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Investigated Samples (investigated + sample)
Selected AbstractsMatrix vapor deposition/recrystallization and dedicated spray preparation for high-resolution scanning microprobe matrix-assisted laser desorption/ionization imaging mass spectrometry (SMALDI-MS) of tissue and single cellsRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 3 2010Werner Bouschen Matrix preparation techniques such as air spraying or vapor deposition were investigated with respect to lateral migration, integration of analyte into matrix crystals and achievable lateral resolution for the purpose of high-resolution biological imaging. The accessible mass range was found to be beyond 5000 u with sufficient analytical sensitivity. Gas-assisted spraying methods (using oxygen-free gases) provide a good compromise between crystal integration of analyte and analyte migration within the sample. Controlling preparational parameters with this method, however, is difficult. Separation of the preparation procedure into two steps, instead, leads to an improved control of migration and incorporation. The first step is a dry vapor deposition of matrix onto the investigated sample. In a second step, incorporation of analyte into the matrix crystal is enhanced by a controlled recrystallization of matrix in a saturated water atmosphere. With this latter method an effective analytical resolution of 2,µm in the x and y direction was achieved for scanning microprobe matrix-assisted laser desorption/ionization imaging mass spectrometry (SMALDI-MS). Cultured A-498 cells of human renal carcinoma were successfully investigated by high-resolution MALDI imaging using the new preparation techniques. Copyright © 2010 John Wiley & Sons, Ltd. [source] CE assay for simultaneous determination of charged and neutral impurities in dexamphetamine sulfate using a dual CD systemELECTROPHORESIS, Issue 9 2010Sudaporn Wongwan Abstract A CE assay for the simultaneous determination of charged and uncharged potential impurities (1S,2S -(+)-norpseudoephedrine, 1R,2S -(,)-norephedrine, phenylacetone and phenylacetone oxime) of dexamphetamine sulfate including the stereoisomer levoamphetamine was developed and validated. The optimized background electrolyte consisted of a 50,mM sodium phosphate buffer, pH 3.0, containing 80,mg/mL sulfobutylether-,-CD and 25,mg/mL sulfated ,-CD. Separations were performed in 40.2/35,cm, 50 ,m id fused-silica capillaries at a temperature of 20°C and an applied voltage of ,10,kV. 1R,2S -(,)-ephedrine was used as internal standard. The assay was validated in the range of 0.05,1.0% for the related substances and in the range of 0.05,5.0% for levoamphetamine. The LOD was 0.01,0.02% depending on the analyte. The assay also allowed the separation of the E,Z-stereoisomers of phenylacetone oxime. The effect of the degree of substitution of sulfobutylether-,-CD was investigated. In commercial samples of dexamphetamine sulfate between 3.2 and 3.7% of levoamphetamine were found. Furthermore, phenylacetone and phenylacetone oxime could be observed at the LOD, indicating the synthetic origin of the investigated samples. [source] Influence of filling fat type on praline products with nougat fillingEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 12 2007Biljana Pajin Abstract The aim of this research was to examine the composition and functional characteristics of three samples of commercial filling fat intended for the making of nougat fillings for confectionary products. The crystallization rate of the fats was measured under static conditions using the NMR technique and under dynamic conditions as well as using a rotational rheometer. The functional characteristics of the fats were estimated by means of sensory values of the prepared praline product. Under the static conditions, all investigated filling fats showed a fast crystallization rate (,2,4%/min). The sample with the highest lauric acid contents started to crystallize immediately (no induction period). The longest induction period was found for the sample with the lowest saturated fatty acid and trans fatty acid contents. During the crystallization under dynamic conditions, all investigated samples started to crystallize more rapidly (rapid viscosity increase) at practically the same temperature (,17,°C). Measuring solid fat content and viscosity are two approaches of determining the suitability of a filling fat to be used in pralines. Both measurements provide valuable information, and particularly viscosity build-up is very important from the view of production on factory scale. [source] Synthesis, Structure and Electrical Properties of Mo-doped CeO2,Materials for SOFCsFUEL CELLS, Issue 5 2009Q. Li Abstract In this paper, we report the synthesis, structure and electrical conductivity of Mo-doped compounds with a nominal chemical formula of Ce1,xMoxO2+, (x,=,0.05, 0.07, 0.1) (CMO). The formation of fluorite-like structure with a small amount of Ce8Mo12O49 impurity (JCPDS Card No. 31-0330) was confirmed using a powder X-ray diffraction (PXRD). The fluoride-type structure was retained under wet H2 and CH4 atmospheres at 700 and 800,°C, while diffraction peaks due to metal Mo were observed in dry H2 under the same condition. AC impedance measurements showed that the total conductivity increases with increasing Mo content in CMO, and among the investigated samples, Ce0.9Mo0.1O2+, exhibited the highest electrical conductivity with a value of 2.8,×,10,4 and 5.08,×,10,2 S cm,1 at 550,°C in air and wet H2, respectively. The electrical conductivity was found to be nearly the same, especially at high temperatures, in air, O2 and N2. Chemical compatibility of Ce0.9Mo0.1O2+, with 10,mol-% Y2O3 stabilised ZrO2 (YSZ) and Ce0.9Gd0.1O1.95 (CGO) oxide ion electrolytes in wet H2 was evaluated at 800,1,000,°C, using PXRD and EDX analyses. PXRD showed that CMO was found to react with YSZ electrolyte at 1,000,°C. The area specific polarisation resistance (ASPR) of Ce0.9Mo0.1O2+, on YSZ was found to be 8.58,ohm,cm2 at 800,°C in wet H2. [source] Organic geochemistry indicates Gebel El Zeit, Gulf of Suez, is a source of bitumen used in some Egyptian mummiesGEOARCHAEOLOGY: AN INTERNATIONAL JOURNAL, Issue 3 2005A.O. Barakat Molecular geochemical properties of crude oils and surface petroleum seeps from the southern part of the Gulf of Suez were evaluated. The characterizations of individual aliphatic, aromatic, and biomarker compounds were based on gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS) analyses. The results provided strong evidence for a close genetic association of these samples. The geochemical characteristics suggest an origin from Tertiary source rocks deposited in a normal marine environment that received continental runoff. The molecular signatures of the investigated samples were very similar to those of the Lower Miocene Rudeis Formation source rock in the southern Gulf of Suez. Further, biomarker fingerprints of the investigated oil seeps were compared with those of the Dead Sea asphalt, as well as the bitumen from some Egyptian mummies reported in the literature. The results demonstrate that oil seeps from the southern end of Gebel El Zeit were used by ancient Egyptians for embalming. © 2005 Wiley Periodicals, Inc. [source] Electrical and thermal properties of nylon 6/calcium carbonate compositesADVANCES IN POLYMER TECHNOLOGY, Issue 4 2009M. A. Moussa Abstract Several polymer composites formed from nylon 6/CaCO3 with different ratios and particle sizes were prepared using modified and unmodified CaCO3 as inorganic filler. The modification of CaCO3 surfaces was carried out by adsorption of oleic acid from toluene. TGA and DSC measurements show that the glass transition temperatures reduced by the presence of inorganic filler, whereas the melting temperature did not influenced. In all prepared polymer composites, the presence of filler accelerates the degradation process of the polymer. Dielectric properties of the investigated samples were studied in the frequency range from 45 Hz to 1 MHz and at temperatures ranging between 50 and 200°C. The presence of CaCO3 led to a remarkable decrease in the conductivity of nylon 6. © 2010 Wiley Periodicals, Inc. Adv Polym Techn 28:257,266, 2009; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/adv.20165 [source] Reaction-induced nucleation and growth v. grain coarsening in contact metamorphic, impure carbonatesJOURNAL OF METAMORPHIC GEOLOGY, Issue 8 2010A. BERGER Abstract The understanding of the evolution of microstructures in a metamorphic rock requires insights into the nucleation and growth history of individual grains, as well as the coarsening processes of the entire aggregate. These two processes are compared in impure carbonates from the contact metamorphic aureole of the Adamello pluton (N-Italy). As a function of increasing distance from the pluton contact, the investigated samples have peak metamorphic temperatures ranging from the stability field of diopside/tremolite down to diagenetic conditions. All samples consist of calcite as the dominant matrix phase, but additionally contain variable amounts of other minerals, the so-called second phases. These second phases are mostly silicate minerals and can be described in a KCMASHC system (K2O, CaO, MgO, Al2O3, SiO2, H2O, CO2), but with variable K/Mg ratios. The modelled and observed metamorphic evolution of these samples are combined with the quantification of the microstructures, i.e. mean grain sizes and crystal size distributions. Growth of the matrix phase and second phases strongly depends on each other owing to coupled grain coarsening. The matrix phase is controlled by the interparticle distances between the second phases, while the second phases need the matrix grain boundary network for mass transfer processes during both grain coarsening and mineral reactions. Interestingly, similar final mean grain sizes of primary second phase and second phases newly formed by nucleation are observed, although the latter formed later but at higher temperatures. Moreover, different kinetic processes, attributed to different driving forces for growth of the newly nucleated grains in comparison with coarsening processes of the pre-existing phases, must have been involved. Chemically induced driving forces of grain growth during reactions are orders of magnitudes larger compared to surface energy, allowing new reaction products subjected to fast growth rates to attain similar grain sizes as phases which underwent long-term grain coarsening. In contrast, observed variations in grain size of the same mineral in samples with a similar T,t history indicate that transport properties depend not only on the growth and coarsening kinetics of the second phases but also on the microstructure of the dominant matrix phase during coupled grain coarsening. Resulting microstructural phenomena such as overgrowth and therefore preservation of former stable minerals by the matrix phase may provide new constraints on the temporal variation of microstructures and provide a unique source for the interpretation of the evolution of metamorphic microstructures. [source] Micro-structural characterization of red decorations of red and green color porcelain (Honglvcai) in ChinaJOURNAL OF RAMAN SPECTROSCOPY, Issue 8 2009Lihua Wang Abstract Red and green color porcelain (Honglvcai) is an important type of polychrome porcelains invented in North China during Song and Jin Dynasties. One of its great successes is its red decoration painted on the surface of glaze and fired at low temperature. Raman spectroscopy and X-ray absorption fine structure (XAFS) at Fe K-edge, were used to characterize the microstructure of red decorations from Song and Jin Dynasties to Ming Dynasty. The analyzing results on eight samples showed that hematite (,-Fe2O3) was the main chromogenic substance in red decorations from different dynasties, which indicated a similar technological skill among the investigated samples. The oxidation state of iron in red decorations was determined to be mainly trivalent, indicating that red decorations were fired under oxidizing atmosphere. Besides, it was found that the hematite (,-Fe2O3) in red decorations had a distorted structure, which was presumed to be an important factor influencing the color of red decorations. Copyright © 2009 John Wiley & Sons, Ltd. [source] Fields of deformation anisotropy exploration in multilayered (In,Ga)As/GaAs structures by high-resolution X-ray scatteringPHYSICA STATUS SOLIDI (A) APPLICATIONS AND MATERIALS SCIENCE, Issue 1 2006O. Yefanov Abstract The results of investigation of In0.3Ga0.7As/GaAs superlattice by high-resolution X-ray scattering are presented. The influence of lattice distortion on diffraction curves (DC) were analyzed with dynamical diffraction theory. It allowed to explain azimuth dependence of experimental diffraction curves. Anisotropic changes in the shape of InGaAs lattice unit cell were shown and measured. The influence of smooth borders between hetero-layers were analyzed. Comparative analysis of different gradient functions on the hetero-border influence on diffraction curves was done. Parameters of heterojunction in investigated samples were determined with the help of DC modelling. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Electrical transport phenomena in magnesium-doped p-type GaNPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 3 2009Leszek Konczewicz Abstract In this paper we present the resistivity and Hall-effect measurements on p-type GaN doped with Mg. The experiments were carried out as a function of hydrostatic pressure up to 1200 MPa in the temperature range 260,400 K. Both bulk GaN crystals as well as GaN:Mg epilayers were studied. In the investigated samples the decrease of resistivity and increase of hole concentration under pressure was observed. Such a behavior, which is contrary to the n-type material, strongly suggests a decrease of the ionization energy of Mg acceptor (Ea = 183 meV) with pressure. This shift is very weak, less than ,2 meV/GPa. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Neutron powder diffraction study of the anion-deficient La0.70Sr0.30MnO3.00-, manganitesPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 5 2009S. V. Trukhanov Abstract Using powder neutron diffraction method the magnetic structure of the anion-deficient La0.70Sr0.30MnO3.00-, (, = 0, 0.15; 0.20) solid solutions at different temperatures has been defined. It is established that the magnetic structure changes with oxygen vacancies concentration. For the investigated samples the structural phase transitions have not been detected. The obtained data confirm the conception of the magnetic phase state forming for the Sr-doped anion-deficient manganites. In according to this conception in case of orbital ordering absence the lowering of the coordination of the magnetic ion results to change of the indirect superexchange interactions Mn3+ -O-Mn3+ sign from positive to negative. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Advanced buffers for AlGaN/GaN HEMT and InGaN/GaN MQW on silicon substratesPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 6 2006Y. Dikme Abstract GaN growth was carried out on silicon (Si) substrates by metalorganic vapor phase epitaxy (MOVPE). A layer structure starting with HT (high-temperature) AlN and containing AlGaN and GaN as interlayers was employed for the subsequent deposition of GaN buffer layers. At first, the influence of the in-situ Al pre-deposition at the process start with different durations was investigated. Each time, the pre-deposition was followed by the same layer sequence and with thin AlGaN and GaN grown on top to form a high electron mobility transistor (HEMT). A significant enhancement could be observed in the properties of the investigated samples by reducing the pre-deposition time from 8 s to 2 s. Based on these results, multiple quantum well structures (MQW) and HEMT were grown on these buffers. For the MQW, the well thickness was increased and a shift to higher wavelengths was observed. The HEMT structures have shown enhanced properties by optimizing the growth temperatures of the top AlGaN layer. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] HgTe segregation process in HgCdTe studied by E1 reflectance peak positionsPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 4 2006M. Pociask Abstract Long term diffusion processes near the Cd1,xHgxTe surface influences the electronic structure as is shown in this paper. Measurements of reflectivity and surface characterisation by means of scanning electron microscopy (SEM) were performed for samples with x = 0.4 and x = 0.62. The optical results were compared with the reflectivity spectra obtained 22 years ago using the same samples. We discuss the observed dramatic changes in the optical changes upon the SEM and comparative analysis. E1 + , reflectance peak position corresponds to binary HgTe in both recently investigated samples. That method reflection is sensitive to no more than 120 µm the upper depth of investigated samples. The measurements of the E1 reflectance peak has proven to be a helpful and convenient tool for mercury telluride segregation near the HgCdTe surface and may be used to determine composition and age of HgCdTe. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Effects of Cyclic Hydrostatic Pressure on the Metabolism of Human Osteoarthritic Chondrocytes Cultivated in a Collagen GelARTIFICIAL ORGANS, Issue 2 2007Karsten Gavénis Abstract:, Among other parameters, the application of mechanical force may provide an important stimulus in modulating the structure and function of tissue-engineered articular cartilage. We developed a cultivation chamber in which six collagen type-I gel samples, seeded with human osteoarthritic chondrocytes, can be cultivated simultaneously. A cyclic hydrostatic pressure of up to 40 kPa with a frequency of 0.0125 Hz was applied, and cultivation was performed for 1, 4, 7, or 14 days. Histological examinations revealed a spheroidal cell morphology in the treatment group. In contrast, control samples of the same patients represented a more fibroblastic appearance. Collagen type-II (col-II) protein was found in the very pericellular region of all investigated samples; the col-II content did not obviously vary between the control and treatment groups. In the treatment group, col-II and aggrecan gene expression were elevated. A spectrophotometric quantification of proteoglycan concentrations in media supernatants revealed a statistically significant enhancement in the treatment group. [source] Electrical transport properties of aliovalent cation-doped CeO2ASIA-PACIFIC JOURNAL OF CHEMICAL ENGINEERING, Issue 1 2009Mark C. Pearce Abstract We report the comparative electrical properties of monovalent (Na+), divalent (Ca2+, Sr2+), trivalent (In3+, La3+) and coupled substitution of divalent and trivalent (Ca2+ + Sm3+) cation-doped CeO2. The investigated samples were prepared by solid-state reaction (ceramic) using the corresponding metal oxides and salts in the temperature range 1000,1600 °C in air. Powder X-ray diffraction (PXRD), laser particle size analysis (LPSA), scanning electron microscopy (SEM), and ac impedance spectroscopy measurements were employed for structural, morphology, and electrical characterization. PXRD studies reveal the formation of single-phase cubic fluorite-type structures for all investigated samples except those doped with In3+. The variation of lattice parameters is consistent with ionic radii (IR) of the dopant metal ions, with the exception of Na+ -doped CeO2. Our attempt to substitute In3+ for Ce4+ in CeO2 using both ceramic and wet chemical methods was unsuccessful. Furthermore, diffraction peaks attributed to CeO2 and In2O3 were observed up to sintering conditions of 1600 °C. Among the single-phase compounds investigated, Ce0.85Ca0.05Sm0.1O1.9 exhibits the highest bulk conductivity of 1.3 × 10,3 S/cm at 500 °C with activation energy of 0.64 eV in air. The electrical conductivity data obtained for Ce0.85Ca0.05Sm0.1O1.9 in air and Ar were found to be very similar over the investigated temperature range, indicating the absence of p-electronic conduction in the high oxygen partial pressure (pO2) range which is consistent with literature reported on Sm-doped CeO2. Copyright © 2008 Curtin University of Technology and John Wiley & Sons, Ltd. [source] Development of the second-order derivative UV spectrophotometric method for direct determination of paracetamol in urine intended for biopharmaceutical characterisation of drug productsBIOPHARMACEUTICS AND DRUG DISPOSITION, Issue 7 2003Jelena Paroj Abstract Paracetamol is a widely used nonsalicylate analgesic and antipyretic drug. The existing methods for the determination of paracetamol in biological fluids are mainly HPLC techniques, although there are some reported methods based on spectrophotometric determinations. However, all these methods involve some extraction or derivatisation procedures. In the present study the UV spectra of investigated samples were recorded over the wavelength range 220,400 nm (, step 0.21 nm; scan speed 60 nm/min) and second-order derivative spectra were calculated. Second-order derivative spectra of different blank urine samples displayed the presence of a zero-crossing point at 245,247 nm defined as ,zc. The zero-order absorption spectra of paracetamol in water displays maximum absorbance at 243 nm, while in second derivative spectra, a minimum peak at 246 nm was observed. Therefore, the application of zero-crossing technique to the second-derivative UV absorption spectrum should be useful for the determination of paracetamol using 2D,zc. The proposed method enables determination of total paracetamol in urine directly and simply by reading the 2D,zc of the diluted samples. The obtained results were in good accordance with published data on cumulative urinary excretion after per oral administration of paracetamol obtained applying different spectrophotometric methods of determination. It could be useful for biopharmaceutical characterisation of drug products (monitoring of the levels of paracetamol in urine in bioavailability testing, for the evaluation of in vitro,in vivo correlation and screening of different formulations during drug product development). Copyright © 2003 John Wiley & Sons, Ltd. [source] High sensitivity of free lambda and free kappa light chains for detection of intrathecal immunoglobulin synthesis in cerebrospinal fluidACTA NEUROLOGICA SCANDINAVICA, Issue 1 2009B. Arneth Background,,, So far, an inflammation of the central nervous system (CNS) is diagnosed by immunoglobulin measurement in cerebrospinal fluid (CSF) and serum as well as by determination of the oligoclonal bands. With the free kappa and lambda light chains, new markers to diagnose intrathecal synthesis are available. Methods,,, In addition to routine diagnostic tests and the assessment of standard parameters, free immunoglobulin light chains were measured in the CSF of patients with neurological disorders. Results,,, A significant agreement was found between an increase in free kappa light chain CSF serum quotients and results of the currently widely applied method of oligoclonal band measurement for the detection of intrathecal immunoglobulin synthesis. A sensitivity of 95% and 100% specificity for free kappa light chain concentrations at a cut-off of 0.41 mg/l was determined for free kappa light chains compared with oligoclonal bands. However, the free lambda light chains in 20 out of the 110 investigated samples were characterized by inconsistent behaviour. These otherwise unremarkable samples yielded increased CSF quotients, leading to the assumption that free lambda light chains represent a highly sensitive measure of intrathecal immunologlobulin synthesis. Thirteen of the 20 samples described above were obtained from patients with cerebral infarction, 4 samples derived from patients with cerebral paresis (primarily facial paresis), one sample was from a patient with multisystem atrophy and two were obtained from patients with migraine and neuralgia. Conclusion,,, These findings suggest that the high sensitivity of lambda light chains for the detection intrathecal immunoglobulin synthesis may be of benefit in establishing clinical diagnoses. [source] Science in Drug Control: The Alkaloid Content of Afghan OpiumCHEMISTRY & BIODIVERSITY, Issue 9 2008Barbara Remberg Abstract Opium samples from Afghanistan were analyzed by HPLC for their content of morphine and three further alkaloids (codeine, thebaine, and papaverine). To our knowledge, this is the largest set of authentic opium samples analyzed in one study until now. The purpose was to assess possible correlations between samples and selected external factors, such as region of origin within Afghanistan, year of harvest, or intra-batch variation. In the investigated samples, a trend towards higher morphine concentrations in opium from the North-Eastern parts of Afghanistan was observed in the period from 2003 to 2005. More than 75% of the samples contained above 10% of morphine, the overall average was 14.4%. [source] | ||||||||||||||||||||||