Low-angle x-ray estimation of macromolecular parameters of the scattering particles in Agave sisalana

Various macromolecular parameters of Agave sisalana (sisal) fiber were investigated by the low-angle x-ray scattering method. The well known Kratky camera of the latest design was utilized for the experimental measurements. The sample studied was a densely packed colloidal system belonging to a general micelle system, and the theories of Kratky and Kratky and Porod were utilized to estimate the parameters. Pore analysis of the substance yields a value for the specific inner surface of the dispersed phase of 0.406 × 10^?1 m²/cm³; the transversal length is the same as the length of inhomogeneity, 107.31 Å, and the length of coherence is 342.21 Å. The air fraction of the scattering particles was found to be 0.01%.     

Separation of metalloporphyrins from metallation reactions by liquid chromatography and electrophoresis

The analytical separation of the indium and manganese complexes of three synthetic, meso-substituted, water-soluble porphyrins from their respective free bases in metallation reaction mixtures is described. The ligands tetra-3N-methylpyridyl porphyrin, tetra-4N-methylpyridyl porphyrin and tetra-N,N,N-trimethylanilinium porphyrin are complexed with In (III) and Mn (III) and are separated from residual free base by high-performance liquid chromatography (HPLC) in acidic conditions with gradient elution on ODS bonded stationary phase. Electrophoretic separation is achieved on both cellulose polyacetate strips and polyacrylamide tube gels under basic conditions. Although analytical separations can be achieved by both HPLC and electrophoresis, only HPLC is suitable for the development of preparative scale separations. Column chromatography, ion-pairing and ion-suppression HPLC techniques fail to separate such highly charged and closely related aromatic compounds.     

Determination of zirconium,thorium and scandium with 2,5-dihydroxy-1,4-benzoquinone

Zirconium is quantitatively precipitated by 2,5-dihydroxy-1,4-benzoquinone and is separated from scandium in 1 N hydrochloric acid solution. Thorium is separated at pH 0.5 from uranium(VI), cerium(IV), lanthanum, yttrium and scandium. Scandium is quantitatively precipitated by this reagent in the pH range 1.4–2.0 and at pH 1.5 equivalent amounts of lanthanum do not interfere; small amounts of yttrium cause interference.     

Mass spectrometric profiling of N-linked oligosaccharides and uncommon glycoform in mouse serum with head and neck tumor

N-linked oligosaccharides obtained from total serum of mice with implanted head and neck tumors were analyzed and compared with those from control samples of healthy mice. Methods used include a combination of a derivatization procedure with phenylhydrazine (PHN) and analysis by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Oligosaccharides were enzymatically released from total serum with PNGaseF and purified by high-performance liquid chromatography (HPLC) on a reversed-phase column. Mass spectra contained ion peaks of labeled oligosaccharides and MS/MS experiments provided useful data for the structural elucidation of these compounds. More than 40 N-glycans with compositions characteristic of high-mannose, hybrid, complex, neutral, and sialylated structures were identified in the serum of tumoral mice. Significant differences between samples were observed with respect to the abundances of high mannose and hybrid glycans. These oligosaccharides showed higher relative intensities in the spectra obtained from the cancer sera. Complex sialylated oligosaccharides had similar abundances in both types of sera, with the exception of fucosylated biantennary disialylated oligosaccharide, which was mostly detected with lower abundance in control samples. In the MALDI spectra, several minor species corresponded to uncommon carbohydrates. These structures have been investigated in detail by MS/MS. Among these novel glycoforms, a few sialylated oligosaccharides without a free reducing end were identified. Also, glycans with an extra 60 u were observed and likely feature the presence of a 2-acetamido-2-deoxyoctose residue attached on antennae of 3- or 6-linked mannose.     

Normal coordinate analysis and quantum chemical study of tris(p-fluorophenyl)antimony di(N-phenylglycinate) [(p-FC6H4)3Sb(O2CCH2NHC6H5)2]

A complete normal coordinate analysis was performed by two different methods: a classical Wilson’s G-F matrix method and the semi-empirical molecular orbital PM3 method, for a five coordinate tris(p-fluorophenyl)antimony di(N-phenylglycinate) [(p-FC₆H₄)₃Sb(O₂CCH₂NHC₆H₅)₂], known to be an in vitro antitumour molecule.      

Realization of an advanced nozzle concept for compact chemical oxygen iodine laser

Conventional supersonic chemical oxygen–iodine lasers (SCOIL) are not only low-pressure systems, with cavity pressure of 2–3 Torr and Mach number of approximately 1.5, but also are high-throughput systems with a typical laser power per unit evacuation capacity of nearly 1 J/l, thus demanding high capacity vacuum systems which mainly determine the compactness of the system. These conventional nozzle-based systems usually require a minimum of a two-stage ejector system for realization of atmospheric pressure recovery in a SCOIL. Typically for a 500 W class SCOIL, a first stage requires a motive gas flow (air) of 120 gm/s to entrain a laser gas flow of 3 g/s and is capable of achieving the pressure recovery in the range of 60–80 Torr. On the other hand, the second stage ejector requires 4.5 kg/s of motive gas (air) to achieve atmospheric pressure recovery. An advanced nozzle, also known as ejector nozzle, suitable for a 500 W-class SCOIL employing an active medium flow of nearly 12 g/s, has been developed and used instead of a conventional slit nozzle. The nozzle has been tested in both cold as well as hot run conditions of SCOIL, achieving a typical cavity pressure of nearly 10 Torr, stagnation pressure of approximately 85 Torr and a cavity Mach number of 2.5. The present study details the gas dynamic aspects of this ejector nozzle and highlights its potential as a SCOIL pressure recovery device. This nozzle in conjunction with a diffuser is capable of achieving pressure recovery equivalent to a more cumbersome first stage of the pressure recovery system used in the case of a conventional slit nozzle-based system. Thus, use of this nozzle in place of a conventional slit nozzle can achieve atmospheric discharge using a single stage ejector system, thereby making the pressure recovery system quite compact.     

Synthesis and characterization of hydrogen-bonded assemblies of W6S8L6 clusters

Ligand-exchange reactions involving octahedral W6S8 clusters and a family of pyridine-based ligands (isonicotinic acid, isonicotinamide, 4-hydroxypyridine, 4-aminopyridine, 4-pyridineacetamide) have been explored with the goal of preparing compounds that crystallize in hydrogen-bonded arrays. Two new compounds, W6S8(4-pyridineacetamide)6.DMF.4-pyridineacetamide (1) and W6S8(4-aminopyridine)6.4DMF (2), were isolated and characterized by single-crystal X-ray diffraction. Both compounds crystallize in the P2(1)/c space group with a = 16.461(1), b = 33.08(2), c = 13.165(10) A, beta = 103.270(15) degrees for 1 and a = 13.8988(5), b = 13.2791(5), c = 15.6293(6) A, beta = 108.5410(10) degrees for 2. Each compound was further characterized by 1H NMR spectroscopy, elemental (CHN) analysis, and thermogravimetric analysis. Examination of the structures shows that 1 forms a three-dimensional hydrogen-bonded network in which each 4-pyridineacetamide ligand interacts with ligands on neighboring clusters or with the free ligand of crystallization. This is the first hydrogen-bonded network formed from W6S8 clusters. In 2, the amino groups act as hydrogen-bond donors toward DMF molecules of crystallization, but an extended array is not formed. In addition, the binding strengths of these pyridine-based ligands to the W6S8 cluster were studied through quantitative 1H NMR studies of ligand-exchange reactions. A qualitative relationship was found between ligand binding strengths and Hammett substituent constants for this group of ligands.     

Broad energy spectrum of laser-accelerated protons for spallation-related physics

A beam of MeV protons, accelerated by ultraintense laser-pulse interactions with a thin target foil, is used to investigate nuclear reactions of interest for spallation physics. The laser-generated proton beam is shown (protons were measured) to have a broad energy distribution, which closely resembles the expected energy spectrum of evaporative protons (below 50 MeV) produced in GeV-proton-induced spallation reactions. The protons are used to quantify the distribution of residual radioisotopes produced in a representative spallation target (Pb), and the results are compared with calculated predictions based on spectra modeled with nuclear Monte Carlo codes. Laser-plasma particle accelerators are shown to provide data relevant to the design and development of accelerator driven systems.     

Lamb wave characteristics of thickness-graded piezoelectric IDT

An equivalent single layer model of Lamb wave generation by thickness-graded piezoelectric IDT on host structure is developed. Various additional complexities, such as the coupling between the Lamb wave modes, complicated nature of the electro-mechanical excitation are considered. The model of infinite IDT is extended to deal with the finite IDT with edge discontinuities. The effects of electromechanical coupling and thickness gradation on the wavelength shifts are investigated. The problem of electrically driven instability within the IDT is analyzed. Numerical results are reported by considering Al2O3/PZT IDT as integral part of the host structure, which show that there are significant changes and improvements in the Lamb wave characteristics due to the graded configuration. Most important among these is the reduced dispersiveness of the Lamb wave modes, which is useful in launching a SAW that propagates with narrower pulse width and less attenuation.