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PubMed2004

Combinatorial solid-state chemistry of inorganic materials.

Throughout history, scientists and engineers have relied on the slow and serendipitous trial-and-error process for discovering and developing new materials. In contrast, an emerging theme in modern materials science is the notion of intelligent design of materials. Pioneered by the pharmaceutical industry and adapted for the purposes of materials science and engineering, the combinatorial approach represents a watershed in the process of accelerated discovery, development and optimization of materials. To survey large compositional landscapes rapidly, thousands of compositionally varying samples may be synthesized, processed and screened in a single experiment. Recent developments have been aided by innovative rapid characterization tools, and by advanced materials synthesis techniques such as laser molecular beam epitaxy which can be used to perform parallel-processed design and control of materials down to the atomic scale. Here we review the fast-growing field of combinatorial materials science, with an emphasis on inorganic functional materials.

Journal Article↗

PubMed1997

Long-lifetime metal-ligand pH probe.

We describe the synthesis and fluorescence spectral characterization of a pH-sensitive metal-ligand complex, [Ru(deabpy)(bpy)2]2., where deabpy is 4,4'-diethylaminomethyl-2,2'-bipyridine. This metal-ligand complex (MLC) was found to display pH-dependent intensities, emission spectra, and decay times, with the changes centered near the physiological useful pH value of 7.5. The apparent pKa values were not found to be dependent on ionic strength. The compound was found to be useful for lifetime-based sensing by phase-modulation fluorometry. Global analysis of the intensity decays over a range of pH values revealed two decay times of 235 and 380 ns, associated with the protonated and unprotonated forms, respectively. Because of its long decay time, optical pH measurements could be accomplished by phase-modulation fluorometry with a conveniently low modulation frequency of 700 kHz. The lifetime data were obtained with either a amplitude-modulated laser or with an amplitude-modulated blue-light-emitting diode. This pH-sensitive complex also displays a modest spectral shift with change in pH, allowing its use as a wavelength-ratiometric MLC probe. One can imagine lifetime sensors for a variety of blood cations and point-of-care assays based on long-lifetime metal-ligand complexes and simple solid-state light sources and detectors.

2,2'-Dipyridyl↗

PubMed2005

Radon track imaging in CR-39 plastic detectors using confocal scanning laser microscopy.

Confocal scanning laser microscopy (CSLM) has been used to provide the first images of radon track populations in two external CR-39 plastic detectors. Measurements of variables including track area distribution and estimates of the angle of track inclination (dip) derived from surface CSLM sections are presented. CSLM depth slices, combined with three-dimensional (3D) visualization techniques, provide a new, non-destructive way of examining the 2D and 3D geometry of the etched tracks within solid-state nuclear track detectors that may prove useful in complementing existing optical microscopy methods.

Journal Article↗

PubMed2003

The birth of a quasiparticle in silicon observed in time-frequency space.

The concept of quasiparticles in solid-state physics is an extremely powerful tool for describing complex many-body phenomena in terms of single-particle excitations. Introducing a simple particle, such as an electron, hole or phonon, deforms a many-body system through its interactions with other particles. In this way, the added particle is 'dressed' or 'renormalized' by a self-energy cloud that describes the response of the many-body system, so forming a new entity--the quasiparticle. Using ultrafast laser techniques, it is possible to impulsively generate bare particles and observe their subsequent dressing by the many-body interactions (that is, quasiparticle formation) on the time and energy scales governed by the Heisenberg uncertainty principle. Here we describe the coherent response of silicon to excitation with a 10-femtosecond (10(-14) s) laser pulse. The optical pulse interacts with the sample by way of the complex second-order nonlinear susceptibility to generate a force on the lattice driving coherent phonon excitation. Transforming the transient reflectivity signal into frequency-time space reveals interference effects leading to the coherent phonon generation and subsequent dressing of the phonon by electron-hole pair excitations.

Journal Article↗

PubMed2003

Expression and characterization of the FXYD ion transport regulators for NMR structural studies in lipid micelles and lipid bilayers.

The proteins PLM (phospholemman), CHIF (channel inducing factor), and Mat8 (mammary tumor protein 8 kDa) are members of the FXYD family of ion transport regulatory membrane proteins. Here we describe their cloning and expression in Escherichia coli, and their purification for NMR structural studies in lipid micelles and lipid bilayers. The molecular masses of the purified recombinant FXYD proteins, determined from SDS-PAGE and from MALDI TOF mass spectrometry, reflect monomeric species. The solution NMR and CD spectra in SDS micelles show that they adopt helical conformations. The solid-state NMR spectra in lipid bilayers give the first view of their transmembrane architecture.

Amino Acid Sequence↗

PubMedDate not supplied

A new method for characterizing beta-ray ophthalmic applicator sources.

A technique is described which enables one to obtain detailed dose characteristics of 90Sr beta-ray ophthalmic applicators. A radiochromic radiation detector which is a solid-state solution of hexahydroxyethyl pararosaniline cyanide in a nylon polymer (i.e., thin foil), has been used to determine the surface dose rate and dose distribution of these sources. The detectors are rugged, easily handled, have an equivalent response (optical density per unit absorbed dose) to photons and electrons, and produce high-resolution images. They have been found useful for this application due to the high surface dose rates [0.10-1.0 Gy (H2O)/s] and their low sensitivity (approximately 10(4) Gy for an optical density of 1.0). The foils have been evaluated on a He-Ne scanning laser densitometer with a resolution of 0.3 mum. Comparison with NIST (formerly NBS) extrapolation ionization chamber measurements indicates surface dose-rate agreement within 6%. Spectral dosimetric characteristics are presented and discussed.

Beta Particles↗

PubMed1989

Transition dipole orientations in the early photolysis intermediates of rhodopsin.

The linear dichroism spectrum of rhodopsin in sonicated bovine disk membranes was measured 30, 60, 170, and 600 ns after room temperature photolysis with a linearly polarized, 7-ns laser pulse (lambda = 355 or 477 nm). A global exponential fitting procedure based on singular value decomposition was used to fit the linear dichroism data to two exponential processes which differed spectrally from one another and whose lifetimes were 42 +/- 7 ns and 225 +/- 40 ns. These results are interpreted in terms of a sequential model where bathorhodopsin (BATHO, lambda max = 543 nm) decays toward equilibrium with a blue shifted intermediate (BSI, lambda max = 478 nm). BSI then decays to lumirhodopsin (LUMI, lambda max = 492 nm). It has been suggested that two bathorhodopsins decay in parallel to their products. However, a Monte Carlo simulation of partial photolysis of solid-state visual pigment samples shows that one mechanism which creates populations of BATHO having different photolysis rates at 77 K may not be responsible for the two decay rates reported here at room temperature. The angle between the cis band and 498-nm band transition dipoles of rhodopsin is determined to be 38 degrees. The angles between both these transition dipoles and those of the long-wave-length bands of BATHO, BSI, and LUMI are also determined. It is shown that when BATHO is formed its transition dipole moves away from the original cis band transition dipole direction. The transition dipole then moves roughly twice as much towards the original cis band direction when BSI appears. Production of LUMI is associated with return of the transition dipole almost to the original orientation relative to the cis band, but with some displacement normal to the plane which contains the previous motions. The correlation between the lambda max of an intermediate and its transition dipole direction is discussed.

Animals↗

PubMed2001

Infrared and EPR Spectroscopic Studies of 2-C(2)H(2)F and 1-C(2)H(2)F Radicals Isolated in Solid Argon.

2-fluorovinyl radicals were generated in solid argon by solid-state chemical reactions of mobile F atoms with acetylene and its deuterated analogues. Highly resolved EPR spectra of the stabilized radicals CHF&dbond;(*)CH, CDF&dbond;(*)CD, CHF&dbond;(*)CD, and CDF&dbond;(*)CH were obtained for the first time. The observed spectra were assigned to cis-2-fluorovinyl radical based on excellent agreement between the measured (a(F) = 6.50, a(betaH) = 3.86, a(alphaH) = 0.25 mT) hyperfine constants and those calculated using density functional (B3LYP) theory. Analogous experiments carried out using infrared spectroscopy yielded a complete assignment of the vibrational frequencies. An unusual reversible photochemical conversion is observed in which cis-2-fluorovinyl radicals can be partially converted to 1-fluorovinyl radicals by pulsed laser photolysis at 532 nm. Photolysis at 355 nm converts 1-fluorovinyl back to cis-2-fluorovinyl. High-resolution EPR and infrared spectra of 1-fluorovinyl were obtained for the first time. The measured hyperfine constants (a(F) = 13.71, a(H1) = 4.21, a(H2) = 1.16 mT) are in good agreement with calculated values. Copyright 2001 Academic Press.

Journal Article↗

PubMed2003

How the confocal laser scanning microscope entered biological research.

A history of the early development of the confocal laser scanning microscope in the MRC Laboratory of Molecular Biology in Cambridge is presented. The rapid uptake of this technology is explained by the wide use of fluorescence in the 80s. The key innovations were the scanning of the light beam over the specimen rather than vice-versa and a high magnification at the level of the detector, allowing the use of a macroscopic iris. These were followed by an achromatic all-reflective relay system, a non-confocal transmission detector and novel software for control and basic image processing. This design was commercialized successfully and has been produced and developed over 17 years, surviving challenges from alternative technologies, including solid-state scanning systems. Lessons are pointed out from the unusual nature of the original funding and research environment. Attention is drawn to the slow adoption of the instrument in diagnostic medicine, despite promising applications.

Animals↗

PubMed1992

A new endoscope for ophthalmic microsurgery.

We present an endoscope designed for ophthalmic microsurgery. The handpiece contains a charge-coupled device, a solid-state imager (250,000 pixels), and a probe (either 0.89 or 1.5 mm in diameter), including the light guide. The light source is a halogen lamp. The clear views the instrument provides of the ciliary sulcus and ciliary body behind the iris make it useful in secondary posterior chamber intraocular lens implantation using the ciliary sulcus suturing technique, and in endolaser photocoagulation of the ciliary body in end-stage glaucoma. It also is useful in performing vitrectomy in cases in which visualization is difficult because of corneal opacification or fluid-gas exchange.

Cataract Extraction↗

PubMed2003

Synthesis, electronic properties, and applications of indium oxide nanowires.

Single-crystalline indium oxide nanowires were synthesized using a laser ablation method and characterized using various techniques. Precise control over the nanowire diameter down to 10 nm was achieved by using monodisperse gold clusters as the catalytic nanoparticles. In addition, field effect transistors with on/off ratios as high as 10(4) were fabricated based on these nanowires. Detailed electronic measurements confirmed that our nanowires were n-type semiconductors with thermal emission as the dominating transport mechanism, as revealed by temperature-dependent measurements. Furthermore, we studied the chemical sensing properties of our In(2)O(3) nanowire transistors at room temperature. Upon exposure to a small amount of NO(2) or NH(3), the nanowire transistors showed a decrease in conductance of up to five or six orders of magnitude, in addition to substantial shifts in the threshold gate voltage. Our devices exhibit significantly improved chemical sensing performance compared to existing solid-state sensors in many aspects, such as the sensitivity, the selectivity, the response time and the lowest detectable concentrations. We have also demonstrated the use of UV light as a "gas cleanser" for In(2)O(3) nanowire chemical sensors, leading to a recovery time as short as 80 seconds.

Crystallization↗

PubMed2003

Use of confocal microscopy to follow the development of penetrative hyphae during growth of Rhizopus oligosporus in an artificial solid-state fermentation system.

Two methods were compared for determining the concentration of penetrative biomass during growth of Rhizopus oligosporus on an artificial solid substrate consisting of an inert gel and starch as the sole source of carbon and energy. The first method was based on the use of a hand microtome to make sections of approximately 0.2- to 0.4-mm thickness parallel to the substrate surface and the determination of the glucosamine content in each slice. Use of glucosamine measurements to estimate biomass concentrations was shown to be problematic due to the large variations in glucosamine content with mycelial age. The second method was a novel method based on the use of confocal scanning laser microscopy to estimate the fractional volume occupied by the biomass. Although it is not simple to translate fractional volumes into dry weights of hyphae due to the lack of experimentally determined conversion factors, measurement of the fractional volumes in themselves is useful for characterizing fungal penetration into the substrate. Growth of penetrative biomass in the artificial model substrate showed two forms of growth with an indistinct mass in the region close to the substrate surface and a few hyphae penetrating perpendicularly to the surface in regions further away from the substrate surface. The biomass profiles against depth obtained from the confocal microscopy showed two linear regions on log-linear plots, which are possibly related to different oxygen availability at different depths within the substrate. Confocal microscopy has the potential to be a powerful tool in the investigation of fungal growth mechanisms in solid-state fermentation.

Biofilms↗

PubMed2003

Overexpression, purification, and characterization of recombinant Ca-ATPase regulators for high-resolution solution and solid-state NMR studies.

Phospholamban (PLB) and Sarcolipin (SLN) are integral membrane proteins that regulate muscle contractility via direct interaction with the Ca-ATPase in cardiac and skeletal muscle, respectively. The molecular details of these protein-protein interactions are as yet undetermined. Solution and solid-state NMR spectroscopies have proven to be effective tools for deciphering such regulatory mechanisms to a high degree of resolution; however, large quantities of pure recombinant protein are required for these studies. Thus, recombinant PLB and SLN production in Escherichia coli was optimized for use in NMR experiments. Fusions of PLB and SLN to maltose binding protein (MBP) were constructed and optimal conditions for protein expression and purification were screened. This facilitated the large-scale production of highly pure protein. To confirm their functionality, the biological activities of recombinant PLB and SLN were compared to those of their synthetic counterparts. The regulation of Ca-ATPase activity by recombinant PLB and SLN was indistinguishable from the regulation by synthetic proteins, demonstrating the functional integrity of the recombinant constructs and ensuring the biological relevance of our future structural studies. Finally, NMR spectroscopic conditions were established and optimized for use in investigations of the mechanism of Ca-ATPase regulation by PLB and SLN.

Amino Acid Sequence↗

PubMed2004

Single-crystal X-ray diffraction studies of photo-induced molecular species.

This tutorial review gathers together the recent developments in single-crystal X-ray diffraction that are starting to enable one to quantify directly the nature of light-induced electronic perturbations in chemical structures. Such structural information is key to understanding many photo-activated chemical processes and physical properties, and a description of the scientific impetus behind this incipient area of structural science, from academic and industrial perspectives, is given. Photoisomerism processes, solid-state photochemical reactions and spin-cross-over magnetic transitions, that have long-lived or irreversible light-induced states, are best understood by unravelling their three-dimensional structures measured in situ in their photo-converted state. A review of steady-state laser-induced single-crystal X-ray diffraction studies conducted, to date, and the experimental methodologies used in order to realise such structures, is presented. The structural characterisation of more transient photo-induced species (down to picosecond lifetimes) is paramount to a better understanding of the materials that undergo high-speed electronic switching, which make operative much of the electronics and optics industry, since there exists an inherent relationship between the excited-state structure and the physical properties exhibited. Prime examples include excited-state structures of molecular conductors and luminescent materials with potential applications as molecular wires, light-emitting diodes, non-linear optics, triboluminescence and electroluminescence. Previously, only indirect and qualitative interpretations of the nature of these excited-states could be formulated via spectroscopic techniques, but the developments in ms-ps time-resolved laser pump, X-ray probe single-crystal diffraction techniques, described herein, are overcoming this barrier, affording results that are entirely quantitative via a three-dimensional structural representation. In this regard, a review of structures of transient species studied to date is presented along with a discussion of the key experimental parameters that are required for a successful experiment, in terms of the X-ray, laser and sample characteristics. The importance of auxiliary spectroscopic work and complementary theoretical calculations is also briefly discussed. The paper concludes with a future outlook on new possible X-ray sources that will facilitate such work and extend it to structural studies on even more ephemeral species in the future.

Journal Article↗

PubMed2003

Molecular weight, tertiary structure, water binding and colon behaviour of ispaghula husk fibre.

Molecular variables, using aqueous and alkaline extracts, of the polysaccharide from ispaghula husk (IH) were examined using gel-permeation chromatography linked to multi-angle laser light scattering. Progressive extraction can yield a component with a molecular weight (MW)value up to about 7 x 106 Da, and gels, which accompany the extraction, have MW ranging from 10-20 x 106 Da. To mimic the polysaccharide degradation, particularly in the colon, the solid IH was degraded progressively using ionising radiation. A chain break occurs every 7.5 kGy in NaOH and every 15 kGy in water. The solid-state matrix is opened by the radiation to yield increased visco-elasticity of the aqueous extracts at critical radiation doses, before further degradation occurs after about 12 kGy. Differential scanning calorimetry is used to study the mechanism of interaction of water with IH. The first water to be taken up is non-freezing water and represents about twelve water molecules/disaccharide unit of the polysaccharide. As the water content is increased, the water becomes bound to the polysaccharide and freezes and melts at a temperature different from free water. This water is thermodynamically distinguishable from free water. It forms amorphous ice on cooling which crystallises exothermically and subsequently melts endothermically. Saturation occurs at a water content of 2-3 g water/g polymer, showing that about 60% of the water in the system is 'bound'. The most surprising conclusion is that despite the fact that the IH swells in water to form a solid and stiff gel, the greater part of that water in the gel is still free and behaves like liquid water.

Chromatography, Gel↗

PubMed2001

A nifedipine coground mixture with sodium deoxycholate. I. Colloidal particle formation and solid-state analysis.

Sodium deoxycholate (DCNa) is a bile salt that forms multimolecular inclusion compounds with a variety of organic substances. In this study, complex formulation of DCNa with nifedipine, a poorly water soluble drug, by grinding was investigated. The coground mixture was prepared with a vibration rod mill, and its solid state was characterized using powder X-ray diffraction, differential scanning calorimetry (DSC), and Fourier transform infrared (FTIR) spectroscopy. A laser diffraction particle size analyzer was also used to determine the particle size distribution curve in solution. When a nifedipine-DCNa (1:2 w/w) mixture coground for 30 min was dispersed into water and a pH 6.8 buffer solution, a semitransparent colloidal solution occurred immediately; 90% of the total particles formed in solution had a diameter less than 600 nm. Both powder X-ray diffraction peaks and DSC endothermic peak of nifedipine crystals were not found for the coground mixture, whereas a new exothermic peak was observed on DSC thermograms. The magnitude of this exothermic peak depended on the weight fraction of DCNa and the grinding time, indicating that nifedipine crystals changed into an amorphous state by complex formation with DCNa during the grinding process. In the FTIR spectrum of the coground mixture, the peaks of aromatic CH out-of-plane bend and dihydropyridine NH stretch of nifedipine were considerably weakened, suggesting that van der Waals interaction may be present between the drug and DCNa molecules. From these results, it is clear that the cogrinding method with DCNa is very useful for the formation of amorphous nifedipine in the solid state and the production of colloidal particles of the drug in solution.

Buffers↗

PubMed2002

Scalable solid-state quantum processor using subradiant two-atom states.

We propose a realization of a scalable, high-performance quantum processor whose qubits are represented by the ground and subradiant states of effective dimers formed by pairs of two-level systems coupled by resonant dipole-dipole interaction. The dimers are implanted in low-temperature solid host material at controllable nanoscale separations. The two-qubit entanglement either relies on the coherent excitation exchange between the dimers or is mediated by external laser fields.

Journal Article↗

PubMed2003

Broadband saturable absorber with cobalt-doped tellurite glasses.

A robust solid-state saturable absorber was developed with cobalt-ion-doped tellurite glasses that has a broad saturable-absorption band in the near-infrared. A nonlinear optical absorber was measured by the Z-scan technique. Numerically fitting the Z-scan experimental data yields excited-state absorption cross sections at a 1064-nm laser wavelength of sigma(es) = 1.45 x 10(-20) and sigma(es) = 1.15 x 10(-20) cm2 for 1.0- and 2.5-at. % Co2+-doped glasses, respectively.

Journal Article↗