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Analytical Techniques (analytical + techniques)
Kinds of Analytical Techniques Selected AbstractsAnalytical Techniques for Nucleation Studies in Lipids: Advantages and DisadvantagesJOURNAL OF FOOD SCIENCE, Issue 9 2004M. Cerdeira ABSTRACT: Crystallization is generally considered a 2-step process. The 1st step, nucleation, involves the formation of molecular aggregates with a critical size great enough to become stable. During the 2nd step, nuclei grow and develop into crystals. Distinguishing between nucleation and growth constitutes a major challenge in lipid crystallization studies. Thus, it is of great importance to discuss the information obtained from the different techniques that are usually used to study nucleation behavior such as nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), rheological techniques, light-scattering techniques such as turbidimetry and scanning diffusive light scattering (SDLS), polarized light microscopy (PLM), and laser polarized optical sets such as laser polarizedlight turbidimetry (LPLT). Techniques to describe the nucleation process must be very sensitive to disregard growth. When crystallization is followed by methods such as DSC, NMR, and rheological measurements, at times, small amounts of crystals are present in the melt before any solids are detected. Clearly, at this stage, well beyond the induction time for nucleation (,), these methods are measuring crystal growth. Techniques of low sensitivity for solid fat contents lower than 0.1% must not be used to evaluate nucleation effects. Sensitive turbidimeters with detectors that saturate below 0.3% solid fat content give good results as do scanning diffusive light-scattering equipment. Although the PLM technique is sensitive enough for these kinds of studies, an understanding of important basic concepts is essential. Laser optical sets are the most appropriated methods to study nucleation in fats systems. [source] Current Awareness in Labelled Compounds and RadiopharmaceuticalsJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 4 2010Article first published online: 21 APR 2010 In order to keep subscribers up-to-date with the latest developments in their field, John Wiley & Sons are providing a current awareness service in each issue of the journal. The bibliography contains newly published material in the field of labelled compounds and radiopharmaceuticals. Each bibliography is divided into 16 sections: 1 Radionuclide Production; 2 Labelled Compound Synthesis; Applications: 3 Biomedical - General; 4 Imaging - General; 5 Fluorine; 6 Carbon; 7 Technetium; 8 Iodine; 9 Copper; 10 Gallium; 11 Indium; 12 Hydrogen; 13 Others; 14 Therapy; 15 Environmental; 16 Analytical Techniques. Within each section, articles are listed in alphabetical order with respect to author. If, in the preceding period, no publications are located relevant to any one of these headings, that section will be omitted. [source] Current Awareness in Labelled Compounds and RadiopharmaceuticalsJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 14 2009Article first published online: 15 DEC 200 In order to keep subscribers up-to-date with the latest developments in their field, John Wiley & Sons are providing a current awareness service in each issue of the journal. The bibliography contains newly published material in the field of labelled compounds and radiopharmaceuticals. Each bibliography is divided into 16 sections: 1 Radionuclide Production; 2 Labelled Compound Synthesis; Applications: 3 Biomedical - General; 4 Imaging - General; 5 Fluorine; 6 Carbon; 7 Technetium; 8 Iodine; 9 Copper; 10 Gallium; 11 Indium; 12 Hydrogen; 13 Others; 14 Therapy; 15 Environmental; 16 Analytical Techniques. Within each section, articles are listed in alphabetical order with respect to author. If, in the preceding period, no publications are located relevant to any one of these headings, that section will be omitted. [source] Current Awareness in Labelled Compounds and RadiopharmaceuticalsJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 12 2009Article first published online: 11 NOV 200 In order to keep subscribers up-to-date with the latest developments in their field, John Wiley & Sons are providing a current awareness service in each issue of the journal. The bibliography contains newly published material in the field of labelled compounds and radiopharmaceuticals. Each bibliography is divided into 16 sections: 1 Radionuclide Production; 2 Labelled Compound Synthesis; Applications: 3 Biomedical - General; 4 Imaging - General; 5 Fluorine; 6 Carbon; 7 Technetium; 8 Iodine; 9 Copper; 10 Gallium; 11 Indium; 12 Hydrogen; 13 Others; 14 Therapy; 15 Environmental; 16 Analytical Techniques. Within each section, articles are listed in alphabetical order with respect to author. If, in the preceding period, no publications are located relevant to any one of these headings, that section will be omitted. [source] Current Awareness in Labelled Compounds and RadiopharmaceuticalsJOURNAL OF LABELLED COMPOUNDS AND RADIOPHARMACEUTICALS, Issue 8 2009Article first published online: 9 JUL 200 In order to keep subscribers up-to-date with the latest developments in their field, John Wiley & Sons are providing a current awareness service in each issue of the journal. The bibliography contains newly published material in the field of labelled compounds and radiopharmaceuticals. Each bibliography is divided into 16 sections: 1 Radionuclide Production; 2 Labelled Compound Synthesis; Applications: 3 Biomedical - General; 4 Imaging - General; 5 Fluorine; 6 Carbon; 7 Technetium; 8 Iodine; 9 Copper; 10 Gallium; 11 Indium; 12 Hydrogen; 13 Others; 14 Therapy; 15 Environmental; 16 Analytical Techniques. Within each section, articles are listed in alphabetical order with respect to author. If, in the preceding period, no publications are located relevant to any one of these headings, that section will be omitted. [source] Cancer Biomarkers , Analytical Techniques for Discovery Wiley-Interscience Series on Mass Spectrometry.PROTEOMICS - CLINICAL APPLICATIONS, Issue 10 2007By Mahmoud H. Hamdan No abstracts. [source] Molecular-cytogenetic comparison of mucosa-associated marginal zone B-cell lymphoma and large B-cell lymphoma arising in the gastro-intestinal tractGENES, CHROMOSOMES AND CANCER, Issue 4 2001Thomas F.E. Barth Extranodal B-cell lymphoma of mucosa-associated lymphoid tissue (MALT) type may represent a model of lymphoma progression, because a small cell component frequently occurs in the large cell variants. We studied 52 extranodal B-cell lymphomas: 18 extranodal marginal zone B-cell lymphomas of MALT type (MZBL,MT), 7 MZBL,MT of the gastro-intestinal tract with a diffuse large B-cell component (giMZBLplusLBCL), and 27 diffuse large B-cell lymphomas of the gastro-intestinal tract without small cell component (giLBCL). Analytical techniques were comparative genomic hybridization (CGH) and fluorescence in situ hybridization (FISH). The translocation t(11;18) was found as the sole aberration in two MZBL,MT only. In contrast to this, t(11;18)-negative MZBL,MT were characterized by frequent gains on chromosome 3 and DNA amplifications on 2p13,p15. Furthermore, we found a clonal lymphoma progression from the small to the large cell component with accumulation of gains and losses of chromosomal material in the large cell component in giMZBLplusLBCL. Aberrations overlapping with MZBL,MT and giMZBLplusLBCL included losses on chromosome 13, amplifications of the REL proto-oncogene, or gains on chromosome 12. In addition, the large cell component revealed gains on 8q24, including amplifications of the MYC proto-oncogene, and losses on 2q. The giLBCL had frequent gains on chromosomes 12 and 9, as well as on 11q, and losses on 6q. We conclude that, based on the distinctive and partly overlapping patterns of genetic aberrations, MALT lymphomas can be divided into different genetic subgroups. © 2001 Wiley-Liss, Inc. [source] Effects of host mineral re-equilibration during uplift and cooling on the fidelity of primary hydrothermal fluid inclusions: a theoretical example using Mississippi Valley-type ore fluidsGEOFLUIDS (ELECTRONIC), Issue 2 2009M. A. McKIBBEN Abstract At the moment of its trapping as a primary fluid inclusion, a hydrothermal fluid is typically at or near equilibrium with multiple mineral species at depth and temperature. After trapping, however, the isolated inclusion fluid can re-equilibrate only with its own host mineral species during later uplift and cooling to surface conditions. Because the solubility versus temperature behavior is unique for each host mineral species, identical inclusions trapped at the same time within different species may re-equilibrate in a disparate manner upon cooling and become variably less representative of the original trapped fluid once they reach ambient temperature. To test the significance of this effect, a series of theoretical equilibrium reaction models was constructed in which a trapped hydrothermal fluid characteristic of Mississippi Valley-type ore deposits is cooled in contact with silicate, sulfide and carbonate hosts, respectively, from 100 to 25°C. Dissolved base metal concentrations are predicted to decline by two to four orders of magnitude in inclusions in all hosts, due to the precipitation of optically undetectable masses of sulfide daughter minerals. Fluids in the calcite host show the greatest decline in dissolved base metals upon cooling, due to its retrograde solubility and consequent shift in the pH and aqueous C speciation of the fluid. ,13C values for CO2 in all hosts become depleted by 2,7, relative to the original trapped fluid, with depletions again being the greatest for the calcite host due to its retrograde dissolution. Analytical techniques that extract and analyze the complete contents of fluid inclusions at room temperature can account for the predicted precipitation of microscopic daughter minerals during cooling, but may not compensate for chemical changes caused by the retrograde dissolution of calcite. Such solubility effects are another reason to be cautious in using carbonate minerals for fluid inclusion studies, in addition to their undesirable physical properties of softness, deformability and perfect cleavage. [source] Practical considerations in development of solid dosage forms that contain cyclodextrinJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 7 2007Lee A. Miller Abstract The following is a review of the literature that addresses the use of cyclodextrin in solid dosage forms. Care was taken to exclude physical and chemical characteristics of cyclodextrin, which have been discussed in the literature. A flow diagram is provided to outline the decision-making steps that are involved in the development process. Both preparation of physical mixtures and inclusion complexes are considered. Analytical techniques to determine the presence of inclusion complexes, the effect of other excipients on complex formation, the effect of size limitation of solid dosages forms, powder processing, and storage of solid dosage forms are discussed. © 2007 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 96: 1691,1707, 2007 [source] Long-term landscape evolution: linking tectonics and surface processesEARTH SURFACE PROCESSES AND LANDFORMS, Issue 3 2007Paul Bishop Abstract Research in landscape evolution over millions to tens of millions of years slowed considerably in the mid-20th century, when Davisian and other approaches to geomorphology were replaced by functional, morphometric and ultimately process-based approaches. Hack's scheme of dynamic equilibrium in landscape evolution was perhaps the major theoretical contribution to long-term landscape evolution between the 1950s and about 1990, but it essentially ,looked back' to Davis for its springboard to a viewpoint contrary to that of Davis, as did less widely known schemes, such as Crickmay's hypothesis of unequal activity. Since about 1990, the field of long-term landscape evolution has blossomed again, stimulated by the plate tectonics revolution and its re-forging of the link between tectonics and topography, and by the development of numerical models that explore the links between tectonic processes and surface processes. This numerical modelling of landscape evolution has been built around formulation of bedrock river processes and slope processes, and has mostly focused on high-elevation passive continental margins and convergent zones; these models now routinely include flexural and denudational isostasy. Major breakthroughs in analytical and geochronological techniques have been of profound relevance to all of the above. Low-temperature thermochronology, and in particular apatite fission track analysis and (U,Th)/He analysis in apatite, have enabled rates of rock uplift and denudational exhumation from relatively shallow crustal depths (up to about 4 km) to be determined directly from, in effect, rock hand specimens. In a few situations, (U,Th)/He analysis has been used to determine the antiquity of major, long-wavelength topography. Cosmogenic isotope analysis has enabled the determination of the ,ages' of bedrock and sedimentary surfaces, and/or the rates of denudation of these surfaces. These latter advances represent in some ways a ,holy grail' in geomorphology in that they enable determination of ,dates and rates' of geomorphological processes directly from rock surfaces. The increasing availability of analytical techniques such as cosmogenic isotope analysis should mean that much larger data sets become possible and lead to more sophisticated analyses, such as probability density functions (PDFs) of cosmogenic ages and even of cosmogenic isotope concentrations (CICs). PDFs of isotope concentrations must be a function of catchment area geomorphology (including tectonics) and it is at least theoretically possible to infer aspects of source area geomorphology and geomorphological processes from PDFs of CICs in sediments (,detrital CICs'). Thus it may be possible to use PDFs of detrital CICs in basin sediments as a tool to infer aspects of the sediments' source area geomorphology and tectonics, complementing the standard sedimentological textural and compositional approaches to such issues. One of the most stimulating of recent conceptual advances has followed the considerations of the relationships between tectonics, climate and surface processes and especially the recognition of the importance of denudational isostasy in driving rock uplift (i.e. in driving tectonics and crustal processes). Attention has been focused very directly on surface processes and on the ways in which they may ,drive' rock uplift and thus even influence sub-surface crustal conditions, such as pressure and temperature. Consequently, the broader geoscience communities are looking to geomorphologists to provide more detailed information on rates and processes of bedrock channel incision, as well as on catchment responses to such bedrock channel processes. More sophisticated numerical models of processes in bedrock channels and on their flanking hillslopes are required. In current numerical models of long-term evolution of hillslopes and interfluves, for example, the simple dependency on slope of both the fluvial and hillslope components of these models means that a Davisian-type of landscape evolution characterized by slope lowering is inevitably ,confirmed' by the models. In numerical modelling, the next advances will require better parameterized algorithms for hillslope processes, and more sophisticated formulations of bedrock channel incision processes, incorporating, for example, the effects of sediment shielding of the bed. Such increasing sophistication must be matched by careful assessment and testing of model outputs using pre-established criteria and tests. Confirmation by these more sophisticated Davisian-type numerical models of slope lowering under conditions of tectonic stability (no active rock uplift), and of constant slope angle and steady-state landscape under conditions of ongoing rock uplift, will indicate that the Davis and Hack models are not mutually exclusive. A Hack-type model (or a variant of it, incorporating slope adjustment to rock strength rather than to regolith strength) will apply to active settings where there is sufficient stream power and/or sediment flux for channels to incise at the rate of rock uplift. Post-orogenic settings of decreased (or zero) active rock uplift would be characterized by a Davisian scheme of declining slope angles and non-steady-state (or transient) landscapes. Such post-orogenic landscapes deserve much more attention than they have received of late, not least because the intriguing questions they pose about the preservation of ancient landscapes were hinted at in passing in the 1960s and have recently re-surfaced. As we begin to ask again some of the grand questions that lay at the heart of geomorphology in its earliest days, large-scale geomorphology is on the threshold of another ,golden' era to match that of the first half of the 20th century, when cyclical approaches underpinned virtually all geomorphological work. Copyright © 2007 John Wiley & Sons, Ltd. [source] THE NEW INSTITUTIONAL ECONOMICS , A DIFFERENT APPROACH TO ECONOMIC ANALYSISECONOMIC AFFAIRS, Issue 3 2008Eirik G. Furubotn The initial objective of the paper is to describe the way in which the term ,New Institutional Economics' (NIE) emerged in the literature and became the designation for a new field concerned with the study of various analytical techniques designed for the exploration of institutional phenomena. It is then shown how some of the more important of these techniques, transaction-cost economics, property-rights analysis and contract theory, have been applied in two central lines of neoinstitutional thought , the Williamsonian and the Northian. Criticisms of these two disparate theoretical positions on the NIE are considered and assessed. Next, a brief review of some of the empirical literature is undertaken so that the explanatory powers of NIE themes can be gauged. Finally, the paper offers a few general remarks on the present state of the NIE and its possible influence on the further development of economics. [source] Simultaneous Quantitative Determination of Cadmium, Lead, and Copper on Carbon-Ink Screen-Printed Electrodes by Differential Pulse Anodic Stripping Voltammetry and Partial Least Squares RegressionELECTROANALYSIS, Issue 23 2008Michael Cauchi Abstract Water is a vital commodity for every living entity on the planet. However, water resources are threatened by various sources of contamination from pesticides, hydrocarbons and heavy metals. This has resulted in the development of concepts and technologies to create a basis for provision of safe and high quality drinking water. This paper focuses on the simultaneous quantitative determination of three common contaminants, the heavy metals cadmium, lead and copper. Multivariate calibration was applied to voltammograms acquired on in-house printed carbon-ink screen-printed electrodes by the highly sensitive electrochemical method of differential pulse anodic stripping voltammetry (DPASV). The statistically inspired modification of partial least squares (SIMPLS) algorithm was employed to effect the multivariate calibration. The application of data pretreatment techniques involving range-scaling, mean-centering, weighting of variables and the effects of peak realignment are also investigated. It was found that peak realignment in conjunction with weighting and SIMPLS led to the better overall root mean square error of prediction (RMSEP) value. This work represents significant progress in the development of multivariate calibration tools in conjunction with analytical techniques for water quality determination. It is the first time that multivariate calibration has been performed on DPASV voltammograms acquired on carbon-ink screen-printed electrodes. [source] Targeting Chemical and Biological Warfare Agents at the Molecular LevelELECTROANALYSIS, Issue 14 2003Omowunmi Abstract After the September,11 tragedies of 2001, scientists and law-enforcement agencies have shown increasing concern that terrorist organizations and their "rogue" foreign government-backers may resort to the use of chemical and/or biological agents against U.S. military or civilian targets. In addition to the right mix of policies, including security measures, intelligence gathering and training for medical personnel on how to recognize symptoms of biochemical warfare agents, the major success in combating terrorism lies in how best to respond to an attack using reliable analytical sensors. The public and regulatory agencies expect sensing methodologies and devices for homeland security to be very reliable. Quality data can only be generated by using analytical sensors that are validated and proven to be under strict design criteria, development and manufacturing controls. Electrochemical devices are ideally suited for obtaining the desired analytical information in a faster, simpler, and cheaper manner compared to traditional (lab-based) assays and hence for meeting the requirements of decentralized biodefense applications. This articler presents a review of the major trends in monitoring technologies for chemical and biological warfare (CBW) agents. It focuses on research and development of sensors (particularly electrochemical ones), discusses how advances in molecular recognition might be used to design new multimission networked sensors (MULNETS) for homeland security. Decision flow-charts for choosing particular analytical techniques for CBW agents are presented. Finally, the paths to designing sensors to meet the needs of today's measurement criteria are analyzed. [source] Analysis of urinary metabolites for metabolomic study by pressurized CECELECTROPHORESIS, Issue 23 2007Guoxiang Xie Abstract A new approach for the metabolomic study of urinary samples using pressurized CEC (pCEC) with gradient elution is proposed as an alternative chromatographic separation tool with higher degree of resolution, selectivity, sensitivity, and efficiency. The pCEC separation of urinary samples was performed on a RP column packed with C18, 5,,m particles with an ACN/water mobile phase containing TFA. The effects of the acid modifiers, applied voltage, mobile phase, and detection wavelength were systematically evaluated using eight spiked standards, as well as urine samples. A typical analytical trial of urine samples from Sprague Dawley (S.D.) rats exposed to high-energy diet was carried out following sample pretreatment. Significant differences in urinary metabolic profiles were observed between the high energy diet-induced obesity rats and the healthy control rats at the 6th,wk postdose. Multivariate statistical analysis revealed the differential metabolites in response to the diet, which were partially validated with the putative standards. This work suggests that such a pCEC-based separation and analysis method may provide a new and cost-effective platform for metabolomic study uniquely positioned between the conventional chromatographic tools such as HPLC, and hyphenated analytical techniques such as LC-MS. [source] Impact of changes in analytical techniques for the measurement of polychlorinated biphenyls and organochlorine pesticides on temporal trends in herring gull eggsENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 7 2010Shane R. de Solla Abstract Changes in analytical approaches during the tenure of monitoring programs for organochlorine (OC) pesticides and polychlorinated biphenyls (PCBs) may affect estimates of temporal trends. We used an in-house reference material to create multiplication factors to adjust the estimates of OC pesticides and PCBs (Aroclor equivalents) in Great Lake herring gull eggs analyzed using electron capture detection (1987,1997) to be more equivalent to estimates using mass spectrometric detection (1998,2005) as well as accompanying differences in analytical procedures. We examined temporal trends in contaminant concentrations in herring gull eggs using change point regressions, to determine whether significant changes in long-term trends were associated with analytical methodology. The highest frequency of change point occurrences shifted from 1997 (when analytical methodology was altered) to 2003 after data adjustment. The explanatory power (r2) of the regressions was lower after adjustment, although only marginally so (mean r2 difference,=,0.04). The initial rates of decline before change points in contaminant concentrations were generally slower after the data adjustment, but after any change points the declines were not significantly different. The regression models did not change for 83.3% of the cases. The effects on the interpretation of long-term temporal trends in herring gull eggs, although not negligible, were minor relative to the magnitude of the temporal changes. Environ. Toxicol. Chem. 2010;29:1476,1483. © 2010 SETAC [source] Acute toxicity of heavy metals to acetate-utilizing mixed cultures of sulfate-reducing bacteria: EC100 and EC50ENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 12 2001Vivek P. Utgikar Abstract Acid mine drainage from abandoned mines and acid mine pit lakes is an important environmental concern and usually contains appreciable concentrations of heavy metals. Because sulfate-reducing bacteria (SRB) are involved in the treatment of acid mine drainage, knowledge of acute metal toxicity levels for SRB is essential for the proper functioning of the treatment system for acid mine drainage. Quantification of heavy metal toxicity to mixed cultures of SRB is complicated by the confounding effects of metal hydroxide and sulfide precipitation, biosorption, and complexation with the constituents of the reaction matrix. The objective of this paper was to demonstrate that measurements of dissolved metal concentrations could be used to determine the toxicity parameters for mixed cultures of sulfate-reducing bacteria. The effective concentration, 100% (EC100), the lowest initial dissolved metal concentrations at which no sulfate reduction is observed, and the effective concentration, 50% (EC50), the initial dissolved metal concentrations resulting in a 50% decrease in sulfate reduction, for copper and zinc were determined in the present study by means of nondestructive, rapid physical and chemical analytical techniques. The reaction medium used in the experiments was designed specifically (in terms of pH and chemical composition) to provide the nutrients necessary for the sulfidogenic activity of the SRB and to preclude chemical precipitation of the metals under investigation. The toxicity-mitigating effects of biosorption of dissolved metals were also quantified. Anaerobic Hungate tubes were set up (at least in triplicate) and monitored for sulfate-reduction activity. The onset of SRB activity was detected by the blackening of the reaction mixture because of formation of insoluble ferrous sulfide. The EC100 values were found to be 12 mg/L for copper and 20 mg/L for zinc. The dissolved metal concentration measurements were effective as the indicators of the effect of the heavy metals at concentrations below EC100. The 7-d EC50 values obtained from the difference between the dissolved metal concentrations for the control tubes (tubes not containing copper or zinc) and tubes containing metals were found to be 10.5 mg/L for copper and 16.5 mg/L for zinc. Measurements of the turbidity and pH, bacterial population estimations by means of a most-probable number technique, and metal recovery in the sulfide precipitate were found to have only a limited applicability in these determinations. [source] IgG2 containing IgM,IgG immune complexes predominate in normal human plasma, but not in plasma of patients with warm autoimmune haemolytic anaemiaEUROPEAN JOURNAL OF HAEMATOLOGY, Issue 3 2006Dorothea Stahl Abstract:, The different physicochemical and sterical properties of IgG subclasses may favour a selective enrichment of defined IgG subclasses in IgM,IgG immune complexes (IC) of human plasma under physiological conditions. Such enrichment of IgG subclasses in IgM,IgG IC of plasma may differ from the normal IgG subclass distribution in plasma itself, and contribute to the physiological functions of IgM,IgG IC. Systematic studies on the IgG subclass distribution in IgM,IgG IC in humans are lacking. Using specific analytical techniques to characterise IgM,IgG IC in human plasma (i.e. fast protein liquid chromatography, enzyme-linked immunosorbent assay, affinity biosensor technology), and taking warm autoimmune haemolytic anaemia (WAIHA) of humans as a disease model, we here demonstrate that: (i) IgG2 is the predominant IgG subclass in IgM,IgG IC under physiological conditions, (ii) the predominance of IgG2 within IgM,IgG IC may get lost in polyclonal IgG-mediated autoimmune disease and (iii) the IgG subclass distribution in IgM,IgG IC influences the interaction between IC and blood cells involved in antigen presentation. The data presented here therefore extend the physiological function of IgG2, which is the protective immune response towards carbohydrate antigens in bacterial infections, and suggest IgG2-dependent regulation of immune responses to self-immunoglobulin in humans. The disturbed IgG subclass distribution in IgM,IgG IC of patients with WAIHA might influence activity of self-reactive B cells involved in the pathophysiology of the disease. [source] Kharasch-Type Cyclizations of 2-Substituted Indole Derivatives Surprisingly Lead to SpiroindolesEUROPEAN JOURNAL OF ORGANIC CHEMISTRY, Issue 28 2010Sarah Van der Jeught Abstract Starting from 1H -indole-2-carboxylic acid, a series of spiro[2-oxoindole-pyrrolidines] could be synthesized in a straightforward manner. The key reaction is a Kharasch radical cyclization reaction of trichloroacetylated precursors. The identity of the tricyclic final products that were formed could be determined as spiro[2-oxoindole-pyrrolidines] by using a combination of different analytical techniques (1H NMR, 13C NMR, gHMBC, HRMS) and additional reactions. The produced skeletons are interesting from a medicinal point of view. [source] Application of Synchrotron Radiation Techniques for Model Validation of Advanced Structural Materials,ADVANCED ENGINEERING MATERIALS, Issue 6 2009Annick Froideval Abstract Synchrotron radiation techniques represent powerful tools to characterize materials down to the nanometer level. This paper presents a survey of the state-of-the-art synchrotron-based techniques which are particularly well-suited for investigating materials properties. Complementary X-ray absorption techniques such as extended X-ray absorption fine structure (EXAFS), X-ray magnetic circular dichroism (XMCD), photoemission electron microscopy (PEEM) are used to address the individual local atomic structure and magnetic moments in Fe,Cr model systems. The formation of atomic clusters/precipitates in such systems is also investigated by means of scanning transmission X-ray microscopy (STXM). Such advanced analytical techniques can not only offer valuable structural and magnetic information on such systems, they can also serve for validating computational calculations performed at different time and length scales which can help improve materials lifetime predictions. [source] Anomalous Oxidation States in Multilayers for Fuel Cell ApplicationsADVANCED FUNCTIONAL MATERIALS, Issue 16 2010James M. Perkins Abstract Significant recent interest has been directed towards the relationship between interfaces and reports of enhanced ionic conductivity. To gain a greater understanding of the effects of hetero-interfaces on ionic conductivity, advanced analytical techniques including electron microscopy (TEM/STEM), electron energy loss spectroscopy (EELS), and secondary ion mass spectrometry (SIMS) are used to characterize CeO2/Ce0.85Sm0.15O2 multilayer thin films grown by pulsed laser deposition. High quality growth is observed, but ionic conductivity measured by impedance spectroscopy and 18O tracer experiments is consistent with bulk materials. EELS analysis reveals the unusual situation of layers containing only Ce(IV) adjacent to layers containing both Ce(III) and Ce(IV). Post oxygen annealing induced oxygen diffusion and mixed oxidation states in both layers, but only in the vicinity of low angle grain boundaries perpendicular to the layers. The implications of the anomalous behavior of the Ce oxidation states on the design of novel electrolytes for solid oxide fuel cells is discussed. [source] Understanding pressures on fishery resources through trade statistics: a pilot study of four products in the Chinese dried seafood marketFISH AND FISHERIES, Issue 1 2004Shelley Clarke Abstract This study investigates the dried seafood trade, centred in Chinese markets, in order to better understand the pressures its demand exerts on global marine resource stocks. Using Hong Kong, the region's largest entrepôt, as a focal point, the trade in shark fins, abalone, bêche-de-mer and dried fish is characterized in terms of product history, volume, source fisheries and species composition. Trends identified in the Hong Kong market are interpreted in the context of the larger Chinese market. Shark fin imports grew 6% per year between 1991 and 2000, most likely because of market expansion in Mainland China, posing increasingly greater pressures on global shark resources. In contrast, the quantities of dried abalone traded through Hong Kong remained steady, but inferences based on this trend are discouraged by suggestions of increasing preferences for fresh product forms and growing domestic production in Mainland China. Hong Kong's imports of dried bêche-de-mer (sea cucumber) have decreased, while the percentage of imports re-exported has remained steady, suggesting that Hong Kong continues as an entrepôt for Mainland China despite declining domestic consumption. Few conclusions can be drawn regarding dried fish products, including whole fish and fish maws, because of a lack of product differentiation in customs data, but a market survey was conducted to provide information on species composition. Comparison of Hong Kong dried seafood trade statistics to those of other key trading partners indicates that, in general, Hong Kong's duty-free status appears to encourage more accurate reporting of traded quantities. Under-reporting biases ranged from 24 to 49% for shark fin and bêche-de-mer, respectively. Comparison to United Nations (UN) Food and Agriculture Organization (FAO) databases indicates additional under-reporting for shark fin such that an alternative minimum estimate of world trade is at least twice the FAO estimates in 1998,2000. The results of a survey of Hong Kong traders provide insight into their attitudes toward harvest, economic and regulatory factors, and suggest that conservation efforts are unlikely to emerge from, or be actively supported by, dried seafood trade organizations. The market's apparent sensitivity to economic sentiment, however, reveals an opportunity for consumer education to play a role in shaping future market growth and resource conservation. Recommendations are provided for improving trade statistics and for developing better analytical techniques to complement traditional methods for monitoring the exploitation and management of fisheries resources. [source] A renaissance in studies of ancient lifeGEOLOGY TODAY, Issue 4 2010J. William Schopf In the Origin of Species, published a century-and-a-half ago, Darwin was mystified by the lack of a ,pre-Cambrian' fossil record, the existence of which he regarded as pivotal to his theory of evolution. For the next 100 years, this ,missing' fossil record,unknown and thought unknowable'stood out as arguably the single greatest blemish to Darwin's theory. Beginning in the 1950s, the answer to Darwin's problem began to be unearthed, a Precambrian record of flourishing communities of microscopic organisms now known to extend to 3500 million years ago. During recent years, studies of such ancient microbes have markedly increased, spurred by an influx of new workers and, especially, by the introduction of new analytical techniques, three of which are featured here: confocal laser scanning microscopy, and Raman-spectral and fluorescence-spectral imagery. Used together, these techniques provide evidence of the three-dimensional form, cellular anatomy, and molecular structure of rock-embedded microscopic fossils and of the minerals in which they are entombed that is unavailable by any other means. [source] Neutron Activation Analysis, Atomic Absorption and X-Ray Fluorescence Spectrometry Review for 2006,2007GEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 4 2008L. Paul Bédard These mature analytical techniques do not show any change in publication level from the previous two years and AAS remains dominant in terms of the number of publications. The last two years have seen fewer technical improvements than in the previous review period. Some interesting papers dealing with uncertainty and quality assurance in INAA were published during 2006,2007. It is suggested that photon activation should be reconsidered because the source of electron accelerators has recently improved. A technique to preconcentrate Se for INAA determination has also been proposed. In the case of AAS, papers on analyte preconcentration continue to be more abundant than those relating to instrumental modification. Sample preparation for AAS is also active and ultrasound-assisted leaching shows some promising applications. There were an unusual number of reviews concerned with AAS and those important to geological samples are cited here. A technique to preconcentrate Cr in water is presented and a new device to determine As and Se is showing some potential uses. Confocal X-ray mapping continues to show interesting developments. One group developed a technique to perform XRF inside an oyster and an interesting application of ,-XRF mapping of sediments is presented. Determination of platinum-group elements (at ,g g1 concentrations) can be carried out very quickly with an improved XRF technique. [source] Comparison of Linear Regression Models for Quantitative Geochemical Analysis: An Example Using X-Ray Fluorescence SpectrometryGEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 3 2005Mirna Guevara calibration analytique; régression linéaire; matériaux de référence en géochimie; géochimie analytique; loi de propagation d'erreurs This paper presents statistical aspects related to the calibration process and a comparison of different regression approaches of relevance to almost all analytical techniques. The models for ordinary least-squares (OLS), weighted least-squares (WLS), and maximum likelihood fitting (MLF) were evaluated and, as a case study, X-ray fluorescence (XRF) calibration curves for major elements in geochemical reference materials were used. The results showed that WLS and MLF models were statistically more consistent in comparison with the usually applied OLS approach. The use of uncertainty on independent and dependent variables during the calibration process and the calculation of final uncertainty on individual results using error propagation equations are the novel aspects of our work. Cet article présente les aspects statistiques liés au processus de calibration et fait une comparaison des différents calculs de régression utilisés dans pratiquement toutes les techniques analytiques. Les modèles des moindres carrés ordinaires (MCO) et pondérés (MCP), et d'ajustement de maximum de vraisemblance (AMV) ont étéévalués et appliqués aux courbes de calibration d'éléments majeurs obtenues en analyse par fluorescence X (XRF) de matériaux certifiés de référence. Les résultats obtenus avec les modèles MCP et AMV sont plus cohérents statistiquement que ceux obtenus la méthode classique des MCO. L'utilisation de l'incertitudes sur des variables indépendantes ou dépendantes durant la procédure de calibration et le calcul de l'incertitude finale sur chaque résultat à partir des lois de propagation d'erreur sont des aspects novateurs de ce travail. [source] Neutron Activation Analysis, Atomic Absorption and X-Ray Fluorescence Spectrometry Review for 2003GEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 1 2005L. Paul Bédard This review for the year 2003 deals with three relatively well-established, mature, analytical techniques (neutron activation analysis, atomic absorption spectrometry and X-ray fluorescence spectrometry) that nevertheless remain very important for the characterisation of geological and environmental samples. Developments in neutron activation analysis included modification to the technique in relation to the determination of platinum-group elements, as well as consideration of sample size in ore grade estimation. A considerable body of literature was published on the application of atomic absorption spectrometry in the analysis of environmental samples. Many of these proposed technical and methodological improvements, notably in extraction procedures. X-ray fluorescence spectrometry saw developments in in situ analysis, synchrotron micro-XRF (,-SRXRF) and a confocal X-ray set-up for 3D elemental imaging. XRF technologies were used in the analysis of geological samples, reference materials, glasses, solutes and environmental materials. [source] Reference Minerals for the Microanalysis of Light ElementsGEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 2-3 2001M. Darby Dyar tourmaline; danburite; spodumène; muscovite; isotopes The quantitative determination of light element concentrations in geological specimens represents a major analytical challenge as the electron probe is generally not suited to this task. With the development of new in situ analytical techniques, and in particular the increasing use of secondary ion mass spectrometry, the routine determination of Li, Be and B contents has become a realistic goal. However, a major obstacle to the development of this research field is the critical dependence of SIMS on the availability of well characterized, homogeneous reference materials that are closely matched in matrix (composition and structure) to the sample being studied. Here we report the first results from a suite of large, gem crystals which cover a broad spectrum of minerals in which light elements are major constituents. We have characterized these materials using both in situ and wet chemical techniques. The samples described here are intended for distribution to geochemical laboratories active in the study of light elements. Further work is needed before reference values for these materials can be finalized, but the availability of this suite of materials represents a major step toward the routine analysis of the light element contents of geological specimens. La détermination quantitative des concentrations en éléments légers dans les échantillons géologiques représente un défi analytique majeur, la sonde électronique ne convenant généralement pas pour ce travail. Avec le développement de nouvelles techniques analytiques in situ, en particulier l'utilisation grandissante de la spectrométrie ionique secondaire, la détermination en routine des teneurs en Li, Be et B est devenue un objectif réaliste. Toutefois, un obstacle majeur dans le développement de cette recherche subsiste : la technique SIMS est dépendante de la disponibilité de matériaux de référence bien caractérisés et homogènes proches en composition et en structure de l'échantillon étudié. Nous rapportons ici les premiers résultats obtenus à partie d'un groupe de grands cristaux de qualité gemme recouvrant un large spectre de minéraux composés essentiellement d'éléments légers. Nous avons caractérisé ces matériaux en utilisant à la fois des techniques in situ et par voie humide. Les échantillons décrits ici vont être distribués dans les laboratoires de géochimie spécialisés dans l'étude des éléments légers. Avant la conclusion des valeurs de référence de ces matériaux, des travaux ultérieurs seront nécessaires, mais la disponibilité de l'ensemble de ces matériaux représente une étape importante vers l'analyse en routine des teneurs en éléments légers d'échantillons géologiques. [source] Molybdenum Concentrations Measured in Eleven USGS Geochemical Reference Materials by Isotope Dilution Thermal Ionisation Mass SpectrometryGEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 2 2000Michael E. Wieser molybdène; dilution isotopique; spectrométrie de masse à; thermo-ionisation; matériaux de référence USGS Molybdenum concentrations in eleven USGS geochemical reference materials AGV-1, BCR-1, BHVO-1, BIR-1, DNC-1, DTS-1, G-2, GSP-1, MAG-1, PCC-1 and W-2 were measured by isotope dilution thermal ionisation mass spectrometry (ID-TIMS). In every case but one, the concentrations determined in this study were significantly lower than the current consensus values. Molybdenum concentrations determined by ID-TIMS are inherently more accurate and precisions may be up to an order of magnitude higher than those measured by other analytical techniques. Les concentrations en molybdène de onze matériaux géochimiques de référence de l'USGS, AGV-1, BCR-1, BHVO-1, BIR-1, DNC-1, DTS-1, G-2, GSP-1, MAG-1, PCC-1 et W-2, ont été mesurées par dilution isotopique et spectrométrie de masse à thermo-ionisation (ID-TIMS). Dans tous les cas sauf un, les concentrations déterminées dans cette étude sont nettement inférieures aux valeurs généralement admises. Les concentrations en molybdène déterminées par ID-TIMS sont par définition plus exactes et leur précision analytique peut tre améliorée d'un ordre de grandeur par rapport à celle déterminée par d'autres techniques analytiques. [source] UV-vis-Induced Vitrification of a Molecular Crystal,ADVANCED FUNCTIONAL MATERIALS, Issue 10 2007T. Naito Abstract A charge-transfer complex of 2,5-dimethyl- N,N,-dicyanoquinonediimine (DM) with silver (crystalline Ag(DM)2, defined as ,) is irreversibly transformed by UV-vis illumination. Depending on the illumination conditions, three new types of solids (defined as ,, ,, and ,) with different structural and physical properties are obtained and examined by a variety of analytical techniques, including solid-state, high-resolution, cross-polarization magic angle spinning (CP-MAS) 13C,NMR, elemental analysis (EA), mass spectrometry (MS), X-ray absorption fine structure (XAFS), and powder X-ray diffraction (XRD). The CP-MAS, EA, MS, and XAFS results indicate that compound , is a glass state of Ag(DM)2. The transformation from crystalline (,) to amorphous (,) solid Ag(DM)2 is an irreversible exothermic glass transition (glass-transition temperature 155.2,°C; ,H,=,,126.8,kJ,mol,1), which implies that the glass form is thermodynamically more stable than the crystalline form. Compound , (Ag(DM)1.5) consists of silver nanoparticles (diameter (7,±,2),nm ) dispersed in a glassy matrix of neutral DM molecules. The N,CN,Ag coordination bonds of the , form are not maintained in the , form. Decomposition of , by intense illumination results in a white solid (,), identified as being composed of silver nanoparticles (diameter (60,±,10),nm). Physical and spectroscopic (XAFS) measurements, together with XRD analysis, indicate that the silver nanoparticles in both , and , are crystalline with lattice parameters similar to bulk silver; however, the magnetic susceptibilities differ from bulk silver. [source] Structure,Property,Function Relationships in Nanoscale Oxide Sensors: A Case Study Based on Zinc Oxide,ADVANCED FUNCTIONAL MATERIALS, Issue 8 2007S. Polarz Abstract Chemical sensing on oxide sensors is a complex phenomenon involving catalytic activity as well as electronic properties. Thus, the properties of oxide sensors are highly sensitive towards structural changes. Effects like surface area, grain size, and, in addition, the occurrence of defects give separate contributions to the current. Structure,property,function relationships can be elucidated using a combination of state-of-the-art analytical techniques. It is shown, that impurity atoms in the oxide lattice influence the performance of ZnO sensors more strongly than the other factors. [source] On the analytical solution of the Bejan-Khair equation arising in free convection in porous mediaHEAT TRANSFER - ASIAN RESEARCH (FORMERLY HEAT TRANSFER-JAPANESE RESEARCH), Issue 5 2010V.J. Bansod Abstract This paper revisits the fundamental problem of free convection heat and mass transfer over a heated vertical surface embedded in a porous medium using analytical techniques. An integral procedure is applied to the boundary layer similar equation for the combined heat and mass transfer from a vertical surface in a porous medium. The analytical approximations have covered a wide range of governing parameters of the problem. The results for both Nusselt and Sherwood numbers agree well with numerical results published in the literature. © 2010 Wiley Periodicals, Inc. Heat Trans Asian Res; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/htj.20297 [source] | |||||||||||||||||||||||||||||||||||||