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Bulk Samples (bulk + sample)
Selected AbstractsThe late Sandbian , earliest Katian (Ordovician) brachiopod immigration and its influence on the brachiopod fauna in the Oslo Region, NorwayLETHAIA, Issue 1 2008JESPER HANSEN Bulk samples of brachiopods from the middle and upper parts of the Arnestad Formation and the entire Frognerkilen Formation in the Oslo Region demonstrate major vertical changes in the Sandbian to Katian amphicratonic fauna of this part of the Baltic Province. The main influx of new taxa occurred in the upper part of the Arnestad Formation (uppermost Sandbian), and in the succeeding Frognerkilen Formation (basal Katian). Faunal change is initially reflected in an increase in diversity and not as a replacement of the previously incumbent genera, which remain throughout the studied sequence. The majority of the new genera migrated from the East Baltic Region or through this region from Avalonia, while the marginal Laurentian taxa first occupied the Scandinavian part of Baltica. Six taxa migrated from Laurentia, three from Avalonia, two from Gondwana and one apparently originated on the South China palaeoplate. The faunal shifts and immigration of brachiopods appear to have been in response to an initial transgression together with the movement of Baltica into more warm temperate latitudes, but the diverse faunas developed both against a background of subsequent regression and in response to an offshore shift of biofacies. The new amphicratonic fauna was thus generated by faunal shifts from elsewhere in the Baltic Province to the marginal environments of the Oslo Region together with more exotic elements from neighbouring continents and microcontinents. [source] Genetic variability of Tomato spotted wilt virus in Australia and validation of real time RT-PCR for its detection in single and bulked leaf samplesANNALS OF APPLIED BIOLOGY, Issue 4 2005R G DIETZGEN Summary The potential for large-scale use of a sensitive real time reverse transcription polymerase chain reaction (RT-PCR) assay was evaluated for the detection of Tomato spotted wilt virus (TSWV) in single and bulked leaf samples by comparing its sensitivity with that of DAS-ELISA. Using total RNA extracted with RNeasy® or leaf soak methods, real time RT-PCR detected TSWV in all infected samples collected from 16 horticultural crop species (including flowers, herbs and vegetables), two arable crop species, and four weed species by both assays. In samples in which DAS-ELISA had previously detected TSWV, real time RT-PCR was effective at detecting it in leaf tissues of all 22 plant species tested at a wide range of concentrations. Bulk samples required more robust and extensive extraction methods with real time RT-PCR, but it generally detected one infected sample in 1000 uninfected ones. By contrast, ELISA was less sensitive when used to test bulked samples, once detecting up to 1 infected in 800 samples with pepper but never detecting more than 1 infected in 200 samples in tomato and lettuce. It was also less reliable than real time RT-PCR when used to test samples from parts of the leaf where the virus concentration was low. The genetic variability among Australian isolates of TSWV was small. Direct sequencing of a 587 bp region of the nucleoprotein gene (S RNA) of 29 isolates from diverse crops and geographical locations yielded a maximum of only 4.3% nucleotide sequence difference. Phylogenetic analysis revealed no obvious groupings of isolates according to geographic origin or host species. TSWV isolates, that break TSWV resistance genes in tomato or pepper did not differ significantly in the N gene region studied, indicating that a different region of the virus genome is responsible for this trait. [source] Hardness Variation and Strain Distribution in Magnesium Alloy AZ31 Processed by Multi-pass Caliber Rolling,ADVANCED ENGINEERING MATERIALS, Issue 8 2009Tadanobu Inoue The evolution of microstructure and hardness with equivalent strain was studied in magnesium alloy AZ31 bars fabricated using a process of multi-pass caliber rolling at 473 K. The inhomogeneity of hardness throughout the cross section in the rolled bars was very similar to that of the strain predicted from FE simulation. The caliber rolling produced a fine-grain structure below 2.5 µm in a bulk sample with a length of over 1000 mm. [source] From Micro to Meso: an exercise in determining hydraulic conductivity of fractured sandstone cores from detailed characterization of the fracturesGEOPHYSICAL JOURNAL INTERNATIONAL, Issue 3 2006Salima Baraka-Lokmane SUMMARY Hydraulic conductivities of fractured sandstone bore cores of 0.1 m in diameter are calculated using detailed characterization of the fracture geometry parameters determined using a resin casting technique. The accuracy of the measurements was about 0.25,1.25 ,m with the image size used. The values of the effective fracture apertures vary between 10 ,m and 50 ,m. For modelling purposes the samples are sectioned serially, perpendicular to the flow direction along the cylinder axis. The hydraulic conductivity of individual slices is estimated by summing the contribution of the matrix (assumed uniform) and each fracture (depending on its length and aperture). Finally, the hydraulic conductivity of the bulk sample is estimated by a harmonic average in series along the flow path. Results of this geometrical upscaling compare favourably with actual conductivity measured in hydraulic and pneumatic experiments carried out prior to sectioning. This study shows that the determination of larger-scale conductivity can be achieved, based on the evaluation of fracture geometry parameters (e.g. fracture aperture, fracture width and fracture length), measured using an optical method, at least at the laboratory scale. [source] Very High Critical Field and Superior Jc -Field Performance in NdFeAsO0.82F0.18 with Tc of 51 K,ADVANCED MATERIALS, Issue 2 2009Xiaolin Wang A new family of oxypnictide superconductors, LaFeAsO0.89F0.11, brings new impetus to the field of high-temperature superconductivity. In this work, we show that the upper critical field values Hc2 (48 K) = 13 T and Hc2(0) can exceed 80,230 T in a high-pressure-fabricated NdO0.82F0.18FeAs bulk sample with Tc of 51 K. We also demonstrate the superior performance of supercurrent density in fields for this new superconductor. [source] Variations of magnetic susceptibility and fine quartz accumulation rate in Daisen loam over the past 200 000 years: Interaction between winter and summer monsoons in south-west JapanISLAND ARC, Issue 2 2001Jun-Ichi Kimura Abstract A loam section near Daisen volcano, South-west Japan, has been examined for low-field magnetic susceptibility (MS) and fine quartz accumulation rate. Fission track dating of tephra layers interbedded in the deposit shows that the loam age ranges from about 200 ka to the Present. The MS was measured for both bulk sample and the < 63 ,m fine fraction. Fine quartz contents in the < 63 ,m fraction were also determined using acid-alkali digestions and recalculated to derive fine quartz accumulation rate (Rqz). Grain size analysis was then carried out on the separated fine quartz. Low-field MS varies from low frequency magnetic suspectibility (,(LF)) 5 to 100 (× 10,6 m3/kg) for bulk samples and from 1 to 30 for fine fractions. The fine fraction ,(LF) variation correlated with Chinese loess MS stratigraphy, which indicated changes in pedogenic enhancement of the MS and is reflected by summer monsoon intensity. The Rqz are high in cool climate stages, with volumes between 0.2 and 0.4 (× 10,2 kg/m2 per yr), whereas in warm stages the rate falls to about 0.1. These values compare well with those reported from the Hokkaido and Kanto areas, suggesting the fine quartz originates from tropospheric dust. The strong winter monsoons during glacial stages alternated with weak summer monsoons as a result of a southward shift of the jet stream. In interglacials, summer monsoons were stronger. Seasonal alternating monsoons appear to have operated in South-west Japan through the past 200 000 years. [source] Effect of Oxygen Partial Pressure on the Formation of Metastable Phases from an Undercooled YbFeO3 Melt Using an Aerodynamic LevitatorJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 4 2009Malahalli S. Vijaya Kumar The Yb2O3,Fe2O3 system was studied to investigate the effect of oxygen partial pressure on the formation of metastable phases over a wide range of oxygen partial pressures from 105 to 10,1 Pa. Two kinds of metastable phases, with space groups of P63cm and P63/mmc, were found through rapid solidification of an undercooled YbFeO3 melt in an atmosphere with reduced Po2. The crystal structure of the as-solidified samples changed from orthorhombic Pbnm to hexagonal P63cm and P63/mmc with decreasing Po2. X-ray diffractometric and scanning electron microscopic results confirmed the existence of various phases in the as-solidified samples. The stabilities of each phase were studied by annealing the bulk sample in the thermogravimetric,differential thermal analysis (TG-DTA) furnace up to 1673 K, and the equilibrium phase diagram was constructed for the Yb,Fe,O system at 1473 K. TG analysis showed an increase of the sample mass during annealing and revealed that the existence of Fe2+, which has an ionic radius larger than that of Fe3+, decreases the tolerance factor and therefore destabilizes the perovskite structure. [source] Noble gas study of the Saratov L4 chondriteMETEORITICS & PLANETARY SCIENCE, Issue 3 2010Jun-ichi MATSUDA The Ar, Kr, and Xe concentrations in the HF/HCl residue are two orders of magnitude higher than those in the bulk sample, while He and Ne concentrations from both are comparable. The residue contains only a portion of the trapped heavy noble gases in Saratov; 40 ± 9% for 36Ar, 58 ± 12% for 84Kr, and 48 ± 10% for 132Xe, respectively. The heavy noble gas elemental pattern in the dissolved fraction is similar to that in the residue but has high release temperatures. Xenon isotopic ratios of the HF/HCl residue indicate that there is no Xe-HL in Saratov, but Ne isotopic ratios in the HF/HCl residue lie on a straight line connecting the cosmogenic component and a composition between Ne-Q and Ne-HL. This implies that the Ne isotopic composition of Q has been changed by incorporating Ne-HL (Huss et al. 1996) or by being mass fractionated during the thermal metamorphism. However, it is most likely that the Ne-Q in Saratov is intrinsically different from this component in other meteorites. The evidence of this is a lack of correlation between the isotopic ratio of Ne-Q and petrologic types of meteorites (Busemann et al. 2000). A neutron capture effect was observed in the Kr isotopes, and this process also affected the 128Xe/132Xe ratio. The 3He and 21Ne exposure ages for the bulk sample are 33 and 35 Ma, respectively. [source] Single-walled carbon nanotubes modified by PFO: An optical absorption and Raman spectroscopic investigationPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 11-12 2009P. Lukaszczuk Abstract In this contribution, we present preliminary results from an optical absorption and resonance Raman spectroscopic investigation on single-walled carbon nanotubes (SWCNT) functionalized by poly(9,9-dioctylfluorenyl-2,7-diyl)- co -bithiophene (PFO-BTP). A route for a stable suspension of SWCNT in a solution of fluorine-base copolymer is shown. Additionally, the detailed analysis of the supernatant and sediment after centrifugation of the functionalized sample is given. The resonance Raman and optical absorption spectroscopic data suggest that selective wrapping of the carbon nanotubes by PFO occurs. Additionally, one can see that the abundance of SWCNT in the supernatant in a bulk sample increased by a factor of 2. [source] Origin of electron spin resonance in La0.7Ca0.3MnO3PHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 2 2003Keon Woo Joh Abstract An electron spin resonance study was carried out for a La0.7Ca0.3MnO3 bulk sample above the ferromagnetic ordering temperature. From careful analysis on the ESR parameters, it is shown that itinerant spins interacting with magnetic spin clusters in bottleneck regime are responsible for the ESR signals. [source] Metallomacrocycles with a Difference: Macrocyclic Complexes with Exocyclic Ruthenium(II)-Containing DomainsCHEMISTRY - A EUROPEAN JOURNAL, Issue 43 2009Edwin Abstract The templated synthesis of organic macrocycles containing rings of up to 96 atoms and three 2,2,-bipyridine (bpy) units is described. Starting with the bpy-centred ligands 5,5,-bis[3-(1,4-dioxahept-6-enylphenyl)]-2,2,-bipyridine and 5,5,-bis[3-(1,4,7-trioxadec-9-enylphenyl)]-2,2,-bipyridine, we have applied Grubbs' methodology to couple the terminal alkene units of the coordinated ligands in [FeL3]2+ complexes. Hydrogenation and demetallation of the iron(II)-containing macrocyclic complexes results in the isolation of large organic macrocycles. The latter bind {Ru(bpy)2} units to give macrocyclic complexes with exocyclic ruthenium(II)-containing domains. The complex [Ru(bpy)2(L)]2+ (isolated as the hexafluorophosphate salt), in which L=5,5,-bis[3-(1,4,7,10-tetraoxatridec-12-enylphenyl)]-2,2,-bipyridine, undergoes intramolecular ring-closing metathesis to yield a macrocycle which retains the exocyclic {Ru(bpy)2} unit. The poly(ethyleneoxy) domains in the latter macrocycle readily scavenge sodium ions, as proven by single-crystal X-ray diffraction and atomic absorption spectroscopy data for the bulk sample. In addition to the new compounds, a series of model complexes have been fully characterized, and representative single-crystal X-ray structural data are presented for iron(II) and ruthenium(II) acyclic and macrocyclic species. [source] Crystal growth and structural refinement of NaMn7O12CRYSTAL RESEARCH AND TECHNOLOGY, Issue 10-11 2005E. Gilioli Abstract We report the crystal growth and the structural refinement of NaMn7O12, a manganite having a double perovskite structure. As in many similar compounds, there is coexistence of Mn3+ and Mn4+ but in this material they orderly occupy different sites for crystallographic reasons. Therefore, this peculiar structure can be considered as a model system for studying complex mechanisms such as charge, orbital and spin ordering. High purity bulk samples and "large" single crystals are needed to study tiny modifications in the crystallographic and magnetic structures associated to the ordering phenomena. Almost single phase (more than 96% pure) and single crystals (up to about 150 µm) of NaMn7O12 were synthesized by solid state reaction under pressure in a multi-anvil apparatus. Single crystal x-ray diffraction and SEM analysis have been used to characterize the crystals. The structure refinement indicates that NaMn7O12 crystallizes in the cubic Im3 space group, with a = 7.312 Å and Z = 2. Further studies are in progress to optimize the synthesis conditions, in order to grow larger crystals. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Method development and validation for the analysis of didanosine using micellar electrokinetic capillary chromatographyELECTROPHORESIS, Issue 21 2005Swapna Mallampati Abstract A selective MEKC method was developed for the analysis of didanosine in bulk samples. Successful separation of didanosine from 13 of its potential impurities, derived from the various synthetic preparation procedures, was achieved. As CZE gave poor separation selectivity, MEKC was preferable. The use of EKC allowed achievement of the separation in a significantly shorter time than conventional HPLC. An anionic long-chain surfactant, lithium dodecyl sulfate (LiDS), was used as the pseudostationary phase and sodium tetraborate buffer as the aqueous phase. In order to obtain the optimal conditions and to test the method robustness, a central composite response surface modeling experiment was performed. The optimized electrophoretic conditions include the use of an uncoated fused-silica capillary with a total length of 40,cm and an ID of 50,,m, a BGE containing 40,mM sodium tetraborate and 110,mM LiDS at pH,8.0, an applied voltage of 18.0,kV, and the capillary temperature maintained at 15°C. The method was found to be robust. The parameters for validation such as linearity, precision, and sensitivity are also reported. Three commercial bulk samples were analyzed with this system. [source] Magnitude and sources of uncertainties in soil organic carbon (SOC) stock assessments at various scalesEUROPEAN JOURNAL OF SOIL SCIENCE, Issue 5 2009E. Goidts Summary Uncertainties in soil organic carbon (SOC) stock assessments are rarely quantified even though they are critical in determining the significance of the results. Previous studies on this topic generally focused on a single variable involved in the SOC stock calculation (SOC concentration, sampling depth, bulk density and rock fragment content) or on a single scale, rather than using an integrated approach (i.e. taking into account interactions between variables). This study aims to apply such an approach to identify and quantify the uncertainties in SOC stock assessments for different scales and spatial landscape units (LSU) under agriculture. The error propagation method (, method) was used to quantify the relative contribution of each variable and interaction involved to the final SOC stock variability. Monte Carlo simulations were used to cross-check the results. Both methods converged (r2=0.78). As expected, the coefficient of variation of the SOC stock increased across scales (from 5 to 35%), and was higher for grassland than for cropland. Although the main source of uncertainty in the SOC stock varied according to the scale and the LSU considered, the variability of SOC concentration (due to errors from the laboratory and to the high SOC spatial variability) and of the rock fragment content were predominant. When assessing SOC stock at the landscape scale, one should focus on the precision of SOC analyses from the laboratory, the reduction of SOC spatial variability (using bulk samples, accurate re-sampling, high sampling density or stratified sampling), and the use of equivalent masses for SOC stock comparison. The regional SOC stock monitoring of agricultural soils in southern Belgium allows the detection of an average SOC stock change of 20% within 11 years if very high rates of SOC stock changes occur (1 t C ha,1 year,1). Amplitude et sources des incertitudes liées aux estimations des stocks de carbone organique dans le sol (COS) à différentes échelles Résumé Les erreurs associées aux estimations du stock de carbone organique dans le sol (COS) sont rarement quantifiées bien qu'elles puissent empêcher l'obtention de résultats significatifs. Les quelques études qui le font focalisent en général sur une seule variable nécessaire au calcul du stock de COS (concentration en COS, profondeur échantillonnée, densité apparente et contenu en fragments rocheux) ou sur une échelle spatiale particulière, sans utiliser d'approche intégrée (prenant en compte les interactions entre les variables). Cette étude a pour objectif d'utiliser une telle approche pour identifier et quantifier les incertitudes liées aux estimations de stock de COS à différentes échelles spatiales et pour diverses unités spatiales de paysages (USP) agricoles. La loi de propagation des erreurs (méthode ,) permet de quantifier la contribution relative de chaque variable et interaction à la variabilité finale du stock de COS. Les simulations de Monte Carlo sont utilisées pour la vérification croisée des résultats. Les deux méthodes ont convergé (r2= 0.78). Comme prévu, le coefficient de variation du stock de COS a proportionnellement augmenté avec l'échelle spatiale considérée (de 5 à 35%), et était plus élevé pour les cultures que pour les prairies. Bien que la principale source d'erreur sur le stock de COS soit fonction de l'échelle spatiale et du type d'USP considérés, la variabilité du contenu en COS (du fait des erreurs de laboratoire et de sa grande variabilité spatiale) et du contenu en fragments rocheux étaient prédominants. Lors de l'estimation des stocks de COS à l'échelle du paysage, l'attention devrait prioritairement porter sur la précision des analyses en COS du laboratoire, la réduction de la variabilité spatiale du COS (en utilisant des échantillons composites, un ré-échantillonnage précis, une densité d'échantillonnage élevée ou un échantillonnage stratifié), et sur l'utilisation de masses équivalentes pour comparer les stocks de COS. Le réseau régional de suivi des stocks de COS des sols agricoles dans le sud de la Belgique permet la détection d'un changement de stock de COS moyen de 20% en 11 ans pour un taux très élevé de changement en stock de COS (1 t C ha,1 year,1). [source] PCR-BASED TECHNIQUE FOR IDENTIFICATION AND DETECTION OF TRICHOGRAMMA SPP. (HYMENOPTERA: TRICHOGRAMMATIDAE) WITH SPECIFIC PRIMERSINSECT SCIENCE, Issue 3 2002LI Zheng-xi Abstract The rDNA-ITS2 regions of T. dendrolimi Matsumura and T. ostriniae Pang et Chen (Hymenoptera: Trichogrammatidae) were cloned and sequenced. The homologous sequences available in GenBank were retrieved and analyzed, and then specific primers were designed for molecular identification and detection of T. dendrolimi. Repeated screening showed that PCR amplification by the diagnostic primers enabled the differentiation of not only bulk samples and single adult (male or female), but also eggs and juveniles, which was not possible by conventional methods. The advantage of this system over morphology-based systems is that non-specialists are able to identify individuals or trace specimens efficiently. The derived molecular detection technique was then used to identify 12 specimens collected from different localities on the Chinese mainland; the results showed that this protocol could be applied to molecular monitoring of Trichogramma species in the field. Finally, 1132s of 6 geographical populations of T. dendrolimi (TdCHA, TDJL, TdXZ, TdKH, TdCZ and TdYBL) were cloned and sequenced. The multialignment analysis of intraspecific ITS2 sequences showed that the diagnostic primers have their own theoretical bases. [source] Influence of Wet Mechanical Mixing on Microstructure and Vickers Hardness of Nanocrystalline Ceramic,Metal CompositesINTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY, Issue 5 2008Tatsuo Kumagai Nanocrystalline (nc) ceramic,metal composite bulk samples have been fabricated by consolidation of mixture of attrition-milled (AM) amorphous base ceramic ((ZrO2,3 mol% Y2O3),20 mol% Al2O3) and AM amorphous base metallic (Ti,48 mol% Al) powders using a pulse-current pressure sintering system. Microstructural observations revealed that the ceramic and metallic colonies appear blocky in morphology in the composite bulk samples, and both the ceramic and the metallic colonies consist of a large number of equiaxed fine grains with the sizes of 78,82 and 81,86 nm, respectively. Mechanical mixing treatments by wet ball milling in ethanol before consolidation process are effective for refinement of the ceramic and metallic colonies. In all the obtained composite bulk samples, the ceramic colonies consist of the dominant phase of tetragonal (t) ZrO2 solid solution (ss) together with the minor phases of monoclinic (m) ZrO2ss and ,-Al2O3. On the other hand, the dominant phase in the metallic colonies changes from Ti3Al (,2) to Tiss (,) with an increase in the t -ZrO2ss volume fraction by abrasion of 3 mol% yttria-stabilized tetragonal polycrystalline zirconia balls during wet mechanical mixing treatments. Such a phase transformation from ,2 to , is considered to be due to the decrease in the aluminum content in the metallic colonies by combination of aluminum with oxygen (i.e., the formation of ,-Al2O3), which is probably taken from ethanol (C2H5OH) into the powders during wet mechanical mixing treatments. The obtained nc composite bulk samples show good Vickers hardness values, which are considerably higher than those estimated from the rule of mixture. [source] Variations of magnetic susceptibility and fine quartz accumulation rate in Daisen loam over the past 200 000 years: Interaction between winter and summer monsoons in south-west JapanISLAND ARC, Issue 2 2001Jun-Ichi Kimura Abstract A loam section near Daisen volcano, South-west Japan, has been examined for low-field magnetic susceptibility (MS) and fine quartz accumulation rate. Fission track dating of tephra layers interbedded in the deposit shows that the loam age ranges from about 200 ka to the Present. The MS was measured for both bulk sample and the < 63 ,m fine fraction. Fine quartz contents in the < 63 ,m fraction were also determined using acid-alkali digestions and recalculated to derive fine quartz accumulation rate (Rqz). Grain size analysis was then carried out on the separated fine quartz. Low-field MS varies from low frequency magnetic suspectibility (,(LF)) 5 to 100 (× 10,6 m3/kg) for bulk samples and from 1 to 30 for fine fractions. The fine fraction ,(LF) variation correlated with Chinese loess MS stratigraphy, which indicated changes in pedogenic enhancement of the MS and is reflected by summer monsoon intensity. The Rqz are high in cool climate stages, with volumes between 0.2 and 0.4 (× 10,2 kg/m2 per yr), whereas in warm stages the rate falls to about 0.1. These values compare well with those reported from the Hokkaido and Kanto areas, suggesting the fine quartz originates from tropospheric dust. The strong winter monsoons during glacial stages alternated with weak summer monsoons as a result of a southward shift of the jet stream. In interglacials, summer monsoons were stronger. Seasonal alternating monsoons appear to have operated in South-west Japan through the past 200 000 years. [source] The new V12 ultra-small-angle neutron scattering and tomography instrument at the Hahn,Meitner InstitutJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2007M. Strobl The new V12 instrument at the Hahn,Meitner Institute in Berlin is a multiple setup combining several techniques to investigate the internal structure of bulk samples. It consists of two double-crystal diffractometers (DCDs) and an attenuation tomography device operating with monochromatic neutrons. The three instrument parts can be used independently at the same time. The DCDs are mainly used in the ultra-small-angle neutron scattering (USANS) regime, where they overlap the accessible range of small-angle neutron scattering instruments, while tomographic methods collect real-space information on a macroscopic scale. Together they enable structural investigations over six orders of magnitude (50,nm to 5,cm). Scattering and tomographic methods can even be combined by means of diffraction and scattering-enhanced imaging. The sample environment can be varied over a large range of temperatures and pressures for USANS measurements and a polarized USANS option is available. [source] A study of sulfamerazine single crystals using atomic force microscopy, transmission light microscopy, and Raman spectroscopyJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 9 2005Xiaoping Cao Abstract Sulfamerazine (SMZ) Form I and II single crystals were prepared from aqueous dispersions of SMZ bulk samples and studied using several microscopic and spectroscopic techniques. Transmission light microscopy and Raman spectroscopy were used to observe and identify single crystals. The results indicated that Form I single crystals tended to be rectangular laths while Form II ones tended to be hexagonal laths. Surface morphology of individual single crystals was further investigated by atomic force microscopy (AFM). AFM images revealed a smooth top surface, a uniform height, and sharp edges for both forms of single crystals. Both height and phase images showed crystalline terraces with different step heights for the top surface of Form I. Surface properties of single crystals were evaluated using AFM force measurements. Experimental results indicated that the top surface of Form I single crystals was more hydrophilic than that of Form II. Theoretical calculations predicted a dominant crystal face of (020) for the Form I single crystals and (002) for the Form II ones. The correlations between calculation predictions and experimental results were discussed. © 2005 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 94:1881,1892, 2005 [source] Compound-specific stable-isotope (,13C) analysis in soil scienceJOURNAL OF PLANT NUTRITION AND SOIL SCIENCE, Issue 5 2005Bruno Glaser Abstract This review provides current state of the art of compound-specific stable-isotope-ratio mass spectrometry (,13C) and gives an overview on innovative applications in soil science. After a short introduction on the background of stable C isotopes and their ecological significance, different techniques for compound-specific stable-isotope analysis are compared. Analogous to the ,13C analysis in bulk samples, by means of elemental analyzer,isotope-ratio mass spectrometry, physical fractions such as particle-size fractions, soil microbial biomass, and water-soluble organic C can be analyzed. The main focus of this review is, however, to discuss the isotope composition of chemical fractions (so-called molecular markers) indicating plant- (pentoses, long-chain n-alkanes, lignin phenols) and microbial-derived residues (phospholipid fatty acids, hexoses, amino sugars, and short-chain n-alkanes) as well as other interesting soil constituents such as "black carbon" and polycyclic aromatic hydrocarbons. For this purpose, innovative techniques such as pyrolysis,gas chromatography,combustion,isotope-ratio mass spectrometry, gas chromatography,combustion,isotope-ratio mass spectrometry, or liquid chromatography,combustion,isotope-ratio mass spectrometry were compared. These techniques can be used in general for two purposes, (1) to quantify sequestration and turnover of specific organic compounds in the environment and (2) to trace the origin of organic substances. Turnover times of physical (sand < silt < clay) and chemical fractions (lignin < phospholipid fatty acids < amino sugars , sugars) are generally shorter compared to bulk soil and increase in the order given in brackets. Tracing the origin of organic compounds such as polycyclic aromatic hydrocarbons is difficult when more than two sources are involved and isotope difference of different sources is small. Therefore, this application is preferentially used when natural (e.g., C3-to-C4 plant conversion) or artificial (positive or negative) 13C labeling is used. Substanzspezifische Stabilisotopenanalyse (,13C) in der Bodenforschung Dieser Artikel fasst den Stand der Forschung bezüglich der substanzspezifischen Stabilisotopenanalyse (,13C) zusammen. Innovative Anwendungen und ein Ausblick für künftige Forschungsaktivitäten werden anhand von Fallbeispielen gegeben. Zunächst wird die ökologische Bedeutung von stabilen C-Isotopen kurz erläutert. Daran schließt sich ein methodischer Teil an, in welchem die verschiedenen Techniken gegenüber gestellt werden. Analog zu ,13C-Messungen der Feinerde mittels Elementaranalysator-Isotopenverhältnis-Massenspektrometrie können physikalisch isolierte Fraktionen (z.,B. Korngrößenfraktionen, mikrobielle Biomasse, DOC) analysiert werden. Der Schwerpunkt dieses Übersichtsartikels liegt jedoch in der Diskussion der C-Isotopensignatur chemischer Fraktionen (sog. Biomarker), welche Rückschlüsse auf Herkunft und Dynamik pflanzlicher (Pentosen, langkettige n-Alkane, Ligninphenole) und mikrobieller Rückstände (Phospholipidfettsäuren, Hexosen, Aminozucker und kurzkettige n-Alkane) sowie anderer interessanter Substanzen im Boden erlaubt wie z.,B. ,Black Carbon" und polyzyklische aromatische Kohlenwasserstoffe. Zu diesem Zweck kommen innovative Techniken zum Einsatz wie z.,B. Pyrolyse-Gaschromatographie-Isotopenverhältnismassenspektrometrie, Gaschromatographie-Verbrennungs-Isotopenverhältnismassenspektrometrie und Flüssigkeitschromatographie-Oxidations-Isotopenverhältnismassenspektrometrie. Innovative ökologische Anwendungen werden erläutert, welche sich prinzipiell in zwei Kategorien einteilen lassen: (1) Quantifizierung der Sequestrierung und des Umsatzes dieser Verbindungen in der Umwelt; (2) Untersuchung der Herkunft spezifischer organischer Substanzen. Umsatzzeiten physikalischer (Sand < Schluff < Ton) und chemischer Fraktionen (Lignin < Phospholipidfettsäuren < Aminozucker , Zucker) sind generall kleiner als jene der gesamten organischen Substanz in der Feinerde und nehmen in der in Klammern angegebenen Reihenfolge zu. Die Untersuchung der Herkunft organischer Substanzen (z.,B. polyzyklischer aromatischer Kohlenwasserstoffe) ist problematisch, weil die Unterschiede der Isotopensignatur verschiedener Quellen gering sind und meist mehr als zwei Quellen zur Isotopensignatur des untersuchten Biomarkers beitragen. Deswegen sollte die Untersuchung der Herkunft organischer Substanzen auf Tracer-Experimente beschränkt werden, wie z.,B. nach natürlicher (C3-C4-Pflanzenwechsel) bzw. künstlicher (13C-An- oder -Abreicherung) Markierung. [source] Raman studies and optical properties of some (PbO)x(Bi2O3)0.2(B2O3)0.8,x glassesJOURNAL OF RAMAN SPECTROSCOPY, Issue 9 2008Katerina Kotkova Abstract Five (PbO)x(Bi2O3)0.2(B2O3)0.8,x glasses, where x = 0, 0.2, 0.3, 0.4 and 0.6, were prepared. The dilatometric glass transition temperature (Tg) was found in the region 470 (x = 0), Tg ( °C) , 347 (x = 0.6), and the density (,) varied within 4.57 (x = 0) , , (g/cm3) , 8.31 (x = 0.6). Raman spectra indicated the conversion of BO3 to BO4 entities for low x values but for x > 0.3, namely, for x , 0.6, back-conversion occurred, most probably. From the measurements of the optical transmission on very thin bulk samples, the room temperature optical gap values (Eg) were determined to be in the range 4.03 (x = 0), Eg (eV) , 3.08 (x = 0.6). The temperature (T) dependence of the optical gap (Eg(T)) in the region 300 , T(K) , 600 was examined and approximated by a linear relationship of the form of Eg(T) = Eg(0), ,T, where , × 10,4(eV/K) varied from 5.1 to 6.8. The non-linear refractive index (n2) was estimated from the optical gap values and it was found to correspond to the n2 values calculated from the experimental third-order non-linear optical susceptibility taken from the literature. Copyright © 2008 John Wiley & Sons, Ltd. [source] Field sampling bias, museum collections and completeness of the fossil recordLETHAIA, Issue 4 2005AARON HUNTER Museum specimens, particularly old collections, typically lack comprehensive field data and determination of substrate, sampling biases, etc., is problematic. Diversity at the generic level of all identifiable latest Cretaceous (Campanian,Maastrichtian) echinoderm remains in major museum collections from the Mons (southern Belgium) and Danish (Jylland (Jutland) and Sjælland (Zealand)) basins were compared to those of the Liège-Limburg Basin. The last-named has been studied in detail, including microscopical analysis of ossicles picked from bulk samples. Echinoids of the Mons Basin show similarities to those of the Liège-Limburg Basin, but crinoids, asteroids and ophiuroids remain poorly known from the former. Echinoderms of the Danish Basin resemble those of similar chalk lithofacies in the Liège-Limburg Basin, despite significant geographical separation. These disparities can be explained, at least in part, by collector bias in sampling methodology, although differences in substrate presumably also had an influence. [source] The fine-grained matrix of the Semarkona LL3.0 ordinary chondrite: An induced thermoluminescence studyMETEORITICS & PLANETARY SCIENCE, Issue 5 2009Jonathan P. CRAIG The samples had TL sensitivities comparable with 4 mg of bulk samples of type 3.2,3.4 ordinary chondrites, which is very high relative to bulk Semarkona. The other induced TL properties of these samples, TL peak temperatures, and TL peak widths distinguish them from other ordinary chondrite samples where the TL is caused by feldspar. Cathodoluminescence images and other data suggest that the cause of the luminescence in the Semarkona fine-grained matrix is forsterite. In some respects the matrix TL data resemble that of Semarkona chondrules, in which the phosphor is forsterite and terrestrial forsterites from a variety of igneous and metamorphic environments. However, differences in the TL peak temperature versus TL peak width relationship between the matrix samples and the other forsterites suggest a fundamentally different formation mechanism. We also note that forsterite appears to be a major component in many primitive materials, such as nebulae, cometary dust, and Stardust particles. [source] Isotopic compositions of different presolar silicon carbide size fractions from the Murchison meteoriteMETEORITICS & PLANETARY SCIENCE, Issue 5 2000Sachiko AMARI Ratios of 12C/13C range from 37 to 42 and 14N/15N ratios from 370 to 520, within the range of single-grain measurements on coarser samples and in agreement with an asymptotic giant branch (AGB) star origin of most of the grains. Variations among size fractions do not show any simple trend and can be explained by varying contamination with isotopically normal material. Silicon isotopic ratios vary only little and, with one exception, lie to the right of the singlegrain mainstream correlation line. This might indicate a higher percentage of the minor populations Y and Z among finer grain-size fractions. All bulk samples have large 26Mg excesses attributed to the presence of short-lived 26Al at the time of grain formation. Inferred 26Al/27Al ratios are much larger than those measured in single larger mainstream grains. This is probably because of the presence of SiC grains of type X; we obtain an estimate of 0.4 for their 26Al/27Al ratio. Our Ca-isotopic measurements, the first made on presolar SiC grains, show excesses in 42Ca and 43Ca, which is in general agreement with theoretical expectations for AGB stars. Calcium-44 excesses are much larger than expected and are probably because of X grains, which have high44Ca excesses because of the decay of short-lived 44Ti produced in supernova explosions. We arrive at an estimate of 0.014 for the initial 44Ti/48Ti ratio of the X grains, within the range obtained from previous single X grain measurements. The Ti-isotopic ratios of the bulk samples show a V-shaped pattern with excesses of all isotopes relative to 48Ti. Isotopes 46Ti, 47Ti, and 50Ti show excesses relative to the correlation between Ti and Si ratios for single grains and are in general agreement with theoretical models of s-process nucleosynthesis in AGB stars. In contrast, 49Ti does not show any excess relative to the singlegrain data; it also fails to agree with theory, which predicts much larger excesses than observed. Measured 53Cr/52Cr and 57Fe/56Fe ratios are normal within errors. The first result is expected even for Cr in AGB star envelopes, but the second result suggests that most of the Fe analyzed originates from contamination. We have found no simple trends in isotopic composition with respect to grain size that can be interpreted in terms of nucleosynthetic origin, unlike the results for Kr, Xe, Ba, and Sr. [source] Bulk and patch ferrite resonator antennas based on the ceramic matrix composite: GdIGx YIG1- xMICROWAVE AND OPTICAL TECHNOLOGY LETTERS, Issue 6 2009P. B. A. Fechine Abstract In this study, the dielectric properties of the GdIGXYIG1,X ferrite composite material at radio frequency (RF) and microwave frequency bands were studied. These measurements were carried out in different sample geometries: thick films and cylindrical ceramic bulk ferrite resonator. In the RF range, we observed that the material is rather stable because of its short changes as a function of temperature and frequency range. The temperature capacitance coefficient values for all the samples (thick films and cylindrical ceramic bulk samples) presented short positive values at the RF range. The GdIG0.5YIG0.5 thick film was used as a substrate for the microstrip antenna device, where the upper Ag electrode served as a circular patch antenna and a microstrip line was used as a feed line. The microstrip antenna operates in this configuration at 8.185 GHz. In the study of the dielectric properties of the composites antenna geometry, with the same ferrite composite, a bulk cylindrical geometry was investigated. A numerical study, together with the experimental, was done, and the dielectric characteristics of the composite like ,r, tg,E, and ,r were obtained. © 2009 Wiley Periodicals, Inc. Microwave Opt Technol Lett 51: 1595,1602, 2009; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/mop.24395 [source] The recovery of the shear viscosity of thermally aged bulk and ribbon glassy Pd40Cu30Ni10P20 by rapid quenching from the supercooled liquid statePHYSICA STATUS SOLIDI - RAPID RESEARCH LETTERS, Issue 2-3 2009V. A. Khonik Abstract Isochronal (= linear heating) measurements of the shear viscosity below the glass transition of bulk and ribbon glassy Pd40Cu30Ni10P20 samples differing ,104 -fold in the production quenching rates have been performed. It has been found that heating up into the supercooled liquid region followed by slow cooling leads to a significant structural relaxation-induced viscosity increase upon subsequent testing. This increase, however, is not truly irreversible and the viscosity can be fully recovered (= decreased) by fast quenching from the supercooled liquid state. The effect is nearly independent of whether ribbon or bulk samples are used despite the fact that those latter are notably denser. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Strong Eu emission of annealed Y2O3:Eu nanotube and nano-sized crystalsPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 13 2004Masami Sekita Abstract We have observed a drastic increase of the Eu3+ emission intensity by annealing nanotubes and nano-sized hexagonal-mesostructured crystals of the Y2O3:Eu system together with bulk samples. It is found that there are three Eu3+ sites in all samples. Stark splitting schemes are proposed for the three homogeneous sites. (© 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Photoluminescence properties of erbium-doped amorphous gallium-germanium-selenium films fabricated by RF sputteringPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue S1 2009Takahiko Imai Abstract Chalcogenide glasses have various useful features for optical devices such as a high refractive index, low-loss transmission in the mid-IR, and low phonon energies. The fabrication of thin films is important for use in waveguide applications and integrated photonics. In this work, we report the properties of vacuum deposited films of gallium-germanium-selenium glasses onto fused silica substrates by an RF magnetron sputtering technique (RF electric power of 40-250 W and growth rate of 0.01-2.1 ,m/min). The concentration of Er3+ ions is controlled by the number of sintered Er2S3 small plates on a target. Samples are shown to be in an amorphous-like state as measured by X-ray diffraction experiments. Film thicknesses are proportional to the RF sputtering power and sputtering time. The compositions of films obtained from energy dispersive X-ray (EDX) analysis. There are much dependent on the condition of the sputtering target, for example whether the target is in the bulk or powder-state. Photoluminescence (PL) spectrum, intensity, and lifetime at 1550 nm band are measured by excitation from a 973 nm laser. The PL band of the films has a similar shape to those of bulk glasses. The PL intensity increased with the RF electric power. The PL lifetime at the 1550 nm band of the film is about 1.8-2.6 ms; the latter values are similar to those of bulk samples. The results show that the RF sputtering is a potential method of fabrication for Er-doped GeGaSe thin films. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Microwave absorption of ferrite powders in a polymer matrixPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 5 2006S. Kolev Abstract The object of this work is to investigate the microwave absorbing properties of nanocomposite bulk samples. As filler we used magnetite with different particle size in a silicone rubber matrix and investigated the influence of the filler concentration and particle size in the polymer matrix on the microwave nonlinearity in a large frequency range (1 ÷ 13 GHz). We found that the intensity and the frequency at the reflection loss minimum depend on the particle size and particle concentration of magnetite in the samples. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] High-speed and high-frequency electron effects in nitride semiconductors for terahertz applicationsPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 7 2005K. W. Kim Abstract We discuss the basic properties of the transient hot-electron transport and dynamic mobility in group-III nitrides under dominant electron,polar-optical-phonon scattering determining their capability for applications in THz frequency range. For bulk samples with high electron concentration, we provide the phase-plane analysis of the time-dependent transient transport and classification of different transient regimes depending on the initial conditions. The calculations predict a frequency interval with negative dynamic electron mobility where the amplification and generation of microwaves in THz frequency range is possible. For quantum-well heterostructures with low electron concentration under the streaming regime at moderate fields, we have revealed THz frequency windows of the negative microwave mobility, which enables the development of a tunable THz laser based on nitride quantum heterostructures. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] | ||||||||||||||||||||||