of a reference method in analytical chemistry is presented. Liquid chromatography with inductively coupled plasma mass spectrometry is employed to perform in speciation analysis. Applications are developed for the determination of seleno-methionine in nutritional supplements. The use of isotope dilution, a primary method, is required to enable measurement traceability. Method validation is ensured by the study of a certified reference material. (authors)

  6. Thiourea catalysis of MeHg ligand exchange between natural dissolved organic matter and a thiol-functionalized resin: a novel method of matrix removal and MeHg preconcentration for ultratrace Hg speciation analysis in freshwaters

    Energy Technology Data Exchange (ETDEWEB)

    Vermillion, Brian R.; Hudson, Robert J.M. [University of Illinois Urbana-Champaign, Department of Natural Resources and Environmental Sciences, Urbana, IL (United States)


    Ultratrace analysis of dissolved MeHg in freshwaters requires both dissociation of MeHg from strong ligands in the sample matrix and preconcentration for detection. Existing solid phase extraction methods generally do not efficiently adsorb MeHg from samples containing high concentrations of natural dissolved organic matter. We demonstrate here that the addition of 10-60 mM thiourea (TU) quantitatively releases MeHg from the dissolved matrix of freshwater samples by forming a more labile complex (MeHgTU{sup +}) that quantitatively exchanges MeHg with thiol-functionalized resins at pH{proportional_to}3.5 during column loading. The contents of these columns were efficiently eluted with acidified TU and MeHg was analyzed by Hg-TU complex ion chromatography with cold-vapor atomic fluorescence spectrometry detection. Routinely more than 90% of MeHg was recovered with good precision (average relative standard deviation of 6%) from natural waters - obtained from pools and saturated sediments of wetlands and from rivers - containing up to 68.7 mg C L{sup -1} dissolved organic matter. With the preconcentration step, the method detection limit of 0.29 pg absolute or 0.007 ng L{sup -1} in 40-mL samples is equivalent to that of the current state-of-the- art as practiced by skilled analysts. MeHg in 20-50-mL samples was completely trapped. On the basis of our knowledge of the chemistry of the process, breakthrough volume should depend on the concentrations of TU and H{sup +}. At a TU concentration of 12 mM breakthrough occurred between 50 and 100 mL, but overall adsorption efficiency was still 85% at 100 mL. Formation of artifactual MeHg is minimal; only about 0.7% of ambient MeHg is artifactual as estimated from samples spiked with 4 {mu}g L{sup -1} Hg{sup II}. (orig.)

  7. Coevolution is linked with phenotypic diversification but not speciation in avian brood parasites (United States)

    Medina, Iliana; Langmore, Naomi E.


    Coevolution is often invoked as an engine of biological diversity. Avian brood parasites and their hosts provide one of the best-known examples of coevolution. Brood parasites lay their eggs in the nests of other species, selecting for host defences and reciprocal counteradaptations in parasites. In theory, this arms race should promote increased rates of speciation and phenotypic evolution. Here, we use recently developed methods to test whether the three largest avian brood parasitic lineages show changes in rates of phenotypic diversity and speciation relative to non-parasitic lineages. Our results challenge the accepted paradigm, and show that there is little consistent evidence that lineages of brood parasites have higher speciation or extinction rates than non-parasitic species. However, we provide the first evidence that the evolution of brood parasitic behaviour may affect rates of evolution in morphological traits associated with parasitism. Specifically, egg size and the colour and pattern of plumage have evolved up to nine times faster in parasitic than in non-parasitic cuckoos. Moreover, cuckoo clades of parasitic species that are sympatric (and share similar host genera) exhibit higher rates of phenotypic evolution. This supports the idea that competition for hosts may be linked to the high phenotypic diversity found in parasitic cuckoos. PMID:26702044

  8. Sorption Speciation of Lanthanides/Actinides on Minerals by TRLFS, EXAFS and DFT Studies: A Review

    Directory of Open Access Journals (Sweden)

    Xiaoli Tan


    Full Text Available Lanthanides/actinides sorption speciation on minerals and oxides by means of time resolved laser fluorescence spectroscopy (TRLFS, extended X-ray absorption fine structure spectroscopy (EXAFS and density functional theory (DFT is reviewed in the field of nuclear disposal safety research. The theoretical aspects of the methods are concisely presented. Examples of recent research results of lanthanide/actinide speciation and local atomic structures using TRLFS, EXAFS and DFT are discussed. The interaction of lanthanides/actinides with oxides and minerals as well as their uptake are also of common interest in radionuclide chemistry. Especially the sorption and inclusion of radionuclides into several minerals lead to an improvement in knowledge of minor components in solids. In the solid-liquid interface, the speciation and local atomic structures of Eu(III, Cm(III, U(VI, and Np(IV/VI in several natural and synthetic minerals and oxides are also reviewed and discussed. The review is important to understand the physicochemical behavior of lanthanides/actinides at a molecular level in the natural environment.

  9. Steam Gasification of Sawdust Biochar Influenced by Chemical Speciation of Alkali and Alkaline Earth Metallic Species

    Directory of Open Access Journals (Sweden)

    Dongdong Feng


    Full Text Available The effect of chemical speciation (H2O/NH4Ac/HCl-soluble and insoluble of alkali and alkaline earth metallic species on the steam gasification of sawdust biochar was investigated in a lab-scale, fixed-bed reactor, with the method of chemical fractionation analysis. The changes in biochar structures and the evolution of biochar reactivity are discussed, with a focus on the contributions of the chemical speciation of alkali and alkaline earth metallic species (AAEMs on the steam gasification of biochar. The results indicate that H2O/NH4Ac/HCl-soluble AAEMs have a significant effect on biochar gasification rates. The release of K occurs mainly in the form of inorganic salts and hydrated ions, while that of Ca occurs mainly as organic ones. The sp3-rich or sp2-sp3 structures and different chemical-speciation AAEMs function together as the preferred active sites during steam gasification. H2O/HCl-soluble AAEMs could promote the transformation of biochar surface functional groups, from ether/alkene C-O-C to carboxylate COO− in biochar, while they may both be improved by NH4Ac-soluble AAEMs. H2O-soluble AAEMs play a crucial catalytic role in biochar reactivity. The effect of NH4Ac-soluble AAEMs is mainly concentrated in the high-conversion stage (biochar conversion >30%, while that of HCl-soluble AAEMs is reflected in the whole activity-testing stage.

  10. Moving Speciation Genetics Forward: Modern Techniques Build on Foundational Studies in Drosophila. (United States)

    Castillo, Dean M; Barbash, Daniel A


    The question of how new species evolve has been examined at every level, from macroevolutionary patterns of diversification to molecular population genetic analyses of specific genomic regions between species pairs. Drosophila has been at the center of many of these research efforts. Though our understanding of the speciation process has grown considerably over the past few decades, very few genes have been identified that contribute to barriers to reproduction. The development of advanced molecular genetic and genomic methods provides promising avenues for the rapid discovery of more genes that contribute to speciation, particularly those involving prezygotic isolation. The continued expansion of tools and resources, especially for species other than Drosophila melanogaster, will be most effective when coupled with comparative approaches that reveal the genetic basis of reproductive isolation across a range of divergence times. Future research programs in Drosophila have high potential to answer long-standing questions in speciation. These include identifying the selective forces that contribute to divergence between populations and the genetic basis of traits that cause reproductive isolation. The latter can be expanded upon to understand how the genetic basis of reproductive isolation changes over time and whether certain pathways and genes are more commonly involved. Copyright © 2017 by the Genetics Society of America.

  11. Selective speciation improves efficacy and lowers toxicity of platinum anticancer and vanadium antidiabetic drugs. (United States)

    Doucette, Kaitlin A; Hassell, Kelly N; Crans, Debbie C


    Improving efficacy and lowering resistance to metal-based drugs can be addressed by consideration of the coordination complex speciation and key reactions important to vanadium antidiabetic drugs or platinum anticancer drugs under biological conditions. The methods of analyses vary depending on the specific metal ion chemistry. The vanadium compounds interconvert readily, whereas the reactions of the platinum compounds are much slower and thus much easier to study. However, the vanadium species are readily differentiated due to vanadium complexes differing in color. For both vanadium and platinum systems, understanding the processes as the compounds, Lipoplatin and Satraplatin, enter cells is needed to better combat the disease; there are many cellular metabolites, which may affect processing and thus the efficacy of the drugs. Examples of two formulations of platinum compounds illustrate how changing the chemistry of the platinum will result in less toxic and better tolerated drugs. The consequence of the much lower toxicity of the drug, can be readily realized because cisplatin administration requires hospital stay whereas Lipoplatin can be done in an outpatient manner. Similarly, the properties of Satraplatin allow for development of an oral drug. These forms of platinum demonstrate that the direct consequence of more selective speciation is lower side effects and cheaper administration of the anticancer agent. Therefore we urge that as the community goes forward in development of new drugs, control of speciation chemistry will be considered as one of the key strategies in the future development of anticancer drugs. Copyright © 2016 Elsevier Inc. All rights reserved.

  12. Speciation Dynamics of Phosphorus during (Hydro)Thermal Treatments of Sewage Sludge. (United States)

    Huang, Rixiang; Tang, Yuanzhi


    (Hydro)thermal treatments of sewage sludge from wastewater treatment process can significantly reduce waste volume and transform sludge into valuable products such as pyrochar and hydrochar. Given the global concern with phosphorus (P) resource depletion, P recycling/reclamation from or direct soil application of the derived chars can be potential P recycling practices. In order to evaluate P recyclability as well as the selection and optimization of treatment techniques, it is critical to understand the effects of different treatment techniques and conditions on P speciation and distribution. In the present study, we systematically characterized P speciation in chars derived from thermal (i.e., pyrolysis) and hydrothermal treatments of municipal sewage sludge using complementary chemical extraction and nuclear magnetic resonance (NMR) spectroscopy methods. P species in the raw activated sludge was dominated by orthophosphate and long-chain polyphosphates, whereas increased amounts of pyrophosphate and short-chain polyphosphates formed after pyrolysis at 250-600 °C. In contrast, hydrothermal treatments resulted in the production of only inorganic orthophosphate in the hydrochar. In addition to the change of molecular speciation, thermal treatments also altered the physical state and extractability of different P species in the pyrochars from pyrolysis, with both total P and polyphosphate being less extractable with increasing pyrolysis temperature. Results from this study suggest that P speciation and availability in sludge-derived chars are tunable by varying treatment techniques and conditions, and provide fundamental knowledge basis for the design and selection of waste management strategies for better nutrient (re)cycling and reclamation.

  13. Bayesian Estimation of Speciation and Extinction from Incomplete Fossil Occurrence Data (United States)

    Silvestro, Daniele; Schnitzler, Jan; Liow, Lee Hsiang; Antonelli, Alexandre; Salamin, Nicolas


    The temporal dynamics of species diversity are shaped by variations in the rates of speciation and extinction, and there is a long history of inferring these rates using first and last appearances of taxa in the fossil record. Understanding diversity dynamics critically depends on unbiased estimates of the unobserved times of speciation and extinction for all lineages, but the inference of these parameters is challenging due to the complex nature of the available data. Here, we present a new probabilistic framework to jointly estimate species-specific times of speciation and extinction and the rates of the underlying birth-death process based on the fossil record. The rates are allowed to vary through time independently of each other, and the probability of preservation and sampling is explicitly incorporated in the model to estimate the true lifespan of each lineage. We implement a Bayesian algorithm to assess the presence of rate shifts by exploring alternative diversification models. Tests on a range of simulated data sets reveal the accuracy and robustness of our approach against violations of the underlying assumptions and various degrees of data incompleteness. Finally, we demonstrate the application of our method with the diversification of the mammal family Rhinocerotidae and reveal a complex history of repeated and independent temporal shifts of both speciation and extinction rates, leading to the expansion and subsequent decline of the group. The estimated parameters of the birth-death process implemented here are directly comparable with those obtained from dated molecular phylogenies. Thus, our model represents a step towards integrating phylogenetic and fossil information to infer macroevolutionary processes. PMID:24510972

  14. Kinetic speciation of nickel in mining and municipal effluents

    Energy Technology Data Exchange (ETDEWEB)

    Chakraborty, Parthasarathi; Gopalapillai, Yamini; Fasfous, Ismail I.; Chakrabarti, Chuni L. [Carleton University, Ottawa-Carleton Chemistry Institute, Department of Chemistry, Ottawa, ON (Canada); Murimboh, John [Acadia University, Department of Chemistry, Wolfville, Nova Scotia (Canada)


    This study presents the results of kinetic speciation of nickel in undiluted mining and municipal effluents and effluents diluted with receiving freshwaters from the surrounding environment. The dilution ratios used for the dilution of the effluents were arbitrarily chosen, but were representative of the prevailing mining practices. The purpose of the this dilution was to mimic dilution with natural waters that result from dilution of the mining and municipal effluents with receiving freshwaters, so that this study would reveal environmental realities that are of concern to the managers and regulators of water resources. Ligand exchange kinetics using the competing ligand exchange method (CLEM) was studied using two independent techniques: graphite furnace atomic absorption spectrometry (GFAAS) with Chelex 100 resin as the competing ligand, and adsorptive cathodic stripping voltammetry (AdCSV) with dimethylglyoxime (DMG) as the competing ligand to determine the percentage of Ni metal released from Ni(II)-DOC complexes and the rate of dissociation of Ni(II)-DOC complexes. Using a sample containing a mixture of 30% Copper Cliff Mine effluent, 40% Sudbury municipal effluent and 30% Vermillion River water, both techniques gave results showing that the dilution of the effluent samples increased the percentage of nickel released from Ni(II)-DOC complexes. This increase in the release of nickel from the Ni(II)-DOC complexes may be of concern to managers and regulators of water resources. Agreement between the results of these two techniques has enhanced the validity of the competing ligand exchange method used by both techniques. (orig.)

  15. Determination of Tolterodine tartrate in bulk and formulation by ...

    African Journals Online (AJOL)

    ... quantification (LOQ) of the method were 0.08 and 1 μg mL-1, respectively. Conclusion: The developed method is validated and has high recovery and precision, and thus is suitable for routine analysis of the drug in bulk and formulations. Keywords: Tolterodine, Tropaeolin, Extractive colorimetry, Validation, Solid dosage ...

  16. Efficient Bulk Operations on Dynamic R-Trees

    DEFF Research Database (Denmark)

    Arge, Lars Allan; Hinrichs, Klaus; Vahrenhold, Jan


    present our technique in terms of the so-called R-tree and its variants, as they have emerged as practically efficient indexing methods for spatial data. Our method uses ideas from the buffer tree lazy buffering technique and fully utilizes the available internal memory and the page size of the operating...... best known bulk update methods with respect to update time, and that it produces a better quality index in terms of query performance. One important novel feature of our technique is that in most cases it allows us to perform a batch of updates and queries simultaneously. To be able to do so...... intensively in the database community. The continuous arrival of massive amounts of new data makes it important to update existing indexes (bulk updating ) efficiently. In this paper we present a simple, yet efficient, technique for performing bulk update and query operations on multidimensional indexes. We...

  17. Generation and Stability of Bulk Nanobubbles. (United States)

    Oh, Seung Hoon; Kim, Jong-Min


    Recently, extremely small bubbles, referred to as nanobubbles, have drawn increased attention due to their novel properties and great potential for various applications. In this study, a novel method for the generation of bulk nanobubbles (BNBs) was introduced, and stability of fabricated BNBs was investigated. BNBs were created from CO2 gas with a mixing method; the chemical identity and phase state of these bubbles can be determined via infrared spectroscopy. The presence of BNBs was observed with a nanoparticle tracking analysis (NTA). The ATR-FTIR spectra of BNBs indicate that the BNBs were filled with CO2 gas. Furthermore, the BNB concentration and its ζ-potential were about 2.94 × 108 particles/mL and -20 mV, respectively (24 h after BNB generation with a mixing time of 120 min). This indicates the continued existence and stability of BNBs in water for an extended period of time.

  18. Sediment phosphorus speciation and mobility under dynamic redox conditions (United States)

    Parsons, Chris T.; Rezanezhad, Fereidoun; O'Connell, David W.; Van Cappellen, Philippe


    Anthropogenic nutrient enrichment has caused phosphorus (P) accumulation in many freshwater sediments, raising concerns that internal loading from legacy P may delay the recovery of aquatic ecosystems suffering from eutrophication. Benthic recycling of P strongly depends on the redox regime within surficial sediment. In many shallow environments, redox conditions tend to be highly dynamic as a result of, among others, bioturbation by macrofauna, root activity, sediment resuspension and seasonal variations in bottom-water oxygen (O2) concentrations. To gain insight into the mobility and biogeochemistry of P under fluctuating redox conditions, a suspension of sediment from a hypereutrophic freshwater marsh was exposed to alternating 7-day periods of purging with air and nitrogen gas (N2), for a total duration of 74 days, in a bioreactor system. We present comprehensive data time series of bulk aqueous- and solid-phase chemistry, solid-phase phosphorus speciation and hydrolytic enzyme activities demonstrating the mass balanced redistribution of P in sediment during redox cycling. Aqueous phosphate concentrations remained low ( ˜ 2.5 µM) under oxic conditions due to sorption to iron(III) oxyhydroxides. During anoxic periods, once nitrate was depleted, the reductive dissolution of iron(III) oxyhydroxides released P. However, only 4.5 % of the released P accumulated in solution while the rest was redistributed between the MgCl2 and NaHCO3 extractable fractions of the solid phase. Thus, under the short redox fluctuations imposed in the experiments, P remobilization to the aqueous phase remained relatively limited. Orthophosphate predominated at all times during the experiment in both the solid and aqueous phase. Combined P monoesters and diesters accounted for between 9 and 16 % of sediment particulate P. Phosphatase activities up to 2.4 mmol h-1 kg-1 indicated the potential for rapid mineralization of organic P (Po), in particular during periods of aeration when the

  19. Handling of bulk solids theory and practice

    CERN Document Server

    Shamlou, P A


    Handling of Bulk Solids provides a comprehensive discussion of the field of solids flow and handling in the process industries. Presentation of the subject follows classical lines of separate discussions for each topic, so each chapter is self-contained and can be read on its own. Topics discussed include bulk solids flow and handling properties; pressure profiles in bulk solids storage vessels; the design of storage silos for reliable discharge of bulk materials; gravity flow of particulate materials from storage vessels; pneumatic transportation of bulk solids; and the hazards of solid-mater

  20. Bulk magnetic domain stability controls paleointensity fidelity (United States)

    Paterson, Greig A.; Muxworthy, Adrian R.; Yamamoto, Yuhji; Pan, Yongxin


    Nonideal, nonsingle-domain magnetic grains are ubiquitous in rocks; however, they can have a detrimental impact on the fidelity of paleomagnetic records—in particular the determination of ancient magnetic field strength (paleointensity), a key means of understanding the evolution of the earliest geodynamo and the formation of the solar system. As a consequence, great effort has been expended to link rock magnetic behavior to paleointensity results, but with little quantitative success. Using the most comprehensive rock magnetic and paleointensity data compilations, we quantify a stability trend in hysteresis data that characterizes the bulk domain stability (BDS) of the magnetic carriers in a paleomagnetic specimen. This trend is evident in both geological and archeological materials that are typically used to obtain paleointensity data and is therefore pervasive throughout most paleomagnetic studies. Comparing this trend to paleointensity data from both laboratory and historical experiments reveals a quantitative relationship between BDS and paleointensity behavior. Specimens that have lower BDS values display higher curvature on the paleointensity analysis plot, which leads to more inaccurate results. In-field quantification of BDS therefore reflects low-field bulk remanence stability. Rapid hysteresis measurements can be used to provide a powerful quantitative method for preselecting paleointensity specimens and postanalyzing previous studies, further improving our ability to select high-fidelity recordings of ancient magnetic fields. BDS analyses will enhance our ability to understand the evolution of the geodynamo and can help in understanding many fundamental Earth and planetary science questions that remain shrouded in controversy.

  1. Epigenetic inheritance, genetic assimilation and speciation. (United States)

    Pál, C; Miklós, I


    Epigenetic inheritance systems enable the environmentally induced phenotypes to be transmitted between generations. Jablonka and Lamb (1991, 1995) proposed that these systems have a substantial role during speciation. They argued that divergence of isolated populations may be first triggered by the accumulation of (heritable) phenotypic differences that are later followed and strengthened by genetic changes. The plausibility of this idea is examined in this paper. At first, we discuss the "exploratory" behaviour of an epigenetic inheritance system on a one peak adaptive landscape. If a quantitative trait is far from the optimum, then it is advantageous to induce heritable phenotypic variation. Conversely, if the genotypes get closer to the peak, it is more favorable to canalize the phenotypic expression of the character. This process would lead to genetic assimilation. Next we show that the divergence of heritable epigenetic marks acts to reduce or to eliminate the genetic barrier between two adaptive peaks. Therefore, an epigenetic inheritance system can increase the probability of transition from one adaptive state to another. Peak shift might be initiated by (i) slight changes in the inducing environment or by (ii) genetic drift of the genes controlling epigenetic variability. Remarkably, drift-induced transition is facilitated even if phenotypic variation is not heritable. A corollary of our thesis is that evolution can proceed through suboptimal phenotypic states, without passing through a deep adaptive valley of the genotype. We also consider the consequences of this finding on the dynamics and mode of reproductive isolation. Copyright 1999 Academic Press.

  2. Arsenic speciation and reactivity in poultry litter (United States)

    Arai, Y.; Lanzirotti, A.; Sutton, S.; Davis, J.A.; Sparks, D.L.


    Recent U.S. government action to lower the maximum concentration levels (MCL) of total arsenic (As) (10 ppb) in drinking water has raised serious concerns about the agricultural use of As-containing biosolids such as poultry litter (PL). In this study, solid-state chemical speciation, desorbability, and total levels of As in PL and long-term amended soils were investigated using novel synchrotronbased probing techniques (microfocused (??) synchrotron X-ray fluorescence (SXRF) and ??-X-ray absorption near-edge structure (XANES) spectroscopies) coupled with chemical digestion and batch experiments. The total As levels in the PL were as high as ???50 mg kg-1, and As(II/III and V) was always concentrated in abundant needle-shaped microscopic particles (???20/ ??m x 850 ??m) associated with Ca, Cu, and Fe and to a lesser extent with S, CI, and Zn. Postedge XANES features of litter particles are dissimilar to those of the organo-As(V) compound in poultry feed (i.e., roxarsone), suggesting possible degradation/transformation of roxarsone in the litter and/or in poultry digestive tracts. The extent of As desorption from the litter increased with increasing time and pH from 4.5 to 7, but at most 15% of the total As was released after 5 d at pH 7, indicating the presence of insoluble phases and/or strongly retained soluble compounds. No significant As accumulation (effects on As contamination in surrounding soilwater environments.

  3. Speciation trajectories in recombining bacterial species.

    Directory of Open Access Journals (Sweden)

    Pekka Marttinen


    Full Text Available It is generally agreed that bacterial diversity can be classified into genetically and ecologically cohesive units, but what produces such variation is a topic of intensive research. Recombination may maintain coherent species of frequently recombining bacteria, but the emergence of distinct clusters within a recombining species, and the impact of habitat structure in this process are not well described, limiting our understanding of how new species are created. Here we present a model of bacterial evolution in overlapping habitat space. We show that the amount of habitat overlap determines the outcome for a pair of clusters, which may range from fast clonal divergence with little interaction between the clusters to a stationary population structure, where different clusters maintain an equilibrium distance between each other for an indefinite time. We fit our model to two data sets. In Streptococcus pneumoniae, we find a genomically and ecologically distinct subset, held at a relatively constant genetic distance from the majority of the population through frequent recombination with it, while in Campylobacter jejuni, we find a minority population we predict will continue to diverge at a higher rate. This approach may predict and define speciation trajectories in multiple bacterial species.

  4. Estimating bulk density of compacted grains in storage bins and modifications of Janssen's load equations as affected by bulk density. (United States)

    Haque, Ekramul


    Janssen created a classical theory based on calculus to estimate static vertical and horizontal pressures within beds of bulk corn. Even today, his equations are widely used to calculate static loadings imposed by granular materials stored in bins. Many standards such as American Concrete Institute (ACI) 313, American Society of Agricultural and Biological Engineers EP 433, German DIN 1055, Canadian Farm Building Code (CFBC), European Code (ENV 1991-4), and Australian Code AS 3774 incorporated Janssen's equations as the standards for static load calculations on bins. One of the main drawbacks of Janssen's equations is the assumption that the bulk density of the stored product remains constant throughout the entire bin. While for all practical purposes, this is true for small bins; in modern commercial-size bins, bulk density of grains substantially increases due to compressive and hoop stresses. Over pressure factors are applied to Janssen loadings to satisfy practical situations such as dynamic loads due to bin filling and emptying, but there are limited theoretical methods available that include the effects of increased bulk density on the loadings of grain transmitted to the storage structures. This article develops a mathematical equation relating the specific weight as a function of location and other variables of materials and storage. It was found that the bulk density of stored granular materials increased with the depth according to a mathematical equation relating the two variables, and applying this bulk-density function, Janssen's equations for vertical and horizontal pressures were modified as presented in this article. The validity of this specific weight function was tested by using the principles of mathematics. As expected, calculations of loads based on the modified equations were consistently higher than the Janssen loadings based on noncompacted bulk densities for all grain depths and types accounting for the effects of increased bulk densities

  5. In-situ identification of iron electrocoagulation speciation and application for natural organic matter (NOM) removal. (United States)

    Dubrawski, Kristian L; Mohseni, Madjid


    In this work, iron speciation in electrocoagulation (EC) was studied to determine the impact of operating parameters on natural organic matter (NOM) removal from natural water. Two electrochemical EC parameters, current density (i) and charge loading rate (CLR), were investigated. Variation of these parameters led to a near unity current efficiency (φ = 0.957 ± 0.03), at any combination of i in a range of 1-25 mA/cm(2) and CLR in a range of 12-300 C/L/min. Higher i and CLR led to a higher bulk pH and limited the amount of dissolved oxygen (DO) reduced at the cathode surface due to mass transfer limitations. A low i (1 mA/cm(2)) and intermediate CLR (60 C/L/min) resulted in low bulk DO (NOM removal of the three identified species was compared, with conditions leading to GR formation showing the greatest dissolved organic carbon removal, and highest removal of the low apparent molecular weight (NOM fraction, determined by high performance size exclusion chromatography. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Speciation of organic aerosols in the Saharan Air Layer and in the free troposphere westerlies (United States)

    García, M. Isabel; van Drooge, Barend L.; Rodríguez, Sergio; Alastuey, Andrés


    We focused this research on the composition of the organic aerosols transported in the two main airflows of the subtropical North Atlantic free troposphere: (i) the Saharan Air Layer - the warm, dry and dusty airstream that expands from North Africa to the Americas at subtropical and tropical latitudes - and (ii) the westerlies, which flow from North America over the North Atlantic at mid- and subtropical latitudes. We determined the inorganic compounds (secondary inorganic species and elemental composition), elemental carbon and the organic fraction (bulk organic carbon and organic speciation) present in the aerosol collected at Izaña Observatory, ˜ 2400 m a.s.l. on the island of Tenerife. The concentrations of all inorganic and almost all organic compounds were higher in the Saharan Air Layer than in the westerlies, with bulk organic matter concentrations within the range 0.02-4.0 µg m-3. In the Saharan Air Layer, the total aerosol population was by far dominated by dust (93 % of bulk mass), which was mixed with secondary inorganic pollutants ( alkanes, hopanes, polycyclic aromatic hydrocarbons and those formed after oxidation of α-pinene and isoprene, determined by gas chromatography coupled with mass spectrometry) accounted for 15 % of the bulk organic matter (determined by the thermo-optical transmission technique); the most abundant organic compounds were saccharides (associated with surface soils), secondary organic aerosols linked to oxidation of biogenic isoprene (SOA ISO) and dicarboxylic acids (linked to several primary sources and SOA). When the Saharan Air Layer shifted southward, Izaña was within the westerlies stream and organic matter accounted for ˜ 28 % of the bulk mass of aerosols. In the westerlies, the organic aerosol species determined accounted for 64 % of the bulk organic matter, with SOA ISO and dicarboxylic acids being the most abundant; the highest concentration of organic matter (3.6 µg m-3) and of some organic species (e

  7. Speciation of cadmium mixed ligand complexes in salt water lakes

    Directory of Open Access Journals (Sweden)

    John L. Kituyi


    Full Text Available Amalgam voltammetry has been used to study heavy metal interaction in model lake water in KNO3 at 23 oC at concentration levels of genuine lake water. The hanging drop amalgam electrode was prepared in situ before exchanging the medium for the sample solution. Half-wave potentials at two metal ion concentrations were measured, one at the actual concentration in the lake while the other at a much lower one. The experimentally determined shifts in half-wave potentials are used to compute several formation constants. At the natural [CO32-] of 0.5 M in the lake, the main contributor to the speciation of cadmium is [Cd(CO3Cl2]2-. At high [Cd2+], the DPASV detects the presence of free Cd2+ ions, hence, potential polluting effect, while the amalgam reports [Cd(CO32Cl] 3- to be dominant above [CO32-] = 0.8 M. There is a variation in the number of complexes detected, their stabilities and percentage distribution in the two methods. Cd2+ ion concentration also affects the number of complexes formed and their stabilities.

  8. Prevalence of contagious mastitis pathogens in bulk tank milk in Prince Edward Island. (United States)

    Olde Riekerink, Richard G M; Barkema, Herman W; Veenstra, Stefan; Poole, Doris E; Dingwell, Randy T; Keefe, Gregory P


    The purpose of this study was to 1) estimate the herd prevalence of contagious mastitis pathogens in bulk milk from Prince Edward Island (PEI) dairy farms, 2) determine the association between bulk milk culture results and mean bulk milk somatic cell count (BMSCC), and 3) investigate the agreement of repeated bulk milk cultures. Three consecutive bulk milk samples were obtained at weekly intervals from all 258 PEI dairy herds and were cultured using routine laboratory methods. Cumulative prevalence of Staphylococcus aureus, Streptococcus agalactiae, and Mycoplasma spp. (M. bovis and M. alkalescens) was 74%, 1.6%, and 1.9%, respectively. Bulk milk somatic cell count of Staph. aureus-positive herds was higher than that of negative herds. Agreement for Staph. aureus isolation between 3 consecutive tests was moderate (kappa = 0.46). Mycoplasma bovis and M. alkalescens in bulk milk are being reported for the 1st time in PEI ever and in Canada since 1972.

  9. 1,10-Phenanthroline Modulated Redox Potentials Explored for Benign Iron Speciation Analysis


    Rizvi, Masood Ahmad; Teshima, Norio; Peerzada, Ghulam Mustafa


    The objective of this study is to develop a simple, environmentally benign alternate analytical method for simultaneous estimation of iron oxidation states. This proposed method of iron speciation is based on 1,10-phenanthroline (phen) modified redox potential of transition metal ions. In a pre-step ex¬cess cerium(IV) oxidizes iron(II) in sample to iron(III). Initial back titration of un-reacted cerium(IV) with cobalt(II) in presence of phen gives amount of iron(II) in sample, reduction of ir...

  10. Analytical tools for speciation in the field of toxicology

    Energy Technology Data Exchange (ETDEWEB)

    Bresson, C. [CEA, DEN, DPC, SEARS, Gif-sur-Yvette (France). Laboratoire de Developpement Analytique Nucleaire, Isotopique et Elementaire; Chartier, F. [CEA, DEN, Gif-sur-Yvette (France). Dept. de Physico-Chimie; Ansoborlo, E. [CEA, DEN, DRCP, CETAMA, Marcoule, Bagnols-sur-ceze (France); Ortega, R. [Bordeaux Univ., CENBG, UMR 5797, Gradignan (France); CNRS, IN2P3, CENBG, UMR 5797, Gradignan (France)


    The knowledge of the speciation of elements at trace and ultra-trace level, in biological and environmental media is essential to acquire a better understanding of the mechanisms of toxicity, transport and accumulation in which they are involved. Determining the speciation of an element in a given medium is challenging and requires the knowledge of different methodological approaches: the calculation approach and the experimental approach through the use of dedicated analytical and spectroscopic tools. In this framework, this mini-review reports the approaches to investigate the speciation of elements in biological and environmental media as well as the experimental techniques of speciation analysis, illustrated by recent examples. The main analytical and spectroscopic techniques to obtain structural, molecular, elemental and isotopic information are described. A brief overview of separation techniques coupled with spectrometric techniques is given. Imaging and micro-localisation techniques, which aim at determining the in situ spatial distribution of elements and molecules in various solid samples, are also presented. The last part deals with the development of micro-analytical systems, since they open crucial perspectives to speciation analysis for low sample amounts and analysis on field. (orig.)

  11. Genomics of Rapid Incipient Speciation in Sympatric Threespine Stickleback.

    Directory of Open Access Journals (Sweden)

    David A Marques


    Full Text Available Ecological speciation is the process by which reproductively isolated populations emerge as a consequence of divergent natural or ecologically-mediated sexual selection. Most genomic studies of ecological speciation have investigated allopatric populations, making it difficult to infer reproductive isolation. The few studies on sympatric ecotypes have focused on advanced stages of the speciation process after thousands of generations of divergence. As a consequence, we still do not know what genomic signatures of the early onset of ecological speciation look like. Here, we examined genomic differentiation among migratory lake and resident stream ecotypes of threespine stickleback reproducing in sympatry in one stream, and in parapatry in another stream. Importantly, these ecotypes started diverging less than 150 years ago. We obtained 34,756 SNPs with restriction-site associated DNA sequencing and identified genomic islands of differentiation using a Hidden Markov Model approach. Consistent with incipient ecological speciation, we found significant genomic differentiation between ecotypes both in sympatry and parapatry. Of 19 islands of differentiation resisting gene flow in sympatry, all were also differentiated in parapatry and were thus likely driven by divergent selection among habitats. These islands clustered in quantitative trait loci controlling divergent traits among the ecotypes, many of them concentrated in one region with low to intermediate recombination. Our findings suggest that adaptive genomic differentiation at many genetic loci can arise and persist in sympatry at the very early stage of ecotype divergence, and that the genomic architecture of adaptation may facilitate this.

  12. Sexual selection drives speciation in an Amazonian frog (United States)

    Boul, K.E.; Funk, W.C.; Darst, C.R.; Cannatella, D.C.; Ryan, M.J.


    One proposed mechanism of speciation is divergent sexual selection, whereby divergence in female preferences and male signals results in behavioural isolation. Despite the appeal of this hypothesis, evidence for it remains inconclusive. Here, we present several lines of evidence that sexual selection is driving behavioural isolation and speciation among populations of an Amazonian frog (Physalaemus petersi). First, sexual selection has promoted divergence in male mating calls and female preferences for calls between neighbouring populations, resulting in strong behavioural isolation. Second, phylogenetic analysis indicates that populations have become fixed for alternative call types several times throughout the species' range, and coalescent analysis rejects genetic drift as a cause for this pattern, suggesting that this divergence is due to selection. Finally, gene flow estimated with microsatellite loci is an average of 30 times lower between populations with different call types than between populations separated by a similar geographical distance with the same call type, demonstrating genetic divergence and incipient speciation. Taken together, these data provide strong evidence that sexual selection is driving behavioural isolation and speciation, supporting sexual selection as a cause for speciation in the wild. ?? 2006 The Royal Society.

  13. On the origin of species by sympatric speciation (United States)

    Dieckmann, Ulf; Doebeli, Michael


    Understanding speciation is a fundamental biological problem. It is believed that many species originated through allopatric divergence, where new species arise from geographically isolated populations of the same ancestral species. In contrast, the possibility of sympatric speciation (in which new species arise without geographical isolation) has often been dismissed, partly because of theoretical difficulties,. Most previous models analysing sympatric speciation concentrated on particular aspects of the problem while neglecting others. Here we present a model that integrates a novel combination of different features and show that sympatric speciation is a likely outcome of competition for resources. We use multilocus genetics to describe sexual reproduction in an individual-based model, and we consider the evolution of assortative mating (where individuals mate preferentially with like individuals) depending either on an ecological character affecting resource use or on a selectively neutral marker trait. In both cases, evolution of assortative mating often leads to reproductive isolation between ecologically diverging subpopulations. When assortative mating depends on a marker trait, and is therefore not directly linked to resource competition, speciation occurs when genetic drift breaks the linkage equilibrium between the marker and the ecological trait. Our theory conforms well with mounting empirical evidence for the sympatric origin of many species.

  14. Song evolution, speciation, and vocal learning in passerine birds. (United States)

    Mason, Nicholas A; Burns, Kevin J; Tobias, Joseph A; Claramunt, Santiago; Seddon, Nathalie; Derryberry, Elizabeth P


    Phenotypic divergence can promote reproductive isolation and speciation, suggesting a possible link between rates of phenotypic evolution and the tempo of speciation at multiple evolutionary scales. To date, most macroevolutionary studies of diversification have focused on morphological traits, whereas behavioral traits─including vocal signals─are rarely considered. Thus, although behavioral traits often mediate mate choice and gene flow, we have a limited understanding of how behavioral evolution contributes to diversification. Furthermore, the developmental mode by which behavioral traits are acquired may affect rates of behavioral evolution, although this hypothesis is seldom tested in a phylogenetic framework. Here, we examine evidence for rate shifts in vocal evolution and speciation across two major radiations of codistributed passerines: one oscine clade with learned songs (Thraupidae) and one suboscine clade with innate songs (Furnariidae). We find that evolutionary bursts in rates of speciation and song evolution are coincident in both thraupids and furnariids. Further, overall rates of vocal evolution are higher among taxa with learned rather than innate songs. Taken together, these findings suggest an association between macroevolutionary bursts in speciation and vocal evolution, and that the tempo of behavioral evolution can be influenced by variation in developmental modes among lineages. © 2016 The Author(s). Evolution © 2016 The Society for the Study of Evolution.

  15. Female mate-choice behavior and sympatric speciation. (United States)

    Verzijden, Machteld N; Lachlan, Robert F; Servedio, Maria R


    Many models have investigated how the process of speciation may occur in sympatry. In these models, individuals are either asexual or mate choice is determined by very simple rules. Females, for example, may be assumed either to compare their phenotype to that of a potential mate, preferring to mate with similar males (phenotype matching), or to possess preference genes that determine which male phenotype they prefer. These rules often do not reflect the mate-choice rules found in empirical studies. In this paper, we compare these two modes of female choice with various types of sexual imprinting. We examine the efficacy of different mate-choice behavior in causing divergence in male traits under simple deterministic one-locus population genetic models as well as under polygenic, individual-based simulations based on the models of Dieckmann and Doebeli (1999). We find that the inheritance mechanism of mate choice can have a large effect on the ease of sympatric speciation. When females imprint on their mothers, the result of the model is similar to phenotype matching, where speciation can occur fairly easily. When females imprint on their fathers or imprint obliquely, speciation becomes considerably less likely. Finally, when females rely on preference genes, male trait evolution occurs easily, but the correlation between trait and preference can be weak, and interpreting these results as speciation may be suspect.

  16. Ephemeral ecological speciation and the latitudinal biodiversity gradient. (United States)

    Cutter, Asher D; Gray, Jeremy C


    The richness of biodiversity in the tropics compared to high-latitude parts of the world forms one of the most globally conspicuous patterns in biology, and yet few hypotheses aim to explain this phenomenon in terms of explicit microevolutionary mechanisms of speciation and extinction. We link population genetic processes of selection and adaptation to speciation and extinction by way of their interaction with environmental factors to drive global scale macroecological patterns. High-latitude regions are both cradle and grave with respect to species diversification. In particular, we point to a conceptual equivalence of "environmental harshness" and "hard selection" as eco-evolutionary drivers of local adaptation and ecological speciation. By describing how ecological speciation likely occurs more readily at high latitudes, with such nascent species especially prone to extinction by fusion, we derive the ephemeral ecological speciation hypothesis as an integrative mechanistic explanation for latitudinal gradients in species turnover and the net accumulation of biodiversity. © 2016 The Author(s). Evolution © 2016 The Society for the Study of Evolution.

  17. Kinetic speciation and bioavailability of copper and nickel in mangrove sediments

    Digital Repository Service at National Institute of Oceanography (India)

    Chakraborty, P.; Chakraborty, S.; Ramteke, D.; Chennuri, K.

    An attempt was made to establish a mechanistic linkage between chemical speciation of copper and nickel, and their bioavailability in mangrove ecosystem. Kinetic speciation study was performed to determine the concentrations of labile metal...

  18. Enhanced bulk heterojunction devices prepared by thermal and solvent vapor annealing processes

    Energy Technology Data Exchange (ETDEWEB)

    Forrest, Stephen R.; Thompson, Mark E.; Wei, Guodan; Wang, Siyi


    A method of preparing a bulk heterojunction organic photovoltaic cell through combinations of thermal and solvent vapor annealing are described. Bulk heterojunction films may prepared by known methods such as spin coating, and then exposed to one or more vaporized solvents and thermally annealed in an effort to enhance the crystalline nature of the photoactive materials.

  19. Coupling brane fields to bulk supergravity

    Energy Technology Data Exchange (ETDEWEB)

    Parameswaran, Susha L. [Uppsala Univ. (Sweden). Theoretical Physics; Schmidt, Jonas [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)


    In this note we present a simple, general prescription for coupling brane localized fields to bulk supergravity. We illustrate the procedure by considering 6D N=2 bulk supergravity on a 2D orbifold, with brane fields localized at the fixed points. The resulting action enjoys the full 6D N=2 symmetries in the bulk, and those of 4D N=1 supergravity at the brane positions. (orig.)

  20. Evolution of uranium distribution and speciation in mill tailings, COMINAK Mine, Niger

    Energy Technology Data Exchange (ETDEWEB)

    Déjeant, Adrien, E-mail: [Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie, Case 115, 4 place Jussieu, 75005 Paris (France); Université Paris Diderot — Paris VII, 5 rue Thomas Mann, 75013 Paris (France); Galoisy, Laurence [Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie, Case 115, 4 place Jussieu, 75005 Paris (France); Université Pierre et Marie Curie — Paris VI, 4 place Jussieu, 75005 Paris (France); Roy, Régis [AREVA Mines — Geoscience Department, Tour AREVA, 1 place Jean Millier, 92084 Paris, La Défense (France); Calas, Georges; Boekhout, Flora [Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie, Case 115, 4 place Jussieu, 75005 Paris (France); Université Pierre et Marie Curie — Paris VI, 4 place Jussieu, 75005 Paris (France); Phrommavanh, Vannapha; Descostes, Michael [AREVA Mines — R& D Department, BAL 0414C-2, Tour AREVA, 1 place Jean Millier, 92084 Paris, La Défense (France)


    This study investigated the evolution of uranium distribution and speciation in mill tailings from the COMINAK mine (Niger), in production since 1978. A multi-scale approach was used, which combined high resolution remote sensing imagery, ICP-MS bulk rock analyses, powder X-ray diffraction, Scanning Electron Microscopy, Focused Ion Beam — Transmission Electron Microscopy and X-ray Absorption Near Edge Spectroscopy. Mineralogical analyses showed that some ore minerals, including residual uraninite and coffinite, undergo alteration and dissolution during tailings storage. The migration of uranium and other contaminants depends on (i) the chemical stability of secondary phases and sorbed species (dissolution and desorption processes), and (ii) the mechanical transport of fine particles bearing these elements. Uranium is stabilized after formation of secondary uranyl sulfates and phosphates, and adsorbed complexes on mineral surfaces (e.g. clay minerals). In particular, the stock of insoluble uranyl phosphates increases with time, thus contributing to the long-term stabilization of uranium. At the surface, a sulfate-cemented duricrust is formed after evaporation of pore water. This duricrust limits water infiltration and dust aerial dispersion, though it is enriched in uranium and many other elements, because of pore water rising from underlying levels by capillary action. Satellite images provided a detailed description of the tailings pile over time and allow monitoring of the chronology of successive tailings deposits. Satellite images suggest that uranium anomalies that occur at deep levels in the pile are most likely former surface duricrusts that have been buried under more recent tailings. - Highlights: • The evolution of U distribution and speciation in mill tailings is investigated. • High resolution satellite images provide useful information on tailings evolution. • U and many other elements are enriched in a sulfate-rich duricrust. • Formation of

  1. Rapid acceleration of plant speciation during the Anthropocene. (United States)

    Thomas, Chris D


    Speciation rates need to be considered when estimating human impacts on the numbers of species on Earth, given that past mass extinctions have been followed by the accelerated origination of new taxa. Here, I suggest that the Anthropocene is already exhibiting a greatly accelerated plant speciation rate due to agriculture, horticulture, and the human-mediated transport of species, followed by hybridisation. For example, more new plant species have come into existence in Europe over the past three centuries than have been documented as becoming extinct over the same period, even though most new hybrid-origin species are likely to remain undetected. Current speciation rates are unusually high and they could be higher than during or after previous mass extinctions. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Simultaneous Speciation of Arsenic, Selenium, and Chromium by HPLC-ICP-MS (United States)

    Wolf, Ruth E.; Morman, Suzette A.; Morrison, Jean M.; Lamothe, Paul J.


    An adaptation of an analytical method developed for chromium speciation has been utilized for the simultaneous determination of As(III), As(V), Se(IV), Se(VI), Cr(III), and Cr(VI) species using high performance liquid chromatography (HPLC) separation with ICP-MS detection. Reduction of interferences for the determination of As, Se, and Cr by ICP-MS is a major consideration for this method. Toward this end, a Dynamic Reaction Cell (DRC) ICP-MS system was used to detect the species eluted from the chromatographic column. A variety of reaction cell gases and conditions may be utilized, and the advantages and limitations of the gases tested to date will be presented and discussed. The separation and detection of the As, Se, and Cr species of interest can be achieved using the same chromatographic conditions in less than 2 minutes by complexing the Cr(III) with EDTA prior to injection on the HPLC column. Practical aspects of simultaneous speciation analysis will be presented and discussed, including issues with HPLC sample vial contamination, standard and sample contamination, species stability, and considerations regarding sample collection and preservation methods. The results of testing to determine the method's robustness to common concomitant element and anion effects will also be discussed. Finally, results will be presented using the method for the analysis of a variety of environmental and geological samples including waters, soil leachates and simulated bio-fluid leachates.

  3. Towards accounting for dissolved iron speciation in global ocean models

    Directory of Open Access Journals (Sweden)

    A. Tagliabue


    Full Text Available The trace metal iron (Fe is now routinely included in state-of-the-art ocean general circulation and biogeochemistry models (OGCBMs because of its key role as a limiting nutrient in regions of the world ocean important for carbon cycling and air-sea CO2 exchange. However, the complexities of the seawater Fe cycle, which impact its speciation and bioavailability, are simplified in such OGCBMs due to gaps in understanding and to avoid high computational costs. In a similar fashion to inorganic carbon speciation, we outline a means by which the complex speciation of Fe can be included in global OGCBMs in a reasonably cost-effective manner. We construct an Fe speciation model based on hypothesised relationships between rate constants and environmental variables (temperature, light, oxygen, pH, salinity and assumptions regarding the binding strengths of Fe complexing organic ligands and test hypotheses regarding their distributions. As a result, we find that the global distribution of different Fe species is tightly controlled by spatio-temporal environmental variability and the distribution of Fe binding ligands. Impacts on bioavailable Fe are highly sensitive to assumptions regarding which Fe species are bioavailable and how those species vary in space and time. When forced by representations of future ocean circulation and climate we find large changes to the speciation of Fe governed by pH mediated changes to redox kinetics. We speculate that these changes may exert selective pressure on phytoplankton Fe uptake strategies in the future ocean. In future work, more information on the sources and sinks of ocean Fe ligands, their bioavailability, the cycling of colloidal Fe species and kinetics of Fe-surface coordination reactions would be invaluable. We hope our modeling approach can provide a means by which new observations of Fe speciation can be tested against hypotheses of the processes present in governing the ocean Fe cycle in an

  4. Possible incipient sympatric ecological speciation in blind mole rats (Spalax). (United States)

    Hadid, Yarin; Tzur, Shay; Pavlícek, Tomáš; Šumbera, Radim; Šklíba, Jan; Lövy, Matěj; Fragman-Sapir, Ori; Beiles, Avigdor; Arieli, Ran; Raz, Shmuel; Nevo, Eviatar


    Sympatric speciation has been controversial since it was first proposed as a mode of speciation. Subterranean blind mole rats (Spalacidae) are considered to speciate allopatrically or peripatrically. Here, we report a possible incipient sympatric adaptive ecological speciation in Spalax galili (2n = 52). The study microsite (0.04 km(2)) is sharply subdivided geologically, edaphically, and ecologically into abutting barrier-free ecologies divergent in rock, soil, and vegetation types. The Pleistocene Alma basalt abuts the Cretaceous Senonian Kerem Ben Zimra chalk. Only 28% of 112 plant species were shared between the soils. We examined mitochondrial DNA in the control region and ATP6 in 28 mole rats from basalt and in 14 from chalk habitats. We also sequenced the complete mtDNA (16,423 bp) of four animals, two from each soil type. Remarkably, the frequency of all major haplotype clusters (HC) was highly soil-biased. HCI and HCII are chalk biased. HC-III was abundant in basalt (36%) but absent in chalk; HC-IV was prevalent in basalt (46.5%) but was low (20%) in chalk. Up to 40% of the mtDNA diversity was edaphically dependent, suggesting constrained gene flow. We identified a homologous recombinant mtDNA in the basalt/chalk studied area. Phenotypically significant divergences differentiate the two populations, inhabiting different soils, in adaptive oxygen consumption and in the amount of outside-nest activity. This identification of a possible incipient sympatric adaptive ecological speciation caused by natural selection indirectly refutes the allopatric alternative. Sympatric ecological speciation may be more prevalent in nature because of abundant and sharply abutting divergent ecologies.

  5. Running with rugby balls: bulk renormalization of codimension-2 branes (United States)

    Williams, M.; Burgess, C. P.; van Nierop, L.; Salvio, A.


    We compute how one-loop bulk effects renormalize both bulk and brane effective interactions for geometries sourced by codimension-two branes. We do so by explicitly integrating out spin-zero, -half and -one particles in 6-dimensional Einstein-Maxwell-Scalar theories compactified to 4 dimensions on a flux-stabilized 2D geometry. (Our methods apply equally well for D dimensions compactified to D - 2 dimensions, although our explicit formulae do not capture all divergences when D > 6.) The renormalization of bulk interactions are independent of the boundary conditions assumed at the brane locations, and reproduce standard heat-kernel calculations. Boundary conditions at any particular brane do affect how bulk loops renormalize this brane's effective action, but not the renormalization of other distant branes. Although we explicitly compute our loops using a rugby ball geometry, because we follow only UV effects our results apply more generally to any geometry containing codimension-two sources with conical singularities. Our results have a variety of uses, including calculating the UV sensitivity of one-loop vacuum energy seen by observers localized on the brane. We show how these one-loop effects combine in a surprising way with bulk back-reaction to give the complete low-energy effective cosmological constant, and comment on the relevance of this calculation to proposed applications of codimension-two 6D models to solutions of the hierarchy and cosmological constant problems.

  6. Confined linear carbon chains as a route to bulk carbyne (United States)

    Shi, Lei; Rohringer, Philip; Suenaga, Kazu; Niimi, Yoshiko; Kotakoski, Jani; Meyer, Jannik C.; Peterlik, Herwig; Wanko, Marius; Cahangirov, Seymur; Rubio, Angel; Lapin, Zachary J.; Novotny, Lukas; Ayala, Paola; Pichler, Thomas


    Strong chemical activity and extreme instability in ambient conditions characterize carbyne, an infinite sp1 hybridized carbon chain. As a result, much less has been explored about carbyne as compared to other carbon allotropes such as fullerenes, nanotubes and graphene. Although end-capping groups can be used to stabilize carbon chains, length limitations are still a barrier for production, and even more so for application. We report a method for the bulk production of long acetylenic linear carbon chains protected by thin double-walled carbon nanotubes. The synthesis of very long arrangements is confirmed by a combination of transmission electron microscopy, X-ray diffraction and (near-field) resonance Raman spectroscopy. Our results establish a route for the bulk production of exceptionally long and stable chains composed of more than 6,000 carbon atoms, representing an elegant forerunner towards the final goal of carbyne’s bulk production.

  7. Phylogenetic analyses of the leaf beetle genus Galerucella: evidence for host switching at speciation?

    NARCIS (Netherlands)

    Borghuis, A.; Madsen, O.; Ouborg, N.J.; Groenendael, van J.


    It is still the subject of lively debate whether sympatric speciation is a general mode of speciation as opposed to allopatric speciation. In herbivorous insects, host switching, i.e. colonization of, and adaptation to, a new host by a herbivore, has been proposed as one of the driving mechanisms of

  8. Incomplete lineage sorting patterns among human, chimpanzee and orangutan suggest recent orangutan speciation and widespread selection

    DEFF Research Database (Denmark)

    Hobolth, Asger; Dutheil, Julien; Hawks, John


    and orangutans (the speciation time) from the genetic divergence time, and we find speciation to be as recent as 9-13 mya (contingent on the calibration point). The analyses provide further support for a recent speciation of human and chimpanzee at ~4 mya and a diverse ancestor of human and chimpanzee...

  9. Speciation and bioavailability of copper in Lake Tjeukemeer


    Verweij, W.


    Chapter 1: introduction

    In this thesis an account is given of a research project dealing with the chemical speciation and bioavailability of copper in Lake Tjeukemeer, a lake in the north of the Netherlands. The reason for the initiation of this project was a lack of knowledge about the speciation of copper and the influence of copper on the behaviour of algae. This influence may be important, because copper is an essential element for algae, but becomes toxic whe...

  10. Speciation Analysis and Environmental Tracer Studies of 129I

    DEFF Research Database (Denmark)

    Zhang, Luyuan

    applied for determination of 129I in natural waters and leachates containing organic iodine species. A method has been established for speciation analysis of 129I and 127I in aerosol samples collected on polypropylene filter. Sequential extraction using water and NaOH solution was employed to extract...... water-soluble iodine (WSI) and NaOH soluble iodine (NSI), and alkaline ashing for residue insoluble aerosol iodine (RII). WSI was further partitioned to iodide and iodate using anion exchange chromatography. Parameters, such as amount of leaching agents used, leaching time, ashing time and temperature...

  11. 27 CFR 20.191 - Bulk articles. (United States)


    ... 27 Alcohol, Tobacco Products and Firearms 1 2010-04-01 2010-04-01 false Bulk articles. 20.191... Users of Specially Denatured Spirits Operations by Users § 20.191 Bulk articles. Users who convey articles in containers exceeding one gallon may provide the recipient with a photocopy of subpart G of this...

  12. Vertical changes of the Co and Mn speciation along a lateritic regolith developed on peridotites (New Caledonia) (United States)

    Dublet, Gabrielle; Juillot, Farid; Brest, Jessica; Noël, Vincent; Fritsch, Emmanuel; Proux, Olivier; Olivi, Luca; Ploquin, Florian; Morin, Guillaume


    Because they can host significant amounts of Co, the Mn-oxides are commonly considered as the major Co-bearing mineral species in lateritic environments. However, little is known about the process leading to the formation and/or the weathering of these Co-rich Mn-oxides. This lack of knowledge is mainly due to the fact that Co concentrations are too low in primary silicates for classical speciation analysis. In this study, we investigated both Co and Mn speciation in a 64 m thick lateritic regolith developed upon peridotites in New Caledonia, by combining High Energy Resolution Fluorescence Detection X-ray absorption Near Edge Structure (HERFD-XANES) spectroscopy at the Co K-edge with classical XANES spectroscopy at the Mn K-edge, bulk chemistry (ICP) and mineralogy (XRD). The results obtained provide new insights into the evolution of Co and Mn speciation as a function of the weathering stages. Co and Mn primarily occur as Co(II) and Mn(II,III) in olivine and serpentine in the bedrock. During the first weathering stage, these forms of Co and Mn are progressively oxidized toward Co(III) and Mn(III,IV), which occur mainly as Co(III)-bearing Mn(III/IV)-oxides in the transition between the saprolite and the laterite. In the uppermost lateritic horizons, long-time weathering resulted in a strong leaching of Co and Mn, and the remaining of these elements occurs as Co(II) and Mn(III) substituting for Fe(III) in goethite. This latter scavenging process emphasizes the importance of Fe-oxides for the long-term stabilization of Co and Mn in such deeply weathered laterites.

  13. Quantification of chemical sulphur species in bulk soil and organic sulphur fractions by S K-edge Xanes spectroscopy

    DEFF Research Database (Denmark)

    Boye, K; Almkvist, G; Nilsson, S I


    A new data treatment method for fitting spectra obtained by sulphur (S) K-edge X-ray absorption near-edge structure (XANES) spectroscopy was used to quantify the chemical S speciation at three experimental sites with arable soils receiving the same long-term field treatments. Two treatments, crop...

  14. Selective arsenic speciation analysis of human urine reference materials using gradient elution ion-exchange HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.


    identical with the reference values given for total arsenic. The obtained values for arsenobetaine and dimethylarsinic acid were identical with the values certified for the NIES No. 18 urine CRM. The speciation data presented here may be valuable for the quality assurance of analytical method development......-performance liquid chromatography ( HPLC) coupled with inductively coupled plasma mass spectrometry (ICP-MS). Nine arsenic species, including arsenic acid, arsenous acid, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine, trimethylarsine oxide, dimethylarsinoylacetic acid, trimethylarsoniopropionate...

  15. Room Temperature Cation Exchange Reaction in Nanocrystals for Ultrasensitive Speciation Analysis of Silver Ions and Silver Nanoparticles. (United States)

    Huang, Ke; Xu, Kailai; Tang, Jie; Yang, Lu; Zhou, Jingrong; Hou, Xiandeng; Zheng, Chengbin


    To evaluate the toxicity of silver nanoparticles (AgNPs) and Ag(+) and gain deep insight into the transformation of AgNPs in the environment or organisms, ultrasensitive analytical methods are needed for their speciation analysis. About 40-fold of Cd(2+) in CdTe ionic nanocrystals can be "bombarded-and-exploded" (exchanged) in less than 1 min simply by mixing the nanocrystals with Ag(+) solution at room temperature, while this cation exchange reaction did not occur when only silver nanoparticles were present. On the basis of this striking difference, an ultrasensitive method was developed for speciation analysis of Ag(+) and AgNPs in complex matrices. The released Cd(2+) was reduced to its volatile species by sodium tetrahydroborate, which was separated and swept to an inductively coupled plasma mass spectrometer (ICPMS) or an atomic fluorescence spectrometer (AFS) for the indirect but ultrasensitive detection of Ag(+). Owing to the remarkable signal amplification via the cation exchange reaction and the advantages of chemical vapor generation for sampling, the limit of detection was 0.0003 μg L(-1) for Ag(+) by ICPMS, which was improved by 100-fold compared to the conventional method. Relative standard deviations are better than 2.5% at a concentration of 0.5 μg L(-1) Ag(+) or AgNPs regardless of the detector. The proposed method retains several unique advantages, including ultrahigh sensitivity, speciation analysis, simplicity and being organic reagent-free, and has been successfully utilized for speciation analysis of Ag(+) and AgNPs in environmental water samples and paramecium cells.

  16. Evidence for progenitor–derivative speciation in sexually deceptive orchids (United States)

    Schlüter, Philipp M.; Ruas, Paulo M.; Kohl, Gudrun; Ruas, Claudete F.; Stuessy, Tod F.; Paulus, Hannes F.


    Background and Aims Sexually deceptive orchids of the genus Ophrys use mimicry of pollinator females to attract specific pollinators. Pollinator shifts may drive speciation in Ophrys, since novel pollinators may in principle act as isolating factors immediately. It is thus possible that evolution of novel species occurs rapidly and with a progenitor–derivative pattern. The aims of this study are to compare genetic structure and diversity among widespread and geographically restricted Ophrys taxa, to test whether genetic structure is associated with specific pollinators, and to investigate whether any widespread species may have acted as a progenitor for the evolution of more restricted taxa. Methods Genetic differentiation and diversity were investigated in O. leucadica and O. cinereophila, the two taxa of the Ophrys fusca sensu lato complex widespread in the Aegean, and three geographically restricted taxa from Rhodes, O. attaviria, O. parvula and O. persephonae, all differing in their specific pollinators. This was done using amplified fragment length polymorphism (AFLP) DNA fingerprinting, and sequencing of the low-copy nuclear gene LEAFY (LFY). Key Results All taxa were found to be separate genetic entities, with O. leucadica forming two geographic groups from the west and east of the Aegean. Genetic structure was significantly shaped by pollinators and geography, and comparison of sequence and AFLP data revealed ancestral polymorphisms shared among several taxa. Among the sampled taxa, O. leucadica harbours the greatest genetic differentiation and geographic structure, and the highest genetic diversity. Part of the genome of O. parvula, endemic to Rhodes, may be derived from O. leucadica. Conclusions Pollinators probably influence the genetic structure of the investigated Ophrys species. The genetic pattern identified is consistent with O. leucadica being the oldest of the sampled taxa, making O. leucadica a candidate progenitor species from which more

  17. Variation of heavy metal speciation during the pyrolysis of sediment collected from the Dianchi Lake, China

    Directory of Open Access Journals (Sweden)

    Zhenggang Gu


    Full Text Available Sediment samples with high organic carbon were collected from the Dianchi Lake in China and thermally treated using a method analogous to biochar production. The speciation of the heavy metals Cu, Cd, Pb, and Zn in sediment and thermally treated sediments (TTSs were analyzed by European Community Bureau of Reference (BCR sequential extraction methods. Heavy metal bioavailability and eco-toxicity were assessed by risk assessment code. This study demonstrates that BCR sequential extraction methods and risk assessment code can be used as valuable tools to assess heavy metal mobility, bioavailability and eco-toxicity. Compared to biochar derived from biomass, TTSs had different characteristics, which may contribute to the formation of organo-mineral complexes. The heavy metals Cu, Cd, Pb, and Zn speciated in TTSs show different patterns from that of the sediment and pyrolysis temperature has a great influence on the fractional distribution of heavy metals. Those different distributions may attribute to the geochemistry of the sediment and the different physicochemical characteristics of heavy metals. In order for the safe application of thermally –treatment sediments (TTSs as a soil amendment, further studies such as field experiments may be required.

  18. Book Review The Speciation and Biogeography of Birds By Ian ...

    African Journals Online (AJOL)

    Open Access DOWNLOAD FULL TEXT Subscription or Fee Access. Book Review The Speciation and Biogeography of Birds By Ian Newton (2003). Rauri CK Bowie. Abstract. Academic Press, London, Linacre House, Jordan Hill, Oxford OX2 8DP, UK, e-mail 668 pages, hardcover. ISBN 012517375X ...

  19. Speciation of Heavy Metals in Sediment of Agbabu Bitumen deposit ...

    African Journals Online (AJOL)

    Michael Horsfall

    soils and water from the vicinity of Agbabu bitumen field (Olajire et al., 2007), and solvent extraction of vanadium from Nigerian bitumen (Oguntimehin and. Ipinmoroti, 2007). The need for this research arose because no study has been reported on the speciation of metals in sediment of Agbabu bitumen deposit environment ...

  20. Bioavailability of iron speciations and EDTA-iron complexes for ...

    African Journals Online (AJOL)



    Jan 19, 2012 ... Full Length Research Paper. Bioavailability of iron speciations and EDTA-iron .... Diatoms are particularly important in the export of organic matter to the deep ocean because of their large size and ... having a costal centric diatom in the size range of 5 to 20. µm. The aim of this study was to determine the.

  1. Evolution and the latitudinal diversity gradient: speciation, extinction and biogeography. (United States)

    Mittelbach, Gary G; Schemske, Douglas W; Cornell, Howard V; Allen, Andrew P; Brown, Jonathan M; Bush, Mark B; Harrison, Susan P; Hurlbert, Allen H; Knowlton, Nancy; Lessios, Harilaos A; McCain, Christy M; McCune, Amy R; McDade, Lucinda A; McPeek, Mark A; Near, Thomas J; Price, Trevor D; Ricklefs, Robert E; Roy, Kaustuv; Sax, Dov F; Schluter, Dolph; Sobel, James M; Turelli, Michael


    A latitudinal gradient in biodiversity has existed since before the time of the dinosaurs, yet how and why this gradient arose remains unresolved. Here we review two major hypotheses for the origin of the latitudinal diversity gradient. The time and area hypothesis holds that tropical climates are older and historically larger, allowing more opportunity for diversification. This hypothesis is supported by observations that temperate taxa are often younger than, and nested within, tropical taxa, and that diversity is positively correlated with the age and area of geographical regions. The diversification rate hypothesis holds that tropical regions diversify faster due to higher rates of speciation (caused by increased opportunities for the evolution of reproductive isolation, or faster molecular evolution, or the increased importance of biotic interactions), or due to lower extinction rates. There is phylogenetic evidence for higher rates of diversification in tropical clades, and palaeontological data demonstrate higher rates of origination for tropical taxa, but mixed evidence for latitudinal differences in extinction rates. Studies of latitudinal variation in incipient speciation also suggest faster speciation in the tropics. Distinguishing the roles of history, speciation and extinction in the origin of the latitudinal gradient represents a major challenge to future research.

  2. Plant evolution: pulses of extinction and speciation in gymnosperm diversity. (United States)

    Davis, Charles C; Schaefer, Hanno


    Living gymnosperms represent the survivors of ancient seed plant lineages whose fossil record reaches back 270 million years. Two recent studies find that recent pulses of extinction and speciation have shaped today's gymnosperm diversity, contradicting the widespread assumption that gymnosperms have remained largely unchanged for tens of millions of years. Copyright © 2011 Elsevier Ltd. All rights reserved.

  3. Underappreciated Consequences of Phenotypic Plasticity for Ecological Speciation

    Directory of Open Access Journals (Sweden)

    Benjamin M. Fitzpatrick


    Full Text Available Phenotypic plasticity was once seen primarily as a constraint on adaptive evolution or merely a nuisance by geneticists. However, some biologists promote plasticity as a source of novelty and a factor in evolution on par with mutation, drift, gene flow, and selection. These claims are controversial and largely untested, but progress has been made on more modest questions about effects of plasticity on local adaptation (the first component of ecological speciation. Adaptive phenotypic plasticity can be a buffer against divergent selection. It can also facilitate colonization of new niches and rapid divergent evolution. The influence of non-adaptive plasticity has been underappreciated. Non-adaptive plasticity, too can interact with selection to promote or inhibit genetic differentiation. Finally, phenotypic plasticity of reproductive characters might directly influence evolution of reproductive isolation (the second component of ecological speciation. Plasticity can cause assortative mating, but its influence on gene flow ultimately depends on maintenance of environmental similarity between parents and offspring. Examples of plasticity influencing mating and habitat choice suggest that this, too, might be an underappreciated factor in speciation. Plasticity is an important consideration for studies of speciation in nature, and this topic promises fertile ground for integrating developmental biology with ecology and evolution.

  4. The molecular basis of speciation: from patterns to processes, rules ...

    Indian Academy of Sciences (India)

    However, the large genetic and reproductive differences between taxa and the multi-factorial nature of each rule have made it difficult to ascribe general mechanisms. Here, we review the extensive progress made since Darwin on understanding the origin of species. We revisit the rules of speciation, regarding them as ...

  5. Latitude, elevational climatic zonation and speciation in New World vertebrates. (United States)

    Cadena, Carlos Daniel; Kozak, Kenneth H; Gómez, Juan Pablo; Parra, Juan Luis; McCain, Christy M; Bowie, Rauri C K; Carnaval, Ana C; Moritz, Craig; Rahbek, Carsten; Roberts, Trina E; Sanders, Nathan J; Schneider, Christopher J; VanDerWal, Jeremy; Zamudio, Kelly R; Graham, Catherine H


    Many biodiversity hotspots are located in montane regions, especially in the tropics. A possible explanation for this pattern is that the narrow thermal tolerances of tropical species and greater climatic stratification of tropical mountains create more opportunities for climate-associated parapatric or allopatric speciation in the tropics relative to the temperate zone. However, it is unclear whether a general relationship exists among latitude, climatic zonation and the ecology of speciation. Recent taxon-specific studies obtained different results regarding the role of climate in speciation in tropical versus temperate areas. Here, we quantify overlap in the climatic distributions of 93 pairs of sister species of mammals, birds, amphibians and reptiles restricted to either the New World tropics or to the Northern temperate zone. We show that elevational ranges of tropical- and temperate-zone species do not differ from one another, yet the temperature range experienced by species in the temperate zone is greater than for those in the tropics. Moreover, tropical sister species tend to exhibit greater similarity in their climatic distributions than temperate sister species. This pattern suggests that evolutionary conservatism in the thermal niches of tropical taxa, coupled with the greater thermal zonation of tropical mountains, may result in increased opportunities for allopatric isolation, speciation and the accumulation of species in tropical montane regions. Our study exemplifies the power of combining phylogenetic and spatial datasets of global climatic variation to explore evolutionary (rather than purely ecological) explanations for the high biodiversity of tropical montane regions.

  6. Geometry, charge distribution, and surface speciation of phosphate on goethite.

    NARCIS (Netherlands)

    Rahnemaie, R.; Hiemstra, T.; Riemsdijk, van W.H.


    The surface speciation of phosphate has been evaluated with surface complexation modeling using an interfacial charge distribution (CD) approach based on ion adsorption and ordering of interfacial water. In the CD model, the charge of adsorbed ions is distributed over two electrostatic potentials in

  7. Speciation of Heavy Metals in Sediment of Agbabu Bitumen deposit ...

    African Journals Online (AJOL)

    Speciation of heavy metals Cu, Cd, Pb, Ni, Zn, Mn, Fe, Cr and Hg was carried out on sediment of Agbabu with a sequential extraction procedure in the dry and rainy seasons of year 2008. Hg was not detected in all the fractions in the two seasons. In the dry season, all the metals were mostly abundant in Fraction-5, however ...

  8. Comparative Studies of the Speciation Patterns of Nickel and ...

    African Journals Online (AJOL)



    Jan 31, 2005 ... Results of speciation studies of nickel and chromium in wastewater, surface and groundwater systems using flame atomic absorption spectrometry (FAAS), graphite furnace atomic absorption spectrometry (GFAAS) and differential pulse adsorptive cathodic stripping voltammetry (DPAdCSV) are presented.

  9. speciation of heavy metals in street dust samples from sakarya

    African Journals Online (AJOL)

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    SPECIATION OF HEAVY METALS IN STREET DUST SAMPLES FROM SAKARYA. I. ORGANIZED INDUSTRIAL DISTRICT USING THE BCR SEQUENTIAL. EXTRACTION PROCEDURE BY ICP-OES. Nilufer Ozcan and Huseyin Altundag*. Sakarya University, Faculty of Arts and Sciences, Department of Chemistry, 54187, ...

  10. Speciation and determination of priority metals in sediments of Oyun ...

    African Journals Online (AJOL)

    This work was carried out to determine the concentrations, bioavailability and mobility of priority metals in sediments of Oyun River, Sango, Ilorin, Nigeria. The river sediments were sampled at six selected locations and the samples were analyzed for some certain priority metals to determine the concentration, speciation and ...

  11. Heavy metal speciation and their accumulation in sediments of Lake ...

    African Journals Online (AJOL)

    Several sediment samples in Lake Burullus have been affected by the discharges of heavy metals through different drains. The study aimed to analyze the chemical speciation of these metals. In particular, the chemical forms of Cd, Cu, Fe, Mn, Pb and Zn in sediments collected in spring season were studied using a ...

  12. Comparative Studies of the Speciation Patterns of Nickel and ...

    African Journals Online (AJOL)

    Results of speciation stdies of nickel and chromium in wastewater, surface and groundwater systems using flame atomic absorption spectrometry (FAAS), graphite furnace atomic absorption spectrometry (GFAAS) and differential pulse adsorptive cathodic stripping voltammetry (DPAdCSV) are presented. Dimethylglyoxime ...

  13. Sympatric speciation in Yponomeuta: No evidence for host plant fidelity

    NARCIS (Netherlands)

    Bakker, A.C.; Roessingh, P.; Menken, S.B.J.


    According to sympatric speciation theory, adaptation to different host plants is expected to pleiotropically lead to assortative mating, an important factor in the reduction of gene flow between the diverging subpopulations. This scenario predicts mating on and oviposition preference for the

  14. Speciation of Iberian diving beetles in Pleistocene refugia (Coleoptera, Dytiscidae). (United States)

    Ribera, Ignacio; Vogler, Alfried P


    The Mediterranean basin is an area of high diversity and endemicity, but the age and origin of its fauna are still largely unknown. Here we use species-level phylogenies based on approximately 1300 base pairs of the genes 16S rRNA and cytochrome oxidase I to establish the relationships of 27 of the 34 endemic Iberian species of diving beetles in the family Dytiscidae, and to investigate their level of divergence. Using a molecular clock approach, 18-19 of these species were estimated to be of Pleistocene origin, with four to six of them from the Late Pleistocene ( approximately 100 000 years). A second, lower speciation frequency peak was assigned to Late Miocene or Early Pliocene. Analysis of the distributional ranges showed that endemic species placed in the tip nodes of the trees are significantly more likely to be allopatric with their sisters than endemic species at lower node levels. Allopatric sister species are also significantly younger than sympatric clades, in agreement with an allopatric mode of speciation and limited subsequent range movement. These results strongly suggest that for some taxa Iberian populations were isolated during the Pleistocene long enough to speciate, and apparently did not expand their ranges to recolonize areas north of the Pyrenees. This is in contradiction to observations from fossil beetles in areas further north, which document large range movements associated with the Pleistocene glacial cycles hypothesized to suppress population isolation and allopatric speciation.

  15. Speciation of Water-Extractable Organic Nutrients in Grassland Soils

    NARCIS (Netherlands)

    Ros, G.H.; Tschudy, T.C.; Chardon, W.J.; Temminghoff, E.J.M.; Salm, van der C.; Koopmans, G.F.


    The release of dissolved organic matter (DOM) from agricultural land can have a large impact on the transport of N and phosphorus (P) to surface waters leading to water quality impairment. The speciation of DOM in agricultural grassland soils has received little attention thus far. Quantification of

  16. Electrochemical metal speciation in natural and model polyelectrolyte systems

    NARCIS (Netherlands)

    Hoop, van den M.A.G.T.


    The purpose of the research described in this thesis was to examine the applicability of electro-analytical techniques in obtaining information on the speciation of metals, i.e. their distribution over different physico-chemical forms, in aquatic systems containing charged macromolecules.

  17. Sympatric speciation in a genus of marine reef fishes. (United States)

    Crow, Karen D; Munehara, Hiroyuki; Bernardi, Giacomo


    Sympatric speciation has been contentious since its inception, yet is increasingly recognized as important based on accumulating theoretical and empirical support. Here, we present a compelling case of sympatric speciation in a taxon of marine reef fishes using a comparative and mechanistic approach. Hexagrammos otakii and H. agrammus occur in sympatry throughout their ranges. Molecular sequence data from six loci, with complete sampling of the genus, support monophyly of these sister species. Although hybridization occurs frequently with an allopatric congener in an area of slight distributional overlap, we found no F(1) hybrids between the focal sympatric taxa throughout their coextensive ranges. We present genetic evidence for complete reproductive isolation based on SNP analysis of 382 individuals indicating fixed polymorphisms, with no shared haplotypes or genotypes, between sympatric species. To address questions of speciation, we take a mechanistic approach and directly compare aspects of reproductive isolation between allopatric and sympatric taxa both in nature and in the laboratory. We conclude that the buildup of reproductive isolation is strikingly different in sympatric vs. allopatric taxa, consistent with theoretical predictions. Lab reared hybrids from allopatric species crosses exhibit severe fitness effects in the F(1) or backcross generation. No intrinsic fitness effects are observed in F(1) hybrids from sympatric species pairs, however these treatments exhibited reduced fertilization success and complete pre-mating isolation is implied in nature because F(1) hybrid adults do not occur. Our study addresses limitations of previous studies and supports new criteria for inferring sympatric speciation.

  18. Investigation on speciation and pollution index of heavy metals in ...

    African Journals Online (AJOL)

    This study investigated the chemical speciation of Cd, Cr, Cu, Ni and Pb and their contamination/pollution indices in the sediment of River Ala in Akure, Nigeria. Sediment samples taken along the course of the river were subjected to Sequential Extraction Technique and the heavy metals were quantified using atomic ...

  19. Speciation of Fe in the Eastern North Atlantic Ocean

    NARCIS (Netherlands)

    Thuroczy, C-E; Gerringa, L. J. A.; Klunder, M. B.; Middag, R.; Laan, P.; Timmermans, K. R.; de Baar, H. J. W.


    In the Eastern North Atlantic Ocean iron (Fe) speciation was investigated in three size fractions the dissolvable from unfiltered samples the dissolved fraction (0 2 mu m) fraction were unsaturated with Fe with respect to the dissolved fraction thus these waters had a scavenging potential Crown

  20. Selenium speciation and extractability in Dutch agricultural soils

    NARCIS (Netherlands)

    Supriatin, Supriatin; Weng, Liping; Comans, Rob N.J.


    The study aimed to understand selenium (Se) speciation and extractability in Dutch agricultural soils. Top soil samples were taken from 42 grassland fields and 41 arable land fields in the Netherlands. Total Se contents measured in aqua regia were between 0.12 and 1.97mgkg-1(on average

  1. The secondary contact phase of allopatric speciation in Darwin's finches (United States)

    Grant, Peter R.; Grant, B. Rosemary


    Speciation, the process by which two species form from one, involves the development of reproductive isolation of two divergent lineages. Here, we report the establishment and persistence of a reproductively isolated population of Darwin's finches on the small Galápagos Island of Daphne Major in the secondary contact phase of speciation. In 1981, an immigrant medium ground finch (Geospiza fortis) arrived on the island. It was unusually large, especially in beak width, sang an unusual song, and carried some Geospiza scandens alleles. We followed the fate of this individual and its descendants for seven generations over a period of 28 years. In the fourth generation, after a severe drought, the lineage was reduced to a single brother and sister, who bred with each other. From then on this lineage, inheriting unusual song, morphology, and a uniquely homozygous marker allele, was reproductively isolated, because their own descendants bred with each other and with no other member of the resident G. fortis population. These observations agree with some expectations of an ecological theory of speciation in that a barrier to interbreeding arises as a correlated effect of adaptive divergence in morphology. However, the important, culturally transmitted, song component of the barrier appears to have arisen by chance through an initial imperfect copying of local song by the immigrant. The study reveals additional stochastic elements of speciation, in which divergence is initiated in allopatry; immigration to a new area of a single male hybrid and initial breeding with a rare hybrid female. PMID:19918081

  2. Speciation and bioavailability of copper in Lake Tjeukemeer

    NARCIS (Netherlands)

    Verweij, W.


    Chapter 1: introduction

    In this thesis an account is given of a research project dealing with the chemical speciation and bioavailability of copper in Lake Tjeukemeer, a lake in the north of the Netherlands. The reason for the initiation of this project was a lack of

  3. Speciation and phase separation of water in quartz (A review ...

    African Journals Online (AJOL)

    Speciation, supersaturation and phase separation of water in hydrothermal grown (synthetic) quartz cryst-als have been examined as fundamental issues determining clustering, nucleation and bubble formation, which have profound influence on hydrolytic weakening, dislocation-bubble interactions and high temperature ...

  4. Speciational view of macroevolution: Are micro and macroevolution decoupled? (United States)

    Schwämmle, V.; Brigatti, E.


    We introduce a simple computational model that, with microscopic dynamics driven by natural selection and mutation alone, allows the description of true speciation events. A statistical analysis of the evolutionary tree so generated captures realistic features showing power laws for frequency distributions in time and size. Finally, some possible interpretations of the absence of punctuated dynamics with mass extinctions are worked out.

  5. Chemical Speciation and Mobility of Some ...

    African Journals Online (AJOL)

    Michael Horsfall

    Chemical Speciation and Mobility of Some Heavy Metals in Soils around Automobile. Waste Dumpsites in Northern ... dumpsites in Northern part of Niger Delta was assessed using Tessier et al. five syteps sequential chemical extraction procedure. ...... Traceinorganics in water Gould, R.F. (ed) Advances in Chemistry Series ...

  6. Lead speciation in indoor dust: a case study to assess old paint contribution in a Canadian urban house. (United States)

    Beauchemin, Suzanne; MacLean, Lachlan C W; Rasmussen, Pat E


    Residents in older homes may experience increased lead (Pb) exposures due to release of lead from interior paints manufactured in past decades, especially pre-1960s. The objective of the study was to determine the speciation of Pb in settled dust from an urban home built during WWII. X-ray absorption near-edge structure (XANES) and micro-X-ray diffraction (XRD) analyses were performed on samples of paint (380-2,920 mg Pb kg(-1)) and dust (200-1,000 mg Pb kg(-1)) collected prior to renovation. All dust samples exhibited a Pb XANES signature similar to that of Pb found in paint. Bulk XANES and micro-XRD identified Pb species commonly found as white paint pigments (Pb oxide, Pb sulfate, and Pb carbonate) as well as rutile, a titanium-based pigment, in the paints still contribute to Pb in the settled dust for this 65-year-old home. The Pb speciation also provided a clearer understanding of the Pb bioaccessibility: Pb carbonate > Pb oxide > Pb sulfate. This study underscores the importance of taking precautions to minimize exposures to Pb in house dust, especially in homes where old paint is exposed due to renovations or deterioration of painted surfaces.

  7. Numerical modelling of iron-pnictide bulk superconductor magnetization (United States)

    Ainslie, Mark D.; Yamamoto, Akiyasu; Fujishiro, Hiroyuki; Weiss, Jeremy D.; Hellstrom, Eric E.


    Iron-based superconductors exhibit a number of properties attractive for applications, including low anisotropy, high upper critical magnetic fields (H c2) in excess of 90 T and intrinsic critical current densities above 1 MA cm-2 (0 T, 4.2 K). It was shown recently that bulk iron-pnictide superconducting magnets capable of trapping over 1 T (5 K) and 0.5 T (20 K) can be fabricated with fine-grain polycrystalline Ba0.6K0.4Fe2As2 (Ba122). These Ba122 magnets were processed by a scalable, versatile and low-cost method using common industrial ceramic processing techniques. In this paper, a standard numerical modelling technique, based on a 2D axisymmetric finite-element model implementing the H -formulation, is used to investigate the magnetisation properties of such iron-pnictide bulk superconductors. Using the measured J c(B, T) characteristics of a small specimen taken from a bulk Ba122 sample, experimentally measured trapped fields are reproduced well for a single bulk, as well as a stack of bulks. Additionally, the influence of the geometric dimensions (thickness and diameter) on the trapped field is analysed, with a view of fabricating larger samples to increase the magnetic field available from such trapped field magnets. It is shown that, with current state-of-the-art superconducting properties, surface trapped fields >2 T could readily be achieved at 5 K (and >1 T at 20 K) with a sample of diameter 50 mm. Finally, an aspect ratio of between 1 and 1.5 for R/H (radius/thickness) would be an appropriate compromise between the accessible, surface trapped field and volume of superconducting material for bulk Ba122 magnets.

  8. Determination of Bulk Dimensional Variation in Castings

    Energy Technology Data Exchange (ETDEWEB)

    Dr. James F. Cuttino Dr. Edward P. Morse


    The purpose of this work is to improve the efficiency of green sand foundries so that they may continue to compete as the most cost-effective method of fabrication while meeting tightening constraints on near-net shape manufacturing. In order to achieve this objective, the study is divided into two major components. The first component concentrated on identifying which processes control surface finish on the castings and which provide potential reductions in variations. The second component identified metrological methods that effectively discern between the geometry of bulk material versus surface finish in order to more accurately determine the quality of a part. The research resulted in the determination of an empirical relationship relating pouring parameters to dimensional variation, with an R2 value of greater than 0.79. A significant difference in variations obtained from vertical vs. horizontal molding machines was also noticed. When analyzed separately, however, the resulting empirical relationships for horizontal and vertical machines had reduced R2 values, probably due to the reduced data sets. Significant parameters when considering vertical and horizontal molding machines together included surface roughness, pattern type, iron type, pouring rate, copper content, amount of Western Bentonite, and permeability.

  9. Promising Thermoelectric Bulk Materials with 2D Structures. (United States)

    Zhou, Yiming; Zhao, Li-Dong


    Given that more than two thirds of all energy is lost, mostly as waste heat, in utilization processes worldwide, thermoelectric materials, which can directly convert waste heat to electricity, provide an alternative option for optimizing energy utilization processes. After the prediction that superlattices may show high thermoelectric performance, various methods based on quantum effects and superlattice theory have been adopted to analyze bulk materials, leading to the rapid development of thermoelectric materials. Bulk materials with two-dimensional (2D) structures show outstanding properties, and their high performance originates from both their low thermal conductivity and high Seebeck coefficient due to their strong anisotropic features. Here, the advantages of superlattices for enhancing the thermoelectric performance, the transport mechanism in bulk materials with 2D structures, and optimization methods are discussed. The phenomenological transport mechanism in these materials indicates that thermal conductivities are reduced in 2D materials with intrinsically short mean free paths. Recent progress in the transport mechanisms of Bi 2 Te 3 -, SnSe-, and BiCuSeO-based systems is summarized. Finally, possible research directions to enhance the thermoelectric performance of bulk materials with 2D structures are briefly considered. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Sulfur Speciation in the Martian Regolith Component in Shergottite Glasses (United States)

    Rao, M. N.; Nyquist, Laurence E.; Sutton, S.; Huth, J.


    We have shown that Gas-Rich Impact-Melt (GRIM) glasses in Shergotty, Zagami, and EET79001 (Lith A and Lith B) contain Martian regolith components that were molten during impact and quenched into glasses in voids of host rock materials based on neutron-capture isotopes, i.e., Sm-150 excesses and Sm-149 deficits in Sm, and Kr-80 excesses produced from Br [1, 2]. These GRIM glasses are rich in S-bearing secondary minerals [3.4]. Evidence for the occurrence of CaSO4 and S-rich aluminosilicates in these glasses is provided by CaO-SO3 and Al2O3-SO3 correlations, which are consistent with the finding of gypsum laths protruding from the molten glass in EET79001 (Lith A) [5]. However, in the case of GRIM glasses from EET79001 (Lith B), Shergotty and Zagami, we find a different set of secondary minerals that show a FeO-SO3 correlation (but no MgOSO3 correlation), instead of CaO-SO3 and Al2O3-SO3 correlations observed in Lith A. These results might indicate different fluidrock interactions near the shergottite source region on Mars. The speciation of sulfur in these salt assemblages was earlier studied by us using XANES techniques [6], where we found that Lith B predominantly contains Fe-sulfide globules (with some sulfate). On the other hand, Lith A showed predominantly Casulfite/ sulfate with some FeS. Furthermore, we found Fe to be present as Fe2+ indicating little oxidation, if any, in these glasses. To examine the sulfide-sulfate association in these glasses, we studied their Fe/Ni ratios with a view to find diagnostic clues for the source fluid. The Fe-sulfide mineral (Fe(0.93)Ni(0.3)S) in EET79001, Lith A is pyrrhotite [7, 8]. It yields an Fe/Ni ratio of 31. In Shergotty, pyrrhotite occurs with a molar ratio of Fe:S of 0.94 and a Ni abundance of 0.12% yielding a Fe/Ni ratio of approx.500 [8]. In this study, we determined a NiO content of approx.0.1% and FeO/NiO ratio of approx.420 in S-rich globules in #507 (EET79001, Lith B) sample using FE-SEM. In the same sample

  11. [Speciation analysis of trace elements Cu, Fe and Zn in serum by flame atomic absorption spectrophotometry]. (United States)

    Hu, Jun; Chang, Yao-Ming; Gao, Shuang-Bin; Hai, Chun-Xu; Li, Jin-Sheng; Xie, Xiao-Ping


    Since biological functions of the elements are generally different, depending on their chemical forms, chemical speciation analysis is really important in metallomics research. Thus, multielement analysis and chemical speciation of the elements in serum were carried out in the present work. A hyphenated technique was developed for high-throughput speciation analysis of the copper, iron and zinc in serum by molecular biology technology and flame atomic absorption spectrophotometry (AAS). Here, Cu, Fe and Zn in serum were classifyied as the forms of combination and non-combination. The serum protein was precipitated by 60% concentration of ethanol under hypothermy. The forms of combination of Cu, Fe and Zn in serum which combined with proteins were in precipitations, and the forms of non-combination of Cu, Fe and Zn in serum, which were free ions, were in supernatant. The total amount of Cu, Fe and Zn in serum and the amount of the forms of non-combination of Cu, Fe and Zn were analyzed by AAS. The amount of the forms of combination of Cu, Fe and Zn was obtained by calculation. The detection limit of Cu in serum by the method is around and 9.84 x 10(-3) microg x mL(-1). For Fe and Zn, the detection limit is about 2.76 x 10(-2) microg x mL(-1) and 1.06 x 10(-3) microg x mL(-1), respectively. The percentage recovery of trace elements Cu, Fe and Zn by the proposed procedure is in the range 95.0%-101.0%, 95.0%-102.0% and 95.0%-103.0%, respectively. The relative standard deviation (RSD) of trace elements Cu, Fe and Zn in the serum is in the range 1.88%-2.26%, 0.56%-1.59% and 0.34%-1.36%, respectively. Speciation of trace elements Cu, Fe and Zn in the serum of SD rat were analyzed by the method.


    Kelić, Katarina; Matić, Sanja; Marović, Danijela; Klarić, Eva; Tarle, Zrinka


    The aim of the study was to determine microhardness of high- and low-viscosity bulk-fill composite resins and compare it with conventional composite materials. Four materials of high-viscosity were tested, including three bulk-fills: QuiXfi l (QF), x-tra fi l (XTF) and Tetric EvoCeram Bulk Fill (TEBCF), while nanohybrid composite GrandioSO (GSO) served as control. The other four were low-viscosity composites, three bulk-fill materials: Smart Dentin Replacement (SDR), Venus Bulk Fill (VBF) and x-tra base (XB), and conventional control material X-Flow (XF). Composite samples (n=5) were polymerized for 20 s with Bluephase G2 curing unit. Vickers hardness was used to determine microhardness of each material at the surface, and at 2-mm and 4-mm depth. GSO on average recorded significantly higher microhardness values than bulk-fill materials (pcomposite XF revealed similar microhardness values as SDR, but significantly lower than XB (pmaterials was lower than microhardness of the conventional composite material (GSO). Surface microhardness of low-viscosity materials was generally even lower. The microhardness of all tested materials at 4 mm was not different from their surface values. However, additional capping layer was a necessity for low-viscosity bulk-fill materials due to their low microhardness.

  13. Evaluation of mercury speciation and removal through air pollution control devices of a 190 MW boiler. (United States)

    Wu, Chengli; Cao, Yan; Dong, Zhongbing; Cheng, Chinmin; Li, Hanxu; Pan, Weiping


    Air pollution control devices (APCDs) are installed at coal-fired power plants for air pollutant regulation. Selective catalytic reduction (SCR) and wet flue gas desulfurization (FGD) systems have the co-benefits of air pollutant and mercury removal. Configuration and operational conditions of APCDs and mercury speciation affect mercury removal efficiently at coal-fired utilities. The Ontario Hydro Method (OHM) recommended by the U.S. Environmental Protection Agency (EPA) was used to determine mercury speciation simultaneously at five sampling locations through SCR-ESP-FGD at a 190 MW unit. Chlorine in coal had been suggested as a factor affecting the mercury speciation in flue gas; and low-chlorine coal was purported to produce less oxidized mercury (Hg2+) and more elemental mercury (Hg0) at the SCR inlet compared to higher chlorine coal. SCR could oxidize elemental mercury into oxidized mercury when SCR was in service, and oxidation efficiency reached 71.0%. Therefore, oxidized mercury removal efficiency was enhanced through a wet FGD system. In the non-ozone season, about 89.5%-96.8% of oxidized mercury was controlled, but only 54.9%-68.8% of the total mercury was captured through wet FGD. Oxidized mercury removal efficiency was 95.9%-98.0%, and there was a big difference in the total mercury removal efficiencies from 78.0% to 90.2% in the ozone season. Mercury mass balance was evaluated to validate reliability of OHM testing data, and the ratio of mercury input in the coal to mercury output at the stack was from 0.84 to 1.08.

  14. Candidemia: Speciation and Antifungal susceptibility testing from a Tertiary Care Hospital in Maharashtra, India

    Directory of Open Access Journals (Sweden)

    Nageswari Rajesh Gandham


    Full Text Available Introduction: Invasive fungal infections are an important nosocomial health problem, candidal infections being the most common. Candidal bloodstream infections (BSIs account for one-fourth of the nosocomial BSIs. Candida albicans once the most common has now been replaced by nonalbicans Candida, accounting for majority of cases of candidal infections. The knowledge and understanding of specific risk factors, epidemiology, prophylactic measures, and outcomes with relation to speciation are changing rapidly. Emergence of antifungal resistance is a cause of concern. With this background, a prospective study was undertaken. Aims and Objectives: To isolate Candida spp. from blood cultures of patients with clinically diagnosed or suspected septicemia; to identify and speciate Candida isolates and carry out the antifungal susceptibility test; to determine incidence of candidemia; to find out the crude mortality rate in candidemia patients. Materials and Methods: Blood cultures received in the Department of Microbiology from various critical care units over a 1-year period were included in this study. Samples were cultured on Sabouraud dextrose agar and routine bacteriological cultures. Speciation of suspected Candida growth was done by conventional and automated system. Results: A total of 225 out of 839 blood cultures were culture positive. A total of 196 were bacterial pathogens. Candida spp. were isolated in 29 samples. These included 10 cases of Candida tropicalis, 8 Candida parapsilosis, and three cases each of C. albicans and Candida krusei. Fluconazole resistance was seen (minimum inhibitory concentration ≥64 μg/ml in 4 isolates, 2 of C. krusei and 2 of Candida haemulonii. Incidence of candidemia was 3.46%. Crude mortality rate in the present study was 24%.

  15. Bionic design methodology for wear reduction of bulk solids handling equipment

    NARCIS (Netherlands)

    Chen, G.; Schott, D.L.; Lodewijks, G.


    Large-scale handling of particulate solids can cause severe wear on bulk solids handling equipment surfaces. Wear reduces equipment life span and increases maintenance cost. Examples of traditional methods to reduce wear of bulk solids handling equipment include optimizing transport operations

  16. Characterization of a bulk-micromachined membraneless in-plane thermopile

    NARCIS (Netherlands)

    Wang, Z.; Andel, Y. van; Jambunathan, M.; Leonov, V.; Elfrink, R.; Vullers, R.J.M.


    This paper describes the characterization method and results for bulk- micromachined in-plane thermopiles. Made of poly-Si or poly-SiGe, the thermocouple legs bridge the hot and cold side of a Si frame, which is formed by bulk micromachining. The characterization of the fabricated devices is carried

  17. Speciation of arsenic(III)/arsenic(V) and selenium(IV)/ selenium(VI) using coupled ion chromatography - hydride generation atomic absorption spectrometry (United States)

    Simple analytical methods have been developed to speciate inorganic arsenic and selenium in the ppb range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determinations of the redox states arsenite A...

  18. Speciation analysis of 129I in seawater by carrier-free AgI-AgCl coprecipitation and accelerator mass spectrometric measurement

    DEFF Research Database (Denmark)

    Luo, Maoyi; Hou, Xiaolin; He, Chaohui


    A rapid and simple method was developed for speciation analysis of 129I in seawater by selective coprecipitation of carrier-free iodide and accelerator mass spectrometry (AMS) measurement of 129I. Iodide was separated from seawater and other species of iodine by coprecipitation of AgI with Ag2SO3...

  19. Speciation analysis of aluminium and aluminium fluoride complexes by HPIC-UVVIS. (United States)

    Frankowski, Marcin; Zioła-Frankowska, Anetta


    The study presents a new analytical method for speciation analysis in fractionation of aluminium fluoride complexes and free Al(3+) in soil samples. Aluminium speciation was studied in model solutions and soil extract samples by means of high performance ion chromatography (HPIC) with UV-VIS detection using post-column reaction with tiron for the separation and detection of aluminium fluoride complex and Al(3+) forms during one analysis. The paper presents particular stages of the chromatographic process optimization involving selecting the appropriate eluent strength, type of elution or concentration and quantity of derivatization reagent. HPIC was performed on a bifunctional analytical column Dionex IonPac CS5A. The use of gradient elution and the eluents A: 1M NH(4)Cl and B: water acidified to pH of eluent phase, enabled full separation of fluoride aluminium forms as AlF(2)(+), AlF(3)(0), AlF(4)(-) (first signal), AlF(2+) (second signal) and form Al(3+) in a single analytical procedure. The proposed new method HPIC-UVVIS was applied successfully in the quantitative and qualitative analysis of soil samples. Copyright © 2010 Elsevier B.V. All rights reserved.


    Energy Technology Data Exchange (ETDEWEB)

    Glenn C. England; Stephanie Wien; Mingchih O. Chang


    This report provides results from the first year of this three-year project to develop dilution measurement technology for characterizing PM2.5 (particles with aerodynamic diameter smaller than 2.5 micrometers) and precursor emissions from stationary combustion sources used in oil, gas and power generation operations. Detailed emission rate and chemical speciation test results for a refinery gas-fired process heater and plans for cogeneration gas turbine tests and pilot-scale tests are presented. Tests were performed using a research dilution sampling apparatus and traditional EPA methods to compare PM2.5 mass and chemical speciation. Test plans are presented for a gas turbine facility that will be tested in the fourth quarter of 2002. A preliminary approach for pilot-scale tests is presented that will help define design constraints for a new dilution sampler design that is smaller, lighter, and less costly to use.

  1. Bulk Laser Material Modification: Towards a Kerfless Laser Wafering Process (United States)

    LeBeau, James

    Due to the ever increasing relevance of finer machining control as well as necessary reduction in material waste by large area semiconductor device manufacturers, a novel bulk laser machining method was investigated. Because the cost of silicon and sapphire substrates are limiting to the reduction in cost of devices in both the light emitting diode (LED) and solar industries, and the present substrate wafering process results in >50% waste, the need for an improved ingot wafering technique exists. The focus of this work is the design and understanding of a novel semiconductor wafering technique that utilizes the nonlinear absorption properties of band-gapped materials to achieve bulk (subsurface) morphological changes in matter using highly focused laser light. A method and tool was designed and developed to form controlled damage regions in the bulk of a crystalline sapphire wafer leaving the surfaces unaltered. The controllability of the subsurface damage geometry was investigated, and the effect of numerical aperture of the focusing optic, energy per pulse, wavelength, and number of pulses was characterized for a nanosecond pulse length variable wavelength Nd:YAG OPO laser. A novel model was developed to describe the geometry of laser induced morphological changes in the bulk of semiconducting materials for nanosecond pulse lengths. The beam propagation aspect of the model was based on ray-optics, and the full Keldysh multiphoton photoionization theory in conjuncture with Thornber's and Drude's models for impact ionization were used to describe high fluence laser light absorption and carrier generation ultimately resulting in permanent material modification though strong electron-plasma absorption and plasma melting. Although the electron-plasma description of laser damage formation is usually reserved for extremely short laser pulses (plane of damage in the bulk of sapphire wafers. This was accomplished using high numerical aperture optics, a variable

  2. Antimony speciation analysis in sediment reference materials using high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Potin-Gautier, M. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Pannier, F. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France)]. E-mail:; Quiroz, W. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Pinochet, H. [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Gregori, I. de [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile)


    This work presents the development of suitable methodologies for determination of the speciation of antimony in sediment reference samples. Liquid chromatography with a post-column photo-oxidation step and hydride generation atomic fluorescence spectrometry as detection system is applied to the separation and determination of Sb(III), Sb(V) and trimethylantimony species. Post-column decomposition and hydride generation steps were studied for sensitive detection with the AFS detector. This method was applied to investigate the conditions under which speciation analysis of antimony in sediment samples can be carried out. Stability studies of Sb species during the extraction processes of solid matrices, using different reagents solutions, were performed. Results demonstrate that for the extraction yield and the stability of Sb species in different marine sediment extracts, citric acid in ascorbic acid medium was the best extracting solution for antimony speciation analysis in this matrix (between 55% and 65% of total Sb was recovered from CRMs, Sb(III) being the predominant species). The developed method allows the separation of the three compounds within 6 min with detection limits of 30 ng g{sup -1} for Sb(III) and TMSbCl2 and 40 ng g{sup -1} for Sb(V) in sediment samples.

  3. A Review on Recent Applications of High-Performance Liquid Chromatography in Metal Determination and Speciation Analysis. (United States)

    Rekhi, Heena; Rani, Susheela; Sharma, Neha; Malik, Ashok Kumar


    High-performance liquid chromatography (HPLC) has several advantages over the conventional methods due to their operational simplicity. It is a vital tool to determine metal ions having same mass but different electronic configuration, to separate complex mixtures and to resolve ions that may be indistinguishable by mass spectrometry alone. Metal ions play vital role in many biological processes and involved in setting up of many diseases. Therefore, the development of simple methods for the detection and quantification of metals in real samples might serve as diagnostic tools for various diseases. This review article focuses on the recent main feature of this technique, i.e. speciation of metal ions and their applications to series of problem of metal ion chemistry in different environmental matrixes. Speciation of metals is of increasing interest and has a great importance because of bioavailability, environmental mobility, toxicity and potential risk of metals. With the capability of partitioning the complex species of different metal ions, HPLC is an efficient technique for this task. This review summarizes recent advances in the development of HPLC to the fundamental understanding of metal ion chemistry in the environment and discusses all the issues that still need a lot of consideration. It has been classified into different sections depending on the role of HPLC in separation used and metal speciation; furthermore, the underlying sample preconcentration techniques and detection systems involved for the determination of metal ions and their applications were discussed.

  4. FAA bulk technology overview for explosives detection (United States)

    Novakoff, Alan K.


    The Federal Aviation Administration (FAA) is the leading federal agency responsible for encouraging and fostering the development of a safe, secure, and efficient national airspace system (NAS). Our goal is to establish an operating environment that ensures a threat-free system to preclude acts of terrorism and fatalities. As part of the process to meet this goal, our research and development activities continually search for technologies to ensure aviation security. Recent acts of terrorism against the aviation community have demonstrated an increasing level of sophistication in the design and deployment of explosive devices. In order to prevent the introduction of explosives onto an aircraft they must be detected prior to passenger and baggage loading. The Bulk Detection program is one method of developing a number of technologies that 'see' into and 'alarm' on suspect baggage. These detection devices must be capable of providing this serve with a confidence commensurate with the state-of-the- art available today. This program utilizes the expertise of government agencies, universities and industries working toward constructing their plans and executing their designs to produce the best available equipment.

  5. Recent developments of film bulk acoustic resonators (United States)

    Gao, Junning; Liu, Guorong; Li, Jie; Li, Guoqiang


    Film bulk acoustic wave resonator (FBAR) experienced skyrocketing development in the past 15 years, owing to the explosive development of mobile communication. It stands out in acoustic filters mainly because of high quality factor, which enables low insertion loss and sharp roll off. Except for the massive application in wireless communication, FBARs are also promising sensors because of the high sensitivity and readily integration ability to miniaturize circuits. On the ground of summarizing FBAR’s application in wireless communication as filters and in sensors including electronic nose, bio field, and pressure sensing, this paper review the main challenges of each application faced. The number of filters installed in the mobile phone has being grown explosively, which leads to overcrowded bands and put harsh requirements on component size and power consumption control for each unit. Data flow and rate are becoming increasingly demanding as well. This paper discusses three promising technical strategies addressing these issues. Among which coupled resonator filter is given intense attention because it is able to vigorously reduce the filter size by stacking two or more resonators together, and it is a great technique to increase data flow and rate. Temperature compensation methods are discussed considering their vital influence on frequency stability. Finally, materials improvement and novel materials exploration for band width modulation, tunable band acquisition, and quality factor improvement are discussed. The authors appeal attention of the academic society to bring AlN epitaxial thin film into the FBAR fabrication and have proposed a configuration to implement this idea.

  6. A brief overview of bulk metallic glasses

    National Research Council Canada - National Science Library

    Mingwei Chen


      The discovery of bulk metallic glasses (BMGs) has stimulated widespread research enthusiasm because of their technological promise for practical applications and scientific importance in understanding glass formation and glass phenomena...

  7. Prions, Radionuclides and Clays: Impact of clay interlayer "acidity" on toxic compound speciation (United States)

    Charlet, L.; Hureau, C.; Sobolev, O.; Cuello, G.; Chapron, Y.


    . The speciation of the Cu-ligand complex was found to be different, in bulk water (Hureau et al., 2006) and in clay suspensions, where n increases. This new speciation of the copper metal ions, used as a molecular probe, allows to "measure" the pH of interlayer water which is shown to be significantly lower than in bulk water pH. Molecular models for PrP attachment to the clay basal plane and Sm location within the clay interlayer were obtained by MD computations. Implications on PrP pathogenicity, following carcase burial and particle ingestions, and on radionuclide mobility, following nuclear waste burial in clay rich repository sites, will be discussed.

  8. Comparison of different models for predicting soil bulk density. Case study - Slovakian agricultural soils (United States)

    Makovníková, Jarmila; Širáň, Miloš; Houšková, Beata; Pálka, Boris; Jones, Arwyn


    Soil bulk density is one of the main direct indicators of soil health, and is an important aspect of models for determining agroecosystem services potential. By way of applying multi-regression methods, we have created a distributed prediction of soil bulk density used subsequently for topsoil carbon stock estimation. The soil data used for this study were from the Slovakian partial monitoring system-soil database. In our work, two models of soil bulk density in an equilibrium state, with different combinations of input parameters (soil particle size distribution and soil organic carbon content in %), have been created, and subsequently validated using a data set from 15 principal sampling sites of Slovakian partial monitoring system-soil, that were different from those used to generate the bulk density equations. We have made a comparison of measured bulk density data and data calculated by the pedotransfer equations against soil bulk density calculated according to equations recommended by Joint Research Centre Sustainable Resources for Europe. The differences between measured soil bulk density and the model values vary from -0.144 to 0.135 g cm-3 in the verification data set. Furthermore, all models based on pedotransfer functions give moderately lower values. The soil bulk density model was then applied to generate a first approximation of soil bulk density map for Slovakia using texture information from 17 523 sampling sites, and was subsequently utilised for topsoil organic carbon estimation.

  9. Measurement Techniques for Thermal Conductivity and Interfacial Thermal Conductance of Bulk and Thin Film Materials


    Zhao, Dongliang; Qian, Xin; Gu, Xiaokun; Jajja, Saad Ayub; Yang, Ronggui


    Thermal conductivity and interfacial thermal conductance play crucial roles in the design of engineering systems where temperature and thermal stress are of concerns. To date, a variety of measurement techniques are available for both bulk and thin film solid-state materials with a broad temperature range. For thermal characterization of bulk material, the steady-state absolute method, laser flash diffusivity method, and transient plane source method are most used. For thin film measurement, ...

  10. Boundary-bulk relation in topological orders (United States)

    Kong, Liang; Wen, Xiao-Gang; Zheng, Hao


    In this paper, we study the relation between an anomaly-free n + 1D topological order, which are often called n + 1D topological order in physics literature, and its nD gapped boundary phases. We argue that the n + 1D bulk anomaly-free topological order for a given nD gapped boundary phase is unique. This uniqueness defines the notion of the "bulk" for a given gapped boundary phase. In this paper, we show that the n + 1D "bulk" phase is given by the "center" of the nD boundary phase. In other words, the geometric notion of the "bulk" corresponds precisely to the algebraic notion of the "center". We achieve this by first introducing the notion of a morphism between two (potentially anomalous) topological orders of the same dimension, then proving that the notion of the "bulk" satisfies the same universal property as that of the "center" of an algebra in mathematics, i.e. "bulk" = center". The entire argument does not require us to know the precise mathematical description of a (potentially anomalous) topological order. This result leads to concrete physical predictions.

  11. Selective Separation and Determination of Heavy Metals (Cd, Pb, Cr) Speciation Forms from Hortic Antrosols (United States)

    Bulgariu, D.; Bulgariu, L.


    The speciation, inter-phases distribution and biodisponibility of heavy metals in soils represent one of main problem of environmental geochemistry and agro-chemistry. This problem is very important in case of hortic antrosols (soils from glasshouses) for the elimination of agricultural products (fruits, vegetables) contamination with heavy metals. In soils from glass houses, the speciation and inter-phases distribution processes of heavy metals have a particular dynamic, different in comparison with those from non-protected soils. The predominant distribution forms of heavy metals in such soils types are: complexes with low mass organic molecules, organic-mineral complexes, complexes with inorganic ligands (hydroxide-complexes, carbonate-complexes, sulphate-complexes, etc.) and basic salts. All of these have high stabilities in conditions of soils from glass houses, and in consequence, the separation and determination of speciation forms (which is directly connected with biodisponibility of heavy metals) by usual methods id very difficult and has a high uncertain degree. In this study is presented an original method for the selective separation and differentiation of speciation forms of heavy metals from glass houses soils, which is based by the combination of solid-liquid sequential extraction (SPE) with the extraction in aqueous polymer-inorganic salt two-phase systems (ABS). The soil samples used for this study have been sampled from three different locations (glass houses from Iasi, Barlad and Bacau - Romania) where the vegetables cultivation have bee performed by three different technologies. In this way was estimated the applicability and the analytical limits of method proposed by as, in function of the chemical-mineralogical and physical-chemical characteristics of soils. As heavy metals have been studied cadmium, lead and chromium, all being known for their high toxicity. The procedure used for the selective separation and differentiation of speciation

  12. Development of a coprecipitation system for the speciation/preconcentration of chromium in tap waters. (United States)

    Karatepe, Aslihan; Korkmaz, Esra; Soylak, Mustafa; Elci, Latif


    A method for the speciation of chromium(III), chromium(VI) and determination of total chromium based on coprecipitation of chromium(III) with dysprosium hydroxide has been investigated and applied to tap water samples. Chromium(III) was quantitatively recovered by the presented method, while the recovery values for chromium(VI) was below 10%. The influences of analytical parameters including amount of dysprosium(III), pH, centrifugation speed and sample volume for the quantitative precipitation were examined. No interferic effects were observed from alkali, earth alkali and some transition metals for the analyte ions. The detection limits (k=3, N=15) were 0.65 microg/L for chromium(III) and 0.78 microg/L for chromium(VI). The validation of the presented method was checked by the analysis of certified reference materials.

  13. Study of Ascorbic Acid as Iron(III Reducing Agent for Spectrophotometric Iron Speciation

    Directory of Open Access Journals (Sweden)

    Antesar Elmagirbi


    Full Text Available The study of ascorbic acid as a reducing agent for iron(III has been investigated in order to obtain an alternative carcinogenic reducing agent, hydroxylamine, used in spectrophotometric standard method based on the formation of a red-orange complex of Fe(II-o-phenanthroline. The study was optimised with regards to ascorbic acid concentration as well as pH solution. The results showed that ascorbic acid showed maximum capacity as reducing agent of iron(III under concentration of 4.46.10-4 M and pH solution of 1-4.Under these conditions, ascorbic acid reduced iron(III proportionally and performed similarly to that of hydroxylamine.  The method gave result to linear calibration over the range of 0.2-2 mg/L withhigh accuracy of 97 % and relative standard deviation of less than 2 %. This method was successfully applied to assay iron speciation in water samples.

  14. Arsenic speciation in natural water samples by coprecipitation-hydride generation atomic absorption spectrometry combination. (United States)

    Tuzen, Mustafa; Citak, Demirhan; Mendil, Durali; Soylak, Mustafa


    A speciation procedure for As(III) and As(V) ions in environmental samples has been presented. As(V) was quantitatively recovered on aluminum hydroxide precipitate. After oxidation of As(III) by using dilute KMnO(4), the developed coprecipitation was applied to determination of total arsenic. Arsenic(III) was calculated as the difference between the total arsenic content and As(V) content. The determination of arsenic levels was performed by hydride generation atomic absorption spectrometry (HG-AAS). The analytical conditions for the quantitative recoveries of As(V) including pH, amount of aluminum as carrier element and sample volume, etc. on the presented coprecipitation system were investigated. The effects of some alkaline, earth alkaline, metal ions and also some anions were also examined. Preconcentration factor was calculated as 25. The detection limits (LOD) based on three times sigma of the blank (N: 21) for As(V) was 0.012 microg L(-1). The satisfactory results for the analysis of arsenic in NIST SRM 2711 Montana soil and LGC 6010 Hard drinking water certified reference materials for the validation of the method was obtained. The presented procedure was successfully applied to real samples including natural waters for arsenic speciation.

  15. Soft X-ray spectromicroscopy for speciation, quantitation and nano-eco-toxicology of nanomaterials. (United States)

    Lawrence, J R; Swerhone, G D W; Dynes, J J; Korber, D R; Hitchcock, A P


    There is a critical need for methods that provide simultaneous detection, identification, quantitation and visualization of nanomaterials at their interface with biological and environmental systems. The approach should allow speciation as well as elemental analysis. Using the intrinsic X-ray absorption properties, soft X-ray scanning transmission X-ray spectromicroscopy (STXM) allows characterization and imaging of a broad range of nanomaterials, including metals, oxides and organic materials, and at the same time is able to provide detailed mapping of biological components. Thus, STXM offers considerable potential for application to research on nanomaterials in biology and the environment. The potential and limitations of STXM in this context are discussed using a range of examples, focusing on the interaction of nanomaterials with microbial cells, biofilms and extracellular polymers. The studies outlined include speciation and mapping of metal-containing nanomaterials (Ti, Ni, Cu) and carbon-based nanomaterials (multiwalled carbon nanotubes, C60 fullerene). The benefits of X-ray fluorescence detection in soft X-ray STXM are illustrated with a study of low levels of Ni in a natural river biofilm. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

  16. Hyphenated techniques as tools for speciation analysis of metal-based pharmaceuticals: developments and applications. (United States)

    Meermann, Björn; Sperling, Michael


    Method development and applications of hyphenated techniques as tools for speciation analysis of metal-based pharmaceuticals are summarized within this review. Advantages and limitations of the separation modes-high-performance liquid chromatography (HPLC), capillary electrophoresis (CE), and gas chromatography (GC)-as well as the detection modes-inductively coupled plasma-mass spectrometry (ICP-MS) and electrospray ionization-mass spectrometry (ESI-MS)-are discussed. ICP-MS detection is found to be advantageous for the quantification of drugs containing metals and other heteroatoms. The species-independent sensitivity and multielement capabilities of ICP-MS allow it to be used for quantification even when species-specific standards are not available, as well as to determine the stoichiometry in metallodrug-biomolecule interactions. Molecular information that is totally destroyed when ICP is applied as ionization source and is therefore not obtainable via ICP-MS detection can be accessed by the complementary technique of ESI-MS. Speciation analysis combining both elemental and molecular information is therefore a powerful tool for the analysis of metal-based pharmaceuticals and their metabolites in body fluids and other relevant matrices.

  17. Speciation of methylmercury and ethylmercury by gas chromatography cold vapor atomic fluresence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Boggess, A. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)


    Existing models and simulants of tank disposition media at SRS have presumed the presence of high concentrations of inorganic mercury. However, recent quarterly tank analyses show that mercury is present as organomercurial species at concentrations that may present challenges to remediation and disposition and may exceed the Saltstone Waste Acceptance Criteria (WAC). To-date, methylmercury analysis for Savannah River Remediation (SRR) has been performed off-site by Eurofins Scientific (Lancaster, PA). A series of optimization and validation experiments has been performed at SRNL, which has resulted in the development of on-site organomercury speciation capabilities using purge and trap gas chromatography coupled with thermal desorption cold vapor atomic fluorescence spectroscopy (P&T GC/CVAFS). Speciation has been achieved for methylmercury, with a method reporting limit (MRL) values of 1.42 pg for methylmercury. Results obtained by SRNL from the analysis of past quarterly samples from tanks 21, 40, and 50 have demonstrated statistically indistinguishable concentration values compared with the concentration data obtained from Eurofins, while the data from SRNL has demonstrated significantly improved precision and processing time.

  18. Correlations Between Magnetic Flux and Levitation Force of HTS Bulk Above a Permanent Magnet Guideway (United States)

    Huang, Huan; Zheng, Jun; Zheng, Botian; Qian, Nan; Li, Haitao; Li, Jipeng; Deng, Zigang


    In order to clarify the correlations between magnetic flux and levitation force of the high-temperature superconducting (HTS) bulk, we measured the magnetic flux density on bottom and top surfaces of a bulk superconductor while vertically moving above a permanent magnet guideway (PMG). The levitation force of the bulk superconductor was measured simultaneously. In this study, the HTS bulk was moved down and up for three times between field-cooling position and working position above the PMG, followed by a relaxation measurement of 300 s at the minimum height position. During the whole processes, the magnetic flux density and levitation force of the bulk superconductor were recorded and collected by a multipoint magnetic field measurement platform and a self-developed maglev measurement system, respectively. The magnetic flux density on the bottom surface reflected the induced field in the superconductor bulk, while on the top, it reveals the penetrated magnetic flux. The results show that the magnetic flux density and levitation force of the bulk superconductor are in direct correlation from the viewpoint of inner supercurrent. In general, this work is instructive for understanding the connection of the magnetic flux density, the inner current density and the levitation behavior of HTS bulk employed in a maglev system. Meanwhile, this magnetic flux density measurement method has enriched present experimental evaluation methods of maglev system.

  19. Investigation of bulk acoustic microwaves excited by an interdigital transducer

    Directory of Open Access Journals (Sweden)

    Reshotka O. G.


    Full Text Available Excitation of bulk and surface acoustic waves with the interdigital transducer (IDT, which is deposited on the surface of piezoelectric crystal, is widely used in the development of devices in acoustoelectronics and in the design of the microwave acousto-optic deflectors. Excitation of bulk acoustic waves by IDT in the devices on surface acoustic waves leads to the appearance of spurious signals. At the same time excitation of bulk acoustic waves with IDT from the surface of lithium niobate crystals allows creating high frequency acousto-optic deflectors, which makes possible to significantly simplify the technology of their production. Therefore, significant attention is paid to the task of excitation and distribution of bulk acoustic waves with IDT including recent times by the method of simulation of their excitation and distribution. The obtained theoretical results require experimental verification. This paper documents the visualization of acoustic beams excited with IDT from the XY-surface of lithium niobate crystals. The Bragg cells with LiNbO3 crystals coated with IDT with a different period of electrodes were manufactured for the experimental research of excitation and distribution of bulk acoustic waves. Visualization results have shown that the acoustic waves excited with IDT distribute in both the Fresnel zone and the Fraunhofer zone. The length of these zones is caused by individual elementary emitters of which consists the IDT (by their size. At the same time the far zone for IDT is located at distances much greater than the actual size of the LiNbO3 crystals. This peculiarity is not always taken into account when calculating diffraction. The achieved results can be used to design high-frequency acousto-optic devices, as well as in the development of devices based on surface acoustic waves.

  20. Speciation of Fe in ambient aerosol and cloudwater

    Energy Technology Data Exchange (ETDEWEB)

    Siefert, Ronald Lyn [California Inst. of Technology (CalTech), Pasadena, CA (United States)


    Atmospheric iron (Fe) is thought to play an important role in cloudwater chemistry (e.g., S(IV) oxidation, oxidant production, etc.), and is also an important source of Fe to certain regions of the worlds oceans where Fe is believed to be a rate-limiting nutrient for primary productivity. This thesis focuses on understanding the chemistry, speciation and abundance of Fe in cloudwater and aerosol in the troposphere, through observations of Fe speciation in the cloudwater and aerosol samples collected over the continental United States and the Arabian Sea. Different chemical species of atmospheric Fe were measured in aerosol and cloudwater samples to help assess the role of Fe in cloudwater chemistry.

  1. U(IV) fluorescence spectroscopy. A new speciation tool

    Energy Technology Data Exchange (ETDEWEB)

    Lehmann, Susanne; Brendler, Vinzenz [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Surface Processes; Steudtner, Robin [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Inst. of Resource Ecology


    We combined absorption and fluorescence spectroscopy to study the speciation of U(IV) in solution in concentrations down to 10{sup -6} M uranium. With our time-resolved laser-induced fluorescence setup we could determine the fluorescence decay time of U(IV) in perchloric as well as in chloric acid with 2.6 ± 0.3 ns at room temperature and 148.4 ± 6.5 ns at liquid nitrogen temperature. For the U(IV) sulfate system, we observed a bathochromic shift and a peak shape modification in the fluorescence spectra with increasing sulfate concentration in solution. Thus, the potential of U(IV) fluorescence for speciation analysis could be proven.

  2. Synergy between Allopatry and Ecology in Population Differentiation and Speciation

    Directory of Open Access Journals (Sweden)

    Yann Surget-Groba


    Full Text Available The general diversity pattern of the Caribbean anole radiation has been described in detail; however, the actual mechanisms at the origin of their diversification remain controversial. In particular, the role of ecological speciation, and the relative importance of divergence in allopatry and in parapatry, is debated. We describe the genetic structure of anole populations across lineage contact zones and ecotones to investigate the effect of allopatric divergence, natural selection, and the combination of both factors on population differentiation. Allopatric divergence had no significant impact on differentiation across the lineage boundary, while a clear bimodality in genetic and morphological characters was observed across an ecotone within a single lineage. Critically, the strongest differentiation was observed when allopatry and ecology act together, leading to a sharp reduction in gene flow between two lineages inhabiting different habitats. We suggest that, for Caribbean anoles to reach full speciation, a synergistic combination of several historical and ecological factors may be requisite.

  3. Forecasting Dry Bulk Freight Index with Improved SVM

    Directory of Open Access Journals (Sweden)

    Qianqian Han


    Full Text Available An improved SVM model is presented to forecast dry bulk freight index (BDI in this paper, which is a powerful tool for operators and investors to manage the market trend and avoid price risking shipping industry. The BDI is influenced by many factors, especially the random incidents in dry bulk market, inducing the difficulty in forecasting of BDI. Therefore, to eliminate the impact of random incidents in dry bulk market, wavelet transform is adopted to denoise the BDI data series. Hence, the combined model of wavelet transform and support vector machine is developed to forecast BDI in this paper. Lastly, the BDI data in 2005 to 2012 are presented to test the proposed model. The 84 prior consecutive monthly BDI data are the inputs of the model, and the last 12 monthly BDI data are the outputs of model. The parameters of the model are optimized by genetic algorithm and the final model is conformed through SVM training. This paper compares the forecasting result of proposed method and three other forecasting methods. The result shows that the proposed method has higher accuracy and could be used to forecast the short-term trend of the BDI.

  4. Speciation via floral heterochrony and presumed mycorrhizal host switching of endemic butterfly orchids on the Azorean archipelago. (United States)

    Bateman, Richard M; Rudall, Paula J; Bidartondo, Martin I; Cozzolino, Salvatore; Tranchida-Lombardo, Valentina; Carine, Mark A; Moura, Mónica


    • Premise of the study: Most orchid species native to the Macaronesian islands reflect immigration from western Europe or North Africa followed by anagenesis. The only putative exception is the butterfly orchids (Platanthera) of the Azores, where three species apparently reflect at least one cladogenetic speciation event. This multidisciplinary study explores the origin, speciation, phenotypic, and genotypic cohesion of these Azorean species and their mainland relatives.• Methods: Plants of Platanthera from 30 localities spanning all nine Azorean islands were compared with those of four continental European relatives for 38 morphometric characters; substantial subsets were also analyzed for plastid microsatellites, and for nrITS of both the orchids and their mycorrhizae.• Key results: Although the three Azorean and four mainland species are all readily distinguished morphometrically using several floral characters, and hybridization appears rare, divergence in ITS and especially plastid sequences is small. Despite occupying similar laurisilva habitats, the Azorean species differ radically in the identities and diversity of their mycorrhizal partners; specialism apparently increases rarity.• Conclusions: Although morphological evidence suggests two invasions of the islands from NW Africa and/or SW Europe, ITS data imply only one. As the molecular data are unable to distinguish among the potential mainland ancestors, two scenarios of relationship are explored that imply different ancestors. Both scenarios require both anagenetic and cladogenetic speciation events, involving homoplastic shifts in overall flower size and (often substantial) changes in the relative dimensions of individual floral organs. Limited genotypic divergence among the three species compared with greater phenotypic divergence suggests comparatively recent speciation. Mycorrhizae may be the most critical factor dictating the respective ecological tolerances, and thus the relative

  5. Chromium Speciation Analysis by Ion Chromatography Coupled ...

    African Journals Online (AJOL)

    Two methods coupling ion chromatography with inductively coupled plasma - optical emission spectroscopy (ICP-OES) were developed for the simultaneous separation and determination of Cr(III) and Cr(VI) species. In the first method, anion chromatography with sodium bicarbonate/carbonate solution as the eluent was ...


    African Journals Online (AJOL)

    Chemical speciation of Pb(II), Cd(II), Hg(II), Co(II), Ni(II), Cu(II) and Zn(II) complexes of L-methionine in 0.0-60 % v/v 1,2-propanediol-water mixtures maintaining an ionic strength of 0.16 M at 303 K has been studied pH metrically. The active forms of ligand are LH2+, LH and L-. The predominant species detected are ML, ...

  7. Sexual selection and natural selection in bird speciation


    Price, T.


    The role of sexual selection in speciation is investigated, addressing two main issues. First, how do sexually selected traits become species recognition traits? Theory and empirical evidence suggest that female preferences often do not evolve as a correlated response to evolution of male traits. This implies that, contrary to runaway (Fisherian) models of sexual selection, premating isolation will not arise as an automatic side effect of divergence between populations in sexually selected tr...

  8. Pu speciation in actual and simulated aged wastes

    Energy Technology Data Exchange (ETDEWEB)

    Lezama-pacheco, Juan S [Los Alamos National Laboratory; Conradson, Steven D [Los Alamos National Laboratory


    X-ray Absorption Fine Structure Spectroscopy (XAFS) at the Pu L{sub II/III} edge was used to determine the speciation of this element in (1) Hanford Z-9 Pu crib samples, (2) deteriorated waste resins from a chloride process ion-exchange purification line, and (3) the sediments from two Waste Isolation Pilot Plant Liter Scale simulant brine systems. The Pu speciation in all of these samples except one is within the range previously displayed by PuO{sub 2+x-2y}(OH){sub y}{center_dot}zH{sub 2}O compounds, which is expected based on the putative thermodynamic stability of this system for Pu equilibrated with excess H{sub 2}O and O{sub 2} under environmental conditions. The primary exception was a near neutral brine experiment that displayed evidence for partial substitution of the normal O-based ligands with Cl{sup -} and a concomitant expansion of the Pu-Pu distance relative to the much more highly ordered Pu near neighbor shell in PuO{sub 2}. However, although the Pu speciation was not necessarily unusual, the Pu chemistry identified via the history of these samples did exhibit unexpected patterns, the most significant of which may be that the presence of the Pu(V)-oxo species may decrease rather than increase the overall solubility of these compounds. Several additional aspects of the Pu speciation have also not been previously observed in laboratory-based samples. The molecular environmental chemistry of Pu is therefore likely to be more complicated than would be predicted based solely on the behavior of PuO{sub 2} under laboratory conditions.

  9. Speciation and gene flow between snails of opposite chirality.

    Directory of Open Access Journals (Sweden)


    Full Text Available Left-right asymmetry in snails is intriguing because individuals of opposite chirality are either unable to mate or can only mate with difficulty, so could be reproductively isolated from each other. We have therefore investigated chiral evolution in the Japanese land snail genus Euhadra to understand whether changes in chirality have promoted speciation. In particular, we aimed to understand the effect of the maternal inheritance of chirality on reproductive isolation and gene flow. We found that the mitochondrial DNA phylogeny of Euhadra is consistent with a single, relatively ancient evolution of sinistral species and suggests either recent "single-gene speciation" or gene flow between chiral morphs that are unable to mate. To clarify the conditions under which new chiral morphs might evolve and whether single-gene speciation can occur, we developed a mathematical model that is relevant to any maternal-effect gene. The model shows that reproductive character displacement can promote the evolution of new chiral morphs, tending to counteract the positive frequency-dependent selection that would otherwise drive the more common chiral morph to fixation. This therefore suggests a general mechanism as to how chiral variation arises in snails. In populations that contain both chiral morphs, two different situations are then possible. In the first, gene flow is substantial between morphs even without interchiral mating, because of the maternal inheritance of chirality. In the second, reproductive isolation is possible but unstable, and will also lead to gene flow if intrachiral matings occasionally produce offspring with the opposite chirality. Together, the results imply that speciation by chiral reversal is only meaningful in the context of a complex biogeographical process, and so must usually involve other factors. In order to understand the roles of reproductive character displacement and gene flow in the chiral evolution of Euhadra, it will be

  10. Speciation of Heavy Metals in Sediment of Agbabu Bitumen deposit ...

    African Journals Online (AJOL)

    Michael Horsfall

    ABSTRACT: Speciation of heavy metals Cu, Cd, Pb, Ni, Zn, Mn, Fe, Cr and Hg was carried out on sediment of. Agbabu with a sequential .... sulphide:The residue from fraction 3 was oxidized as follows: 3ml of 0.02M HNO3 and 5ml of ... Another 3ml of 30% hydrogen peroxide, adjusted to. pH2 with HNO3, was then added.



    Parikh Vikas C.; Karkhanis V.V


    A simple, sensitive and accurate UV spectrophotometric method has been developed for the determination of Gemfibrozil in bulk and pharmaceutical tablet dosage formulation. This method obeys Beer’s law in the concentration range of 30-90 µg/ml. with correlation coefficient of 0.9993 and exhibiting maximum absorption at 276 nm with apparent molar absorptivity of 0.1703 × 104 L mole-1 cm-1. The method is accurate and precise and is extended to pharmaceutical tablet dosage forms and there was no ...

  12. The role of male contest competition over mates in speciation

    Directory of Open Access Journals (Sweden)

    Anna QVARNSTRÖM, Niclas VALLIN, Andreas RUDH


    Full Text Available Research on the role of sexual selection in the speciation process largely focuses on the diversifying role of mate choice. In particular, much attention has been drawn to the fact that population divergence in mate choice and in the male traits subject to choice directly can lead to assortative mating. However, male contest competition over mates also constitutes an important mechanism of sexual selection. We review recent empirical studies and argue that sexual selection through male contest competition can affect speciation in ways other than mate choice. For example, biases in aggression towards similar competitors can lead to disruptive and negative frequency-dependent selection on the traits used in contest competition in a similar way as competition for other types of limited resources. Moreover, male contest abilities often trade-off against other abilities such as parasite resistance, protection against predators and general stress tolerance. Populations experiencing different ecological conditions should therefore quickly diverge non-randomly in a number of traits including male contest abilities. In resource based breeding systems, a feedback loop between competitive ability and habitat use may lead to further population divergence. We discuss how population divergence in traits used in male contest competition can lead to the build up of reproductive isolation through a number of different pathways. Our main conclusion is that the role of male contest competition in speciation remains largely scientifically unexplored [Current Zoology 58 (3: 490–506, 2012].

  13. The influence of speciation on the ecotoxic effects of heavy metals in aquatic systems

    DEFF Research Database (Denmark)

    Jensen, Karen S.; Borggaard, Ole K.; Hauschild, Michael Zwicky

    The fate, bioavailability and exposure of aquatic organisms to potentially toxic metals are strongly influenced by the speciation of the metal ions in the medium. Metal speciation is mainly controlled by pH, ionic strength, and presence of ligands ranging from small ions (e.g. citrate, EDTA...... for the total chemical mass emitted into the environment. In this study we show that by means of the metal speciation, EF can be corrected in such a way that the resulting CF becomes more accurate for each metal in the LCIA. The chemical speciation in various media was calculated by Visual Minteq ver. 2.......56. Calculations showed that the speciation is very dependent on the metal concentration and the composition of the media. A large variation in heavy metal toxicity for the same test organism was found for a given metal in different media. Our main hypothesis is that this is due to differences in speciation...

  14. The Effect of Bulk Depth and Irradiation Time on the Surface Hardness and Degree of Cure of Bulk-Fill Composites

    Directory of Open Access Journals (Sweden)

    Farahat F


    Full Text Available Statement of Problem: For many years, application of the composite restoration with a thickness less than 2 mm for achieving the minimum polymerization contraction and stress has been accepted as a principle. But through the recent development in dental material a group of resin based composites (RBCs called Bulk Fill is introduced whose producers claim the possibility of achieving a good restoration in bulks with depths of 4 or even 5 mm. Objectives: To evaluate the effect of irradiation times and bulk depths on the degree of cure (DC of a bulk fill composite and compare it with the universal type. Materials and Methods: This study was conducted on two groups of dental RBCs including Tetric N Ceram Bulk Fill and Tetric N Ceram Universal. The composite samples were prepared in Teflon moulds with a diameter of 5 mm and height of 2, 4 and 6 mm. Then, half of the samples in each depth were cured from the upper side of the mould for 20s by LED light curing unit. The irradiation time for other specimens was 40s. After 24 hours of storage in distilled water, the microhardness of the top and bottom of the samples was measured using a Future Tech (Japan- Model FM 700 Vickers hardness testing machine. Data were analyzed statistically using the one and multi way ANOVAand Tukey’s test (p = 0.050. Results: The DC of Tetric N Ceram Bulk Fill in defined irradiation time and bulk depth was significantly more than the universal type (p < 0.001. Also, the DC of both composites studied was significantly (p < 0.001 reduced by increasing the bulk depths. Increasing the curing time from 20 to 40 seconds had a marginally significant effect (p ≤ 0.040 on the DC of both bulk fill and universal studied RBC samples. Conclusions: The DC of the investigated bulk fill composite was better than the universal type in all the irradiation times and bulk depths. The studied universal and bulk fill RBCs had an appropriate DC at the 2 and 4 mm bulk depths respectively and

  15. Development of Low Density CaMg-A1-Based Bulk Metallic Glasses (Preprint)

    National Research Council Canada - National Science Library

    Senkov, O. N; Scott, J. M; Miracle, D. B


    Low density Ca-Mg-Al-based bulk metallic glasses containing additionally Cu and Zn, were produced by a copper mold casting method as wedge-shaped samples with thicknesses varying from 0.5 mm to 10 rom...

  16. Arsenic Speciation of Waters from the Aegean Region, Turkey by Hydride Generation: Atomic Absorption Spectrometry. (United States)

    Çiftçi, Tülin Deniz; Henden, Emur


    Arsenic in drinking water is a serious problem for human health. Since the toxicity of arsenic species As(III) and As(V) is different, it is important to determine the concentrations separately. Therefore, it is necessary to develop an accurate and sensitive method for the speciation of arsenic. It was intended with this work to determine the concentrations of arsenic species in water samples collected from Izmir, Manisa and nearby areas. A batch type hydride generation atomic absorption spectrometer was used. As(V) gave no signal under the optimal measurement conditions of As(III). A certified reference drinking water was analyzed by the method and the results showed excellent agreement with the reported values. The procedure was applied to 34 water samples. Eleven tap water, two spring water, 19 artesian well water and two thermal water samples were analyzed under the optimal conditions.

  17. Holographic bulk reconstruction with α' corrections (United States)

    Roy, Shubho R.; Sarkar, Debajyoti


    We outline a holographic recipe to reconstruct α' corrections to anti-de Sitter (AdS) (quantum) gravity from an underlying CFT in the strictly planar limit (N →∞ ). Assuming that the boundary CFT can be solved in principle to all orders of the 't Hooft coupling λ , for scalar primary operators, the λ-1 expansion of the conformal dimensions can be mapped to higher curvature corrections of the dual bulk scalar field action. Furthermore, for the metric perturbations in the bulk, the AdS /CFT operator-field isomorphism forces these corrections to be of the Lovelock type. We demonstrate this by reconstructing the coefficient of the leading Lovelock correction, also known as the Gauss-Bonnet term in a bulk AdS gravity action using the expression of stress-tensor two-point function up to subleading order in λ-1.

  18. Bulk amorphous Mg-based alloys

    DEFF Research Database (Denmark)

    Pryds, Nini


    and a low glass transition temperature. The alloys were prepared by using a relatively simple technique, i.e. rapid cooling of the melt in a copper wedge mould. The essential structural changes that are achieved by going from the amorphous to the crystalline state through the supercooled liquid state...... are discussed in this paper. On the basis of these measurements phase diagrams of the different systems were constructed. Finally, it is demonstrated that when pressing the bulk amorphous alloy onto a metallic dies at temperatures within the supercooled liquid region, the alloy faithfully replicates the surface......The present paper describes the preparation and properties of bulk amorphous quarternary Mg-based alloys and the influence of additional elements on the ability of the alloy to form bulk amorphous. The main goal is to find a Mg-based alloy system which shows both high strength to weight ratio...

  19. Orchestrating Bulk Data Movement in Grid Environments

    Energy Technology Data Exchange (ETDEWEB)

    Vazhkudai, SS


    Data Grids provide a convenient environment for researchers to manage and access massively distributed bulk data by addressing several system and transfer challenges inherent to these environments. This work addresses issues involved in the efficient selection and access of replicated data in Grid environments in the context of the Globus Toolkit{trademark}, building middleware that (1) selects datasets in highly replicated environments, enabling efficient scheduling of data transfer requests; (2) predicts transfer times of bulk wide-area data transfers using extensive statistical analysis; and (3) co-allocates bulk data transfer requests, enabling parallel downloads from mirrored sites. These efforts have demonstrated a decentralized data scheduling architecture, a set of forecasting tools that predict bandwidth availability within 15% error and co-allocation architecture, and heuristics that expedites data downloads by up to 2 times.

  20. Bulk Material Based Thermoelectric Energy Harvesting for Wireless Sensor Applications

    Energy Technology Data Exchange (ETDEWEB)

    Wang, W S; Magnin, W; Wang, N; Hayes, M; O' Flynn, B; O' Mathuna, C, E-mail: [Tyndall National Institute, Dyke Parade, Cork (Ireland)


    The trend towards smart building and modern manufacturing demands ubiquitous sensing in the foreseeable future. Self-powered Wireless sensor networks (WSNs) are essential for such applications. This paper describes bulk material based thermoelectric generator (TEG) design and implementation for WSN. A 20cm{sup 2} Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} based TEG was created with optimized configuration and generates 2.7mW in typical condition. A novel load matching method is used to maximize the power output. The implemented power management module delivers 651{mu}W to WSN in 50 deg. C. With average power consumption of Tyndall WSN measured at 72{mu}W, feasibility of utilizing bulk material TEG to power WSN is demonstrated.

  1. Copper speciation in municipal solid waste incinerator bottom ash leachates; Kopparformer i lakvatten fraan energiaskor

    Energy Technology Data Exchange (ETDEWEB)

    Olsson, Susanna; Gustafsson, Jon Petter [Royal Inst. of Tech., Stockholm (Sweden); Schaik, Joris van; Berggren Kleja, Dan [Swedish Univ. of Agricultural Sciences, Uppsala (Sweden); Hees, Patrick van [Oerebro Univ. (Sweden)


    The formation of copper (Cu) complexes with dissolved organic carbon (DOC) in bottom ash from municipal solid waste incineration (MSWI) may increase the total amount of Cu released but at the same time reduce its toxicity. In this study, DOC in a MSWI bottom ash leachate was characterized and the Cu-binding properties of different DOC fractions in the ash leachate and in a soil solution were studied. This knowledge may be used for improved environmental assessment of MSWI bottom ash in engineering applications. The Cu{sup 2+} activity at different pH values was measured potentiometrically using a Cu-ion selective electrode (Cu-ISE). Experimental copper complexation results were compared to speciation calculations made in Visual MINTEQ with the NICA-Donnan model and the Stockholm Humic Model (SHM). The MSWI bottom ash leachate contained a larger proportion of hydrophilic organic carbon than the investigated soil solution and other natural waters. The hydrophilic fraction of both samples showed Cu{sup 2+} binding properties similar to that of the bulk, cation-exchanged, leachate. For the ash leachate, the pH dependence of the Cu activity was not correctly captured by neither the SHM nor the NICA-Donnan model, but for the soil solution the model predictions of Cu speciation were in good agreement with the obtained results. The complex formation properties of the ash DOC appears to be less pH-dependent than what is assumed for DOC in natural waters. Hence, models calibrated for natural DOC may give inconsistent simulations of Cu-DOC complexation in MSWI bottom ash leachate. A Biotic Ligand Model for Daphnia Magna was used to provide an estimate of the copper concentrations at LC50 for a simulated bottom ash leachate. It was concluded that the Cu concentrations in certain bottom ash leachates are high enough to pose an ecotoxicological risk; however, after dilution and soil sorption, the risks for neighboring water bodies are most likely negligible. Three processes were

  2. Revisiting the particular role of host shifts in initiating insect speciation. (United States)

    Forbes, Andrew A; Devine, Sara N; Hippee, Alaine C; Tvedte, Eric S; Ward, Anna K G; Widmayer, Heather A; Wilson, Caleb J


    The notion that shifts to new hosts can initiate insect speciation is more than 150 years old, yet widespread conflation with paradigms of sympatric speciation has led to confusion about how much support exists for this hypothesis. Here, we review 85 insect systems and evaluate the relationship between host shifting, reproductive isolation, and speciation. We sort insects into five categories: (1) systems in which a host shift has initiated speciation; (2) systems in which a host shift has made a contribution to speciation; (3) systems in which a host shift has caused the evolution of new reproductive isolating barriers; (4) systems with host-associated genetic differences; and (5) systems with no evidence of host-associated genetic differences. We find host-associated genetic structure in 65 systems, 43 of which show that host shifts have resulted in the evolution of new reproductive barriers. Twenty-six of the latter also support a role for host shifts in speciation, including eight studies that definitively support the hypothesis that a host shift has initiated speciation. While this review is agnostic as to the fraction of all insect speciation events to which host shifts have contributed, it clarifies that host shifts absolutely can and do initiate speciation. © 2017 The Author(s). Evolution © 2017 The Society for the Study of Evolution.

  3. Thermal relics in cosmology with bulk viscosity

    Energy Technology Data Exchange (ETDEWEB)

    Iorio, A. [Charles University in Prague, Faculty of Mathematics and Physics, Prague (Czech Republic); Lambiase, G. [Universita di Salerno, Dipartimento di Fisica E.R. Caianiello, Fisciano (Italy); INFN, Gruppo Collegato di Salerno, Fisciano (Italy)


    In this paper we discuss some consequences of cosmological models in which the primordial cosmic matter is described by a relativistic imperfect fluid. The latter takes into account the dissipative effects (bulk viscosity) arising from different cooling rates of the fluid components in the expanding Universe. We discuss, in particular, the effects of the bulk viscosity on Big Bang Nucleosynthesis and on the thermal relic abundance of particles, looking at recent results of PAMELA experiment. The latter has determined an anomalous excess of positron events, which cannot be explained by conventional cosmology and particle physics. (orig.)

  4. A mechanistic analysis of bulk powder caking (United States)

    Calvert, G.; Curcic, N.; Ghadiri, M.


    Bulk powder transformations, such as caking, can lead to numerous problems within industry when storing or processing materials. In this paper a new Environmental Caking Rig (ECR) is introduced and has been used to evaluate the caking propensity of a hygroscopic powder as a function of temperature, Relative Humidity (RH), mechanical stress and also when RH is cycled. A linear relationship exists between cake strength and the extent of bulk deformation, here defined by the engineering strain. An empirical model has been used to predict the caking behaviour based on consolidation stress and environmental conditions.

  5. Synthesis of Bulk Superconducting Magnesium Diboride

    Directory of Open Access Journals (Sweden)

    Margie Olbinado


    Full Text Available Bulk polycrystalline superconducting magnesium diboride, MgB2, samples were successfully prepared via a one-step sintering program at 750°C, in pre Argon with a pressure of 1atm. Both electrical resistivity and magnetic susceptibility measurements confirmed the superconductivity of the material at 39K, with a transition width of 5K. The polycrystalline nature, granular morphology, and composition of the sintered bulk material were confirmed using X-ray diffractometry (XRD, scanning electron microscopy (SEM, and energy dispersive X-ray analysis (EDX.

  6. Cobalt speciation study in the cobalt-cysteine system by electrospray ionization mass spectrometry and anion-exchange chromatography inductively coupled plasma atomic emission spectrometry. (United States)

    Bresson, Carole; Colin, Christèle; Chartier, Frédéric; Moulin, Christophe


    This paper describes the ability of the combination of electrospray ionization mass spectrometry (ESI-MS) and anion-exchange chromatography coupled with inductively coupled plasma atomic emission spectrometry (AEC-ICP-AES) for cobalt speciation study in the binary cobalt-cysteine system. ESI-MS, allowing the identification and the characterization of the analytes, is used as a technique complementary to AEC-ICP-AES, providing elemental information on the separated species. The methods have been developed through the study of samples containing Co2+ and 1-fold to 5-fold molar ratios of cysteine over a pH range 2.5 to 11. In each case, cobalt-cysteine complexes were characterized by ESI-MS in negative ion mode. AEC-ICP-AES allowed further separation and detection of the cobalt species previously characterized. The strong influence of pH and ligand-to-metal ratios on the nature and stoichiometry of the species is demonstrated. For the first time, a direct experimental speciation diagram of cobalt species has been established owing to these analytical techniques. This work is a promising basis for the speciation analysis of cobalt, since a good knowledge of cobalt speciation is of prime importance to better understanding its fate in biological and environmental media.

  7. Use of Innovative and Advanced Computer Simulations of Chemical Speciation of Heavy Metals in Soils and Other Environmental Samples

    Directory of Open Access Journals (Sweden)

    Jeske Agnieszka


    Full Text Available The article presents several aspects of computer simulations and models of heavy metals speciation in environmental samples. The methods can be effectively used in environmental sciences, soil science, and assessment of mobility and bioavailability of heavy metals in contaminated areas. The article presents all of the methods based on examples, and with interpretation of results. The effect depends on the reliability of data used in models. The results are essential for predicting the fate and behaviour of elements in the environment, and can also be used to develop solubility curves.

  8. Testing of bulk tank milk for Salmonella Dublin infection in Danish dairy herds

    DEFF Research Database (Denmark)

    Wedderkopp, A.; Stroger, U.; Bitsch, V.


    of being test-negative in the third test round was 0.926 for a herd with 2 previous test-negative results. It was concluded that the investigated ELISA method was in general accordance with the cases of clinical S. Dublin infection recorded. and that the method has a potential for national screening......The usefulness of enzyme-linked immunosorbent assay (ELISA) was investigated as a simple method to screen for Salmonella Dublin infection in dairy herds, examining bulk tank milk samples for lipopolysaccharide (O:1,9,12) antibodies. The cut-off value for the ELISA on bulk tank milk was established...... based on individual milk samples (n = 2887) and bulk tank milk from 52 herds. Bulk tank milk samples (n = 5108) were collected from 1464 dairy herds located in 19 different areas. About 10% of the dairy herds in Denmark participated in the study. The percentage of herds changing from test...

  9. Characterisation of ferroelectric bulk materials and thin films

    CERN Document Server

    Cain, Markys G


    This book presents a comprehensive review of the most important methods used in the characterisation of piezoelectric, ferroelectric and pyroelectric materials. It covers techniques for the analysis of bulk materials and thick and thin film materials and devices. There is a growing demand by industry to adapt and integrate piezoelectric materials into ever smaller devices and structures. Such applications development requires the joint development of reliable, robust, accurate and - most importantly - relevant and applicable measurement and characterisation methods and models. In the past f


    NARCIS (Netherlands)


    We discuss the separation problem of bulk vs interface contributions in optical Second-Harmonic Generation (SHG). A new method is presented, which - in special cases - provides a full separation of all interface and bulk tenser components. The method is based on measurements in a thin-film geometry,

  11. Cellulosic ethanol byproducts as a bulking agent (United States)

    J.M. Considine; D. Coffin; J.Y. Zhu; D.H. Mann; X. Tang


    Financial enhancement of biomass value prior to pulping requires subsequent use of remaining materials; e.g., high value use of remaining stock material after cellulosic ethanol production would improve the economics for cellulosic ethanol. In this work, use of enzymatic hydrolysis residual solids (EHRS), a cellulosic ethanol byproduct, were investigated as a bulking...


    Directory of Open Access Journals (Sweden)



    Full Text Available This paper presents the experiments that were conducted on the installation of continuous bulking and thermofixing “SUPERBA” type TVP-2S for optimization of the plush yarns bulking process. There were considered plush yarns Nm 6.5/2, made of the fibrous blend of 50% indigenous wool sort 41 and 50% PES. In the first stage, it performs a thermal treatment with a turboprevaporizer at a temperature lower than thermofixing temperature, at atmospheric pressure, such that the plush yarns - deposed in a freely state on a belt conveyor - are uniformly bulking and contracting. It was followed the mathematical modeling procedure, working with a factorial program, rotatable central composite type, and two independent variables. After analyzing the parameters that have a direct influence on the bulking degree, there were selected the pre-vaporization temperature (coded x1,oC and the velocity of belt inside pre-vaporizer (coded x 2, m/min. As for the dependent variable, it was chosen the plush yarn diameter (coded y, mm. There were found the coordinates of the optimal point, and then this pair of values was verified in practice. These coordinates are: x1optim= 90oC and x 2optim= 6.5 m/min. The conclusion is that the goal was accomplished: it was obtained a good cover degree f or double-plush carpets by reducing the number of tufts per unit surface.

  13. Characteristics of bulk liquid undercooling and crystallization ...

    Indian Academy of Sciences (India)

    157–161. c Indian Academy of Sciences. Characteristics of bulk liquid undercooling and crystallization behaviors of jet electrodeposition Ni–W–P alloy. J K YU. ∗. , Y H WANG, G Z XING, Q QIAO, B LIU, Z J CHU, C L LI and F YOU. State Key Laboratory of Metastable Materials Science and Technology, Yanshan University,.

  14. Characteristics of bulk liquid undercooling and crystallization ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 38; Issue 1. Characteristics of bulk liquid undercooling and crystallization behaviors of jet electrodeposition Ni–W–P alloy. J K Yu Y H Wang G Z Xing Q Qiao B Liu Z J Chu C L Li F You. Volume 38 Issue 1 February 2015 pp 157-161 ...

  15. Failure by fracture in bulk metal forming

    DEFF Research Database (Denmark)

    Silva, C.M.A.; Alves, Luis M.; Nielsen, Chris Valentin


    This paper revisits formability in bulk metal forming in the light of fundamental concepts of plasticity,ductile damage and crack opening modes. It proposes a new test to appraise the accuracy, reliability and validity of fracture loci associated with crack opening by tension and out-of-plane shear...

  16. Thermal bulk polymerization of cholesteryl acrylate

    NARCIS (Netherlands)

    de Visser, A.C.; de Groot, K.; Feijen, Jan; Bantjes, A.


    The thermal bulk polymerization of cholesteryl acrylate was carried out in the solid phase, the mesomorphic phase, and the liquid phase to study the effect of monomer ordering on polymerization rate and polymer properties. The rate increased with decreasing ordering (or enhanced mobility) of the

  17. A large-scale biomass bulk terminal

    NARCIS (Netherlands)

    Wu, M.R.


    This research explores the possibility of a large-scale bulk terminal in West Europe dedicated to handle solid and liquid biomass materials. Various issues regarding the conceptual design of such a terminal have been investigated and demonstrated in this research: the potential biomass materials

  18. Bulk metamaterials: Design, fabrication and characterization

    DEFF Research Database (Denmark)

    Andryieuski, Andrei; Malureanu, Radu; Alabastri, Alessandro


    Bulk metamaterials claim a lot of attention worldwide. We report about our activity and advances in design, fabrication and characterization of metal-dielectric composites with three-dimensional lattices. The nomenclature of designs exhibiting negative index behaviour in the near infrared includes...

  19. Modelling ventilated bulk storage of agromaterials

    NARCIS (Netherlands)

    Grubben, N.L.M.; Keesman, K.J.


    Storage of season-dependent agro-materials is a key process in providing food, feed and biomass throughout the whole year. We review the state of the art in physical modelling, simulation and control of ventilated bulk storage facilities, and in particular the storage of potatoes, from a

  20. Teaching Advanced SQL Skills: Text Bulk Loading (United States)

    Olsen, David; Hauser, Karina


    Studies show that advanced database skills are important for students to be prepared for today's highly competitive job market. A common task for database administrators is to insert a large amount of data into a database. This paper illustrates how an up-to-date, advanced database topic, namely bulk insert, can be incorporated into a database…