Effects of Solid Solution Treatments on the Microstructure and Mechanical Properties of a Nanoscale Precipitate-Strengthened Ferritic Steel

NASA Astrophysics Data System (ADS)

Zhao, Y.; Guo, H.; Xu, S. S.; Mao, M. J.; Chen, L.; Gokhman, O.; Zhang, Z. W.

2018-05-01

Solid solution treatment (SST) and age hardening are the two main treatments used to produce nanoscale precipitation-strengthened steels. In this work, solution treatment and aging are employed to develop a nanoscale precipitation-strengthened steel displaying high degrees of strength, ductility, and toughness. The effects of SST on the microstructure and mechanical properties of the produced steel are investigated. The results show that the solution temperature strongly influences the matrix microstructure. Partial austenitization between A_{{{c}1}} and A_{{{c}3}} favors the formation of granular ferrite, while complete austenitization above A_{{{c}3}} leads to the formation of polygonal ferrite. Refined granular ferrite with a low dislocation density can effectively improve the plasticity and low-temperature toughness of steel. Precipitation strengthening is mainly related to the nature of the nano-precipitates, specifically their size and number density, independently of the matrix microstructure.

Carbon nanotubes as adsorbent of solid-phase extraction and matrix for laser desorption/ionization mass spectrometry.

PubMed

Pan, Chensong; Xu, Songyun; Zou, Hanfa; Guo, Zhong; Zhang, Yu; Guo, Baochuan

2005-02-01

A method with carbon nanotubes functioning both as the adsorbent of solid-phase extraction (SPE) and the matrix for matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) to analyze small molecules in solution has been developed. In this method, 10 microL suspensions of carbon nanotubes in 50% (vol/vol) methanol were added to the sample solution to extract analytes onto surface of carbon nanotubes because of their dramatic hydrophobicity. Carbon nanotubes in solution are deposited onto the bottom of tube with centrifugation. After removing the supernatant fluid, carbon nanotubes are suspended again with dispersant and pipetted directly onto the sample target of the MALDI-MS to perform a mass spectrometric analysis. It was demonstrated by analysis of a variety of small molecules that the resolution of peaks and the efficiency of desorption/ionization on the carbon nanotubes are better than those on the activated carbon. It is found that with the addition of glycerol and sucrose to the dispersant, the intensity, the ratio of signal to noise (S/N), and the resolution of peaks for analytes by mass spectrometry increased greatly. Compared with the previously reported method by depositing sample solution onto thin layer of carbon nanotubes, it is observed that the detection limit for analytes can be enhanced about 10 to 100 times due to solid-phase extraction of analytes in solution by carbon nanotubes. An acceptable result of simultaneously quantitative analysis of three analytes in solution has been achieved. The application in determining drugs spiked into urine has also been realized.

A hybrid method for transient wave propagation in a multilayered solid

NASA Astrophysics Data System (ADS)

Tian, Jiayong; Xie, Zhoumin

2009-08-01

We present a hybrid method for the evaluation of transient elastic-wave propagation in a multilayered solid, integrating reverberation matrix method with the theory of generalized rays. Adopting reverberation matrix formulation, Laplace-Fourier domain solutions of elastic waves in the multilayered solid are expanded into the sum of a series of generalized-ray group integrals. Each generalized-ray group integral containing Kth power of reverberation matrix R represents the set of K-times reflections and refractions of source waves arriving at receivers in the multilayered solid, which was computed by fast inverse Laplace transform (FILT) and fast Fourier transform (FFT) algorithms. However, the calculation burden and low precision of FILT-FFT algorithm limit the application of reverberation matrix method. In this paper, we expand each of generalized-ray group integrals into the sum of a series of generalized-ray integrals, each of which is accurately evaluated by Cagniard-De Hoop method in the theory of generalized ray. The numerical examples demonstrate that the proposed method makes it possible to calculate the early-time transient response in the complex multilayered-solid configuration efficiently.

Stabilization of a supersaturated solution of mefenamic acid from a solid dispersion with EUDRAGIT(®) EPO.

PubMed

Kojima, Taro; Higashi, Kenjirou; Suzuki, Toyofumi; Tomono, Kazuo; Moribe, Kunikazu; Yamamoto, Keiji

2012-10-01

The stabilization mechanism of a supersaturated solution of mefenamic acid (MFA) from a solid dispersion with EUDRAGIT(®) EPO (EPO) was investigated. The solid dispersions were prepared by cryogenic grinding method. Powder X-ray diffractometry, in vitro dissolution test, in vivo oral absorption study, infrared spectroscopy, and solid- and solution-state NMR spectroscopies were used to characterize the solid dispersions. Dissolution tests in acetate buffer (pH 5.5) revealed that solid dispersion showed > 200-fold higher concentration of MFA. Supersaturated solution was stable over 1 month and exhibited improved oral bioavailability of MFA in rats, with a 7.8-fold higher area under the plasma concentration-versus-time curve. Solid-state (1)H spin-lattice relaxation time (T(1)) measurement showed that MFA was almost monomolecularly dispersed in the EPO polymer matrix. Intermolecular interaction between MFA and EPO was indicated by solid-state infrared and (13)C-T(1) measurements. Solution-state (1)H-NMR measurement demonstrated that MFA existed in monomolecular state in supersaturated solution. (1)H-T(1) and difference nuclear Overhauser effect measurements indicated that cross relaxation occurred between MFA and EPO due to the small distance between them. The formation and high stability of the supersaturated solution were attributable to the specifically formed intermolecular interactions between MFA and EPO.

The solid-solution region for the langasite-type Ca3TaGa3Si2O14 crystal as determined by a lever rule

NASA Astrophysics Data System (ADS)

Zhao, Hengyu; Uda, Satoshi; Maeda, Kensaku; Nozawa, Jun; Koizumi, Haruhiko; Fujiwara, Kozo

2015-04-01

A lever rule was applied to data concerning the compositions and proportions of secondary phases coexisting with a Ca3TaGa3Si2O14 (CTGS) matrix to determine the boundary compositions of the solid-solution region for CTGS at 1320 °C, as a means of ascertaining the solid-solution for the langasite-type phase in the quaternary CaO-Ta2O5-Ga2O3-SiO2 system. The compositions and proportions of secondary phases were assessed by electron probe micro-analysis as well as through back-scattered electron images. The experimental results showed that the narrow solid-solution region for CTGS is located in a Ta-poor, Ga-poor and Si-rich region relative to its stoichiometric composition.

Lattice mismatch modeling of aluminum alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shin, Dongwon; Roy, Shibayan; Watkins, Thomas R.

We present a theoretical framework to accurately predict the lattice mismatch between the fcc matrix and precipitates in the multi-component aluminum alloys as a function of temperature and composition. We use a computational thermodynamic approach to model the lattice parameters of the multi-component fcc solid solution and θ'-Al2Cu precipitate phase. Better agreement between the predicted lattice parameters of fcc aluminum in five commercial alloys (206, 319, 356, A356, and A356 + 0.5Cu) and experimental data from the synchrotron X-ray diffraction (SXD) has been obtained when simulating supersaturated rather than equilibrium solid solutions. We use the thermal expansion coefficient of thermodynamicallymore » stable θ-Al2Cu to describe temperature-dependent lattice parameters of meta-stable θ' and to show good agreement with the SXD data. Both coherent and semi-coherent interface mismatches between the fcc aluminum matrix and θ' in Al-Cu alloys are presented as a function of temperature. Our calculation results show that the concentration of solute atoms, particularly Cu, in the matrix greatly affects the lattice mismatch« less

Design principles for radiation-resistant solid solutions

NASA Astrophysics Data System (ADS)

Schuler, Thomas; Trinkle, Dallas R.; Bellon, Pascal; Averback, Robert

2017-05-01

We develop a multiscale approach to quantify the increase in the recombined fraction of point defects under irradiation resulting from dilute solute additions to a solid solution. This methodology provides design principles for radiation-resistant materials. Using an existing database of solute diffusivities, we identify Sb as one of the most efficient solutes for this purpose in a Cu matrix. We perform density-functional-theory calculations to obtain binding and migration energies of Sb atoms, vacancies, and self-interstitial atoms in various configurations. The computed data informs the self-consistent mean-field formalism to calculate transport coefficients, allowing us to make quantitative predictions of the recombined fraction of point defects as a function of temperature and irradiation rate using homogeneous rate equations. We identify two different mechanisms according to which solutes lead to an increase in the recombined fraction of point defects; at low temperature, solutes slow down vacancies (kinetic effect), while at high temperature, solutes stabilize vacancies in the solid solution (thermodynamic effect). Extension to other metallic matrices and solutes are discussed.

Dual-phase Cr-Ta alloys for structural applications

DOEpatents

Liu, Chain T.; Brady, Michael P.; Zhu, Jiahong; Tortorelli, Peter F.

2001-01-01

Dual phase alloys of chromium containing 2 to 11 atomic percent tantalum with minor amounts of Mo, Cr, Ti, Y, La, Cr, Si and Ge are disclosed. These alloys contain two phases including Laves phase and Cr-rich solid solution in either eutectic structures or dispersed Laves phase particles in the Cr-rich solid solution matrix. The alloys have superior mechanical properties at high temperature and good oxidation resistance when heated to above 1000.degree. C. in air.

The effect of solute additions on the steady-state creep behavior of dispersion-strengthened aluminum.

NASA Technical Reports Server (NTRS)

Reynolds, G. H.; Lenel, F. V.; Ansell, G. S.

1971-01-01

The effect of solute additions on the steady-state creep behavior of coarse-grained dispersion-strengthened aluminum alloys was studied. Recrystallized dispersion-strengthened solid solutions were found to have stress and temperature sensitivities quite unlike those observed in single-phase solid solutions having the same composition and grain size. The addition of magnesium or copper to the matrix of a recrystallized dispersion-strengthened aluminum causes a decrease in the steady-state creep rate which is much smaller than that caused by similar amounts of solute in single-phase solid solutions. All alloys exhibited essentially a 4.0 power stress exponent in agreement with the model of Ansell and Weertman. The activation energy for steady-state creep in dispersion-strengthened Al-Mg alloys, as well as the stress dependence, was in agreement with the physical model of dislocation climb over the dispersed particles.

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

PubMed

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

INTERNATIONAL CONFERENCE ON SEMICONDUCTOR INJECTION LASERS SELCO-87: Method for calculation of electrical and optical properties of laser active media

NASA Astrophysics Data System (ADS)

Aleksandrov, D. G.; Filipov, F. I.

1988-11-01

A method is proposed for calculation of the electron band structure of multicomponent semiconductor solid solutions. Use is made of virtual atomic orbitals formed from real orbitals. The method represents essentially an approximation of a multicomponent solid solution by a binary one. The matrix elements of the Hamiltonian are obtained in the methods of linear combinations of atomic and bound orbitals. Some approximations used in these methods are described.

Effects of Drying Process on an IgG1 Monoclonal Antibody Using Solid-State Hydrogen Deuterium Exchange with Mass Spectrometric Analysis (ssHDX-MS).

PubMed

Moussa, Ehab M; Wilson, Nathan E; Zhou, Qi Tony; Singh, Satish K; Nema, Sandeep; Topp, Elizabeth M

2018-01-03

Lyophilization and spray drying are widely used to manufacture solid forms of therapeutic proteins. Lyophilization is used to stabilize proteins vulnerable to degradation in solution, whereas spray drying is mainly used to prepare inhalation powders or as an alternative to freezing for storing bulk drug substance. Both processes impose stresses that may adversely affect protein structure, stability and bioactivity. Here, we compared lyophilization with and without controlled ice nucleation, and spray drying for their effects on the solid-state conformation and matrix interactions of a model IgG1 monoclonal antibody (mAb). Solid-state conformation and matrix interactions of the mAb were probed using solid-state hydrogen-deuterium exchange with mass spectrometric analysis (ssHDX-MS), and solid-state Fourier transform infrared (ssFTIR) and solid-state fluorescence spectroscopies. mAb conformation and/or matrix interactions were most perturbed in mannitol-containing samples and the distribution of states was more heterogeneous in sucrose and trehalose samples that were spray dried. The findings demonstrate the sensitivity of ssHDX-MS to changes weakly indicated by spectroscopic methods, and support the broader use of ssHDX-MS to probe formulation and process effects on proteins in solid samples.

Assessment of Recovery of Milk Protein Allergens from Processed Food for Mass Spectrometry Quantification.

PubMed

Groves, Kate; Cryar, Adam; Walker, Michael; Quaglia, Milena

2018-01-01

Assessing the recovery of food allergens from solid processed matrixes is one of the most difficult steps that needs to be overcome to enable the accurate quantification of protein allergens by immunoassay and MS. A feasibility study is described herein applying International System of Units (SI)-traceably quantified milk protein solutions to assess recovery by an improved extraction method. Untargeted MS analysis suggests that this novel extraction method can be further developed to provide high recoveries for a broad range of food allergens. A solution of α-casein was traceably quantified to the SI for the content of α-S1 casein. Cookie dough was prepared by spiking a known amount of the SI-traceable quantified solution into a mixture of flour, sugar, and soya spread, followed by baking. A novel method for the extraction of protein food allergens from solid matrixes based on proteolytic digestion was developed, and its performance was compared with the performance of methods reported in the literature.

Method for treating liquid wastes

DOEpatents

Katti, K.V.; Volkert, W.A.; Singh, P.; Ketring, A.R.

1995-12-26

The method of treating liquid waste in a media is accomplished by exposing the media to phosphinimines and sequestering {sup 99}Tc from the media by the phosphinimine (PN) functionalities. The system for treating the liquid waste in the media includes extraction of {sup 99}TcO{sub 4}{sup {minus}} from aqueous solutions into organic solvents or mixed organic/polar media, extraction of {sup 99}Tc from solutions on a solid matrix by using a container containing PN functionalities on solid matrices including an inlet and outlet for allowing flow of media through an immobilized phosphinimine ligand system contained within the container. Also, insoluble suspensions of phosphinimine functionalities on solid matrices in liquid solutions or present on supported liquid membranes (SLM) can be used to sequester {sup 99}Tc from those liquids. 6 figs.

Method for treating liquid wastes

DOEpatents

Katti, Kattesh V.; Volkert, Wynn A.; Singh, Prahlad; Ketring, Alan R.

1995-01-01

The method of treating liquid waste in a media is accomplished by exposing the media to phosphinimines and sequestering .sup.99 Tc from the media by the phosphinimine (PN) functionalities. The system for treating the liquid waste in the media includes extraction of .sup.99 TcO.sub.4.sup.- from aqueous solutions into organic solvents or mixed organic/polar media, extraction of .sup.99 Tc from solutions on a solid matrix by using a container containing PN functionalities on solid matrices including an inlet and outlet for allowing flow of media through an immobilized phosphinimine ligand system contained within the container. Also, insoluble suspensions of phosphinimine functionalities on solid matrices in liquid solutions or present on supported liquid membranes (SLM) can be used to sequester .sup.99 Tc from those liquids.

Iron in solution with aluminum matrix after non-equilibrium processing: an atom probe tomography study

NASA Astrophysics Data System (ADS)

Saller, Brandon D.; Sha, Gang; Yang, Li Mei; Liu, Fan; Ringer, Simon P.; Schoenung, Julie M.

2017-03-01

In this paper, we report on the influence of rapid solidification and severe plastic deformation on the solid solubility of Fe in Al. Atom probe tomography, for the first time, was performed on fine (3-4 μm diameter) and coarse ( 100 μm) as-atomised Al-5 at.% Fe powder and cryomilled Al-5 at.% Fe powder. The atomised powders exhibited negligible Fe in solution with Al, whereas the cryomilled powder contained 2 at.% Fe in solution. Moreover, our results suggest that severe plastic deformation is preferable to atomisation/rapid solidification for increasing the non-equilibrium solid solubility of Fe in Al.

Impact of polymers on the crystallization and phase transition kinetics of amorphous nifedipine during dissolution in aqueous media.

PubMed

Raina, Shweta A; Alonzo, David E; Zhang, Geoff G Z; Gao, Yi; Taylor, Lynne S

2014-10-06

The commercial and clinical success of amorphous solid dispersions (ASD) in overcoming the low bioavailability of poorly soluble molecules has generated momentum among pharmaceutical scientists to advance the fundamental understanding of these complex systems. A major limitation of these formulations stems from the propensity of amorphous solids to crystallize upon exposure to aqueous media. This study was specifically focused on developing analytical techniques to evaluate the impact of polymers on the crystallization behavior during dissolution, which is critical in designing effective amorphous formulations. In the study, the crystallization and polymorphic conversions of a model compound, nifedipine, were explored in the absence and presence of polyvinylpyrrolidone (PVP), hydroxypropylmethyl cellulose (HPMC), and HPMC-acetate succinate (HPMC-AS). A combination of analytical approaches including Raman spectroscopy, polarized light microscopy, and chemometric techniques such as multivariate curve resolution (MCR) were used to evaluate the kinetics of crystallization and polymorphic transitions as well as to identify the primary route of crystallization, i.e., whether crystallization took place in the dissolving solid matrix or from the supersaturated solutions generated during dissolution. Pure amorphous nifedipine, when exposed to aqueous media, was found to crystallize rapidly from the amorphous matrix, even when polymers were present in the dissolution medium. Matrix crystallization was avoided when amorphous solid dispersions were prepared, however, crystallization from the solution phase was rapid. MCR was found to be an excellent data processing technique to deconvolute the complex phase transition behavior of nifedipine.

Synthesis and fluorescence properties of some difluoroboron β-diketonate complexes and composite containing PMMA

NASA Astrophysics Data System (ADS)

Xing, Dongye; Hou, Yanjun; Niu, Haijun

2018-03-01

A series of difluoroboron β-diketonate complexes, containing the indon-β-diketonate ligand carrying methyl or methoxyl substituents was synthesized. The crystal structures of the complexes were confirmed by single crystal X-ray diffraction studies. The fluorescence properties of compounds were studied in solution state, solid state and on PMMA polymer matrix. The photophysical data of compounds 2a-2d exhibited strong fluorescence and photostability under the ultraviolet light (Hg lamp). The complex 2b showed higher fluorescence intensity in solution state as compared to other complexes of the series. The complexes 2c and 2d showed higher fluorescence intensity in the solid state, which are ascribed to the stronger π-π interactions between ligands in the solid state. The introduction of methoxyl or methyl groups on the benzene rings enhanced the absorption intensity, emission intensity, quantum yields and fluorescence lifetimes due to their electron-donating nature. Furthermore, the complex 2b was doped into the PMMA to produce hybrid materials, where the PMMA matrix acted as sensitizer for the central boron ion to enhance the fluorescence emission intensity and quantum yields.

Impact of fluid-rock chemical interactions on tracer transport in fractured rocks.

PubMed

Mukhopadhyay, Sumit; Liu, H-H; Spycher, N; Kennedy, B M

2013-11-01

In this paper, we investigate the impact of chemical interactions, in the form of mineral precipitation and dissolution reactions, on tracer transport in fractured rocks. When a tracer is introduced in fractured rocks, it moves through the fracture primarily by advection and it also enters the stagnant water of the surrounding rock matrix through diffusion. Inside the porous rock matrix, the tracer chemically interacts with the solid materials of the rock, where it can precipitate depending on the local equilibrium conditions. Alternatively, it can be dissolved from the solid phase of the rock matrix into the matrix pore water, diffuse into the flowing fluids of the fracture and is advected out of it. We show that such chemical interactions between the fluid and solid phases have significant impact on tracer transport in fractured rocks. We invoke the dual-porosity conceptualization to represent the fractured rocks and develop a semi-analytical solution to describe the transient transport of tracers in interacting fluid-rock systems. To test the accuracy and stability of the semi-analytical solution, we compare it with simulation results obtained with the TOUGHREACT simulator. We observe that, in a chemically interacting system, the tracer breakthrough curve exhibits a pseudo-steady state, where the tracer concentration remains more or less constant over a finite period of time. Such a pseudo-steady condition is not observed in a non-reactive fluid-rock system. We show that the duration of the pseudo-state depends on the physical and chemical parameters of the system, and can be exploited to extract information about the fractured rock system, such as the fracture spacing and fracture-matrix interface area. © 2013.

Development of clinical dosage forms for a poorly water-soluble drug II: formulation and characterization of a novel solid microemulsion preconcentrate system for oral delivery of a poorly water-soluble drug.

PubMed

Li, Ping; Hynes, Sara R; Haefele, Thomas F; Pudipeddi, Madhu; Royce, Alan E; Serajuddin, Abu T M

2009-05-01

The solution of a poorly water-soluble drug in a liquid lipid-surfactant mixture, which served as a microemulsion preconcentrate, was converted into a solid form by incorporating it in a solid polyethylene glycol (PEG) matrix. The solid microemulsion preconcentrates thus formed consisted of Capmul PG8 (propylene glycol monocaprylate) as oil, Cremophor EL (polyoxyl 35 castor oil) as surfactant, and hydrophilic polymer PEG 3350 as solid matrix. The drug (aqueous solubility: 0.17 microg/mL at pH 1-8 and 25 degrees C) was dissolved in a melt of the mixture at 65-70 degrees C and then the hot solution was filled into hard gelatin capsules; the liquid gradually solidified upon cooling below 55 degrees C. The solid system was characterized by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), confocal Raman microscopy (CRM), and the dispersion testing in water. It was confirmed that a solid microemulsion preconcentrate is a two-phase system, where clusters of crystalline PEG 3350 formed the solid structure (m.p. 55-60 degrees C) and the liquid microemulsion preconcentrate dispersed in between PEG 3350 crystals as a separate phase. The drug remained dissolved in the liquid phase. In vitro release testing showed that the preconcentrate dispersed readily in water forming a microemulsion with the drug dissolved in the oil particles (<150 nm) and the presence of PEG 3350 did not interfere with the process of self-microemulsification.

Transient Liquid-Phase Diffusion Bonding of Aluminum Metal Matrix Composite Using a Mixed Cu-Ni Powder Interlayer

NASA Astrophysics Data System (ADS)

Maity, Joydeep; Pal, Tapan Kumar

2012-07-01

In the present study, the transient liquid-phase diffusion bonding of an aluminum metal matrix composite (6061-15 wt.% SiCp) has been investigated for the first time using a mixed Cu-Ni powder interlayer at 560 °C, 0.2 MPa, for different holding times up to 6 h. The microstructure of the isothermally solidified zone contains equilibrium precipitate CuAl2, metastable precipitate Al9Ni2 in the matrix of α-solid solution along with the reinforcement particles (SiC). On the other hand, the microstructure of the central bond zone consists of equilibrium phases such as NiAl3, Al7Cu4Ni and α-solid solution along with SiC particles (without any segregation) and the presence of microporosities. During shear test, the crack originates from microporosities and propagates along the interphase interfaces resulting in poor bond strength for lower holding times. As the bonding time increases, with continual diffusion, the structural heterogeneity is diminished, and the microporosities are eliminated at the central bond zone. Accordingly, after 6-h holding, the microstructure of the central bond zone mainly consists of NiAl3 without any visible microporosity. This provides a joint efficiency of 84% with failure primarily occurring through decohesion at the SiC particle/matrix interface.

Heat and corrosion resistant cast CN-12 type stainless steel with improved high temperature strength and ductility

DOEpatents

Mazias, Philip J [Oak Ridge, TN; McGreevy, Tim [Morton, IL; Pollard, Michael James [East Peoria, IL; Siebenaler, Chad W [Peoria, IL; Swindeman, Robert W [Oak Ridge, TN

2007-08-14

A cast stainless steel alloy and articles formed therefrom containing about 0.5 wt. % to about 10 wt. % manganese, 0.02 wt. % to 0.50 wt. % N, and less than 0.15 wt. % sulfur provides high temperature strength both in the matrix and at the grain boundaries without reducing ductility due to cracking along boundaries with continuous or nearly-continuous carbides. Alloys of the present invention also have increased nitrogen solubility thereby enhancing strength at all temperatures because nitride precipitates or nitrogen porosity during casting are not observed. The solubility of nitrogen is dramatically enhanced by the presence of manganese, which also retains or improves the solubility of carbon thereby providing additional solid solution strengthening due to the presence of manganese and nitrogen, and combined carbon. Such solution strengthening enhances the high temperature precipitation-strengthening benefits of fine dispersions of NbC. Such solid solution effects also enhance the stability of the austenite matrix from resistance to excess sigma phase or chrome carbide formation at higher service temperatures. The presence of sulfides is substantially eliminated.

Composite Properties of Polyimide Resins Made From "Salt-Like" Solution Precursors

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Weiser, Erik S.; SaintClair, Terry L.; Echigo, Yoshiaki; Kaneshiro, Hisayasu

1997-01-01

Recent work in high temperature materials at NASA Langley Research Center (LaRC (trademark)) have led to the development of new polyimide resin systems with very attractive properties. The majority of the work done with these resin systems has concentrated on determining engineering mechanical properties of composites prepared from a poly(amide acid) precursor. Three NASA Langley-developed polyimide matrix resins, LaRC (trademark) -IA, LaRC (trademark) -IAX, and LaRC (trademark) -8515, were produced via a salt-like process developed by Unitika Ltd. The 'salt-like' solutions (sixty-five percent solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC Multipurpose Tape Machine. Process parameters were determined and composite panels fabricated. Mechanical properties are presented for these three intermediate modulus carbon fiber/polyimide matrix composites and compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (thirty-five percent solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of polyimide composites.

Micromechanics investigation of expansive reactions in chemoelastic concrete.

PubMed

Lemarchand, Eric; Dormieux, Luc; Ulm, Franz-Josef

2005-11-15

Expansive reactions damage porous materials through the formation of reaction products of a volume in excess of the available space left by the reactants and the natural porosity of the material. This leads to pressurizing the pore space accessible to the reaction products, which differs when the chemical reaction is through-solution or topochemical or both in nature. This paper investigates expansive reactions from a micromechanical point of view, which allows bridging the scale from the local chemo-mechanical mechanisms to the macroscopically observable stress-free expansion. In particular, the study of the effect of morphology of the pore space, in which the chemical expansion occurs locally, on the macroscopically observable expansion is the main focus of this paper. The first part revisits the through-solution and the topochemical reaction mechanism within the framework of micro-macro-homogenization theories, and the effect of the microscopic geometry of pores and microcracks in the solid matrix on the macroscopic chemical expansion is examined. The second part deals with the transition from a topochemical to a through-solution-like mechanism that occurs in a solid matrix with inclusions (cracks, pores) of different morphology.

Survey of Portions of the Chromium-Cobalt-Nickel-Molybdenum Quaternary System at 1,200 Degrees C

NASA Technical Reports Server (NTRS)

Rideout, Sheldon Paul; Beck, Paul A

1953-01-01

A survey was made of portions of the chromium-cobalt-nickel-molybdenum quaternary system at 1,200 degrees c by means of microscopic and x-ray diffraction studies. Since the face-centered cubic (alpha) solid solutions form the matrix of almost all practically useful high-temperature alloys, the solid solubility limits of the quaternary alpha phase were determined up to 20 percent molybdenum. The component cobalt-nickel-molybdenum, chromium-cobalt-molybdenum, and chromium-nickel-molybdenum ternary systems were also studied. The survey of these systems was confined to the determination of the boundaries of the face-centered cubic (alpha) solid solutions and of the phases coexisting with alpha at 1,200 degrees c.

Poly(2-ethyl-2-oxazoline) as matrix excipient for drug formulation by hot melt extrusion and injection molding.

PubMed

Claeys, Bart; Vervaeck, Anouk; Vervaet, Chris; Remon, Jean Paul; Hoogenboom, Richard; De Geest, Bruno G

2012-10-15

Here we evaluate poly(2-ethyl-2-oxazoline)s (PEtOx) as a matrix excipient for the production of oral solid dosage forms by hot melt extrusion (HME) followed by injection molding (IM). Using metoprolol tartrate as a good water-soluble model drug we demonstrate that drug release can be delayed by HME/IM, with the release rate controlled by the molecular weight of the PEtOx. Using fenofibrate as a lipophilic model drug we demonstrate that relative to the pure drug the dissolution rate is strongly enhanced by formulation in HME/IM tablets. For both drug molecules we find that solid solutions, i.e. molecularly dissolved drug in a polymeric matrix, are obtained by HME/IM. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigation of in situ gelling alginate formulations as a sustained release vehicle for co-precipitates of dextromethrophan and Eudragit S 100.

PubMed

El Maghraby, Gamal Mohamed; Elzayat, Ehab Mostafa; Alanazi, Fars Kaed

2014-03-01

Alginate vehicles are capable of forming a gel matrix in situ when they come into contact with gastric medium in the presence of calcium ions. However, the gel structure is pH dependent and can break after gastric emptying, leading to dose dumping. The aim of this work was to develop modified in situ gelling alginate formulations capable of sustaining dextromethorphan release throughout the gastrointestinal tract. Alginate solution (2 %, m/m) was used as a vehicle for the tested formulations. Solid matrix of the drug and Eudragit S 100 was prepared by dissolving the drug and polymer in acetone. The organic solvent was then evaporated and the deposited solid matrix was micronized, sieved and dispersed in alginate solution to obtain candidate formulations. The release behavior of dextromethorphan was monitored and evaluated in a medium simulating the gastric and intestinal pH. Drug-polymer compatibility and possible solid-state interactions suggested physical interaction through hydrogen bonding between the drug and the polymer. A significant decrease in the rate and extent of dextromethorphan release was observed with increasing Eudragit S 100 concentration in the prepared particles. Most formulations showed sustained release profiles similar to that of a commercial sustained-release liquid based on ion exchange resin. The release pattern indicated strict control of drug release both under gastric and intestinal conditions, suggesting the potential advantage of using a solid dispersion of drug-Eudragit S 100 to overcome the problem of dose dumping after the rupture of the pH dependent alginate gels.

Flexible poly(ethylene carbonate)/garnet composite solid electrolyte reinforced by poly(vinylidene fluoride-hexafluoropropylene) for lithium metal batteries

NASA Astrophysics Data System (ADS)

He, Zijian; Chen, Long; Zhang, Bochen; Liu, Yongchang; Fan, Li-Zhen

2018-07-01

Solid-state electrolytes with high ionic conductivities, great flexibility, and easy processability are needed for high-performance solid-state rechargeable lithium batteries. In this work, we synthesize nanosized cubic Li6.25Al0.25La3Zr2O12 (LLZO) by solution combustion method and develop a flexible garnet-based composite solid electrolyte composed of LLZO, poly(ethylene carbonate) (PEC), poly(vinylidene fluoride-hexafluoropropylene) (P(VdF-HFP) and lithium bis(fluorosulfonyl)imide (LiFSI)). In the flexible composite solid electrolytes, LLZO nanoparticles, as ceramic matrix, have a positive effect on ionic conductivities and lithium ion transference number (tLi+). PEC, as a fast ion-conducting polymer, possesses high tLi+ inherently. P(VdF-HFP), as a binder, can strengthen mechanical properties. Consequently, the as-prepared composite solid electrolyte demonstrates high tLi+ (0.82) and superb thermal stability (remaining LLZO matrix after burning). All-solid-state LiFePO4|Li cells assembled with the flexible composite solid electrolyte deliver a high initial discharge specific capacity of 121.4 mAh g-1 and good cycling stability at 55 °C.

Microbial response to environmental gradients in a ceramic-based diffusion system.

PubMed

Wolfaardt, G M; Hendry, M J; Birkham, T; Bressel, A; Gardner, M N; Sousa, A J; Korber, D R; Pilaski, M

2008-05-01

A solid, porous matrix was used to establish steady-state concentration profiles upon which microbial responses to concentration gradients of nutrients or antimicrobial agents could be quantified. This technique relies on the development of spatially defined concentration gradients across a ceramic plate resulting from the diffusion of solutes through the porous ceramic matrix. A two-dimensional, finite-element numerical transport model was used to predict the establishment of concentration profiles, after which concentration profiles of conservative tracers were quantified fluorometrically and chemically at the solid-liquid interface to verify the simulated profiles. Microbial growth responses to nutrient, hypochloride, and antimicrobial concentration gradients were then quantified using epifluorescent or scanning confocal laser microscopy. The observed microbial response verified the establishment and maintenance of stable concentration gradients along the solid-liquid interface. These results indicate the ceramic diffusion system has potential for the isolation of heterogeneous microbial communities as well as for testing the efficacy of antimicrobial agents. In addition, the durability of the solid matrix allowed long-term investigations, making this approach preferable to conventional gel-stabilized systems that are impeded by erosion as well as expansion or shrinkage of the gel. Copyright 2008 Wiley Periodicals, Inc.

Coulomb matrix elements in multi-orbital Hubbard models.

PubMed

Bünemann, Jörg; Gebhard, Florian

2017-04-26

Coulomb matrix elements are needed in all studies in solid-state theory that are based on Hubbard-type multi-orbital models. Due to symmetries, the matrix elements are not independent. We determine a set of independent Coulomb parameters for a d-shell and an f-shell and all point groups with up to 16 elements (O h , O, T d , T h , D 6h , and D 4h ). Furthermore, we express all other matrix elements as a function of the independent Coulomb parameters. Apart from the solution of the general point-group problem we investigate in detail the spherical approximation and first-order corrections to the spherical approximation.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Zeen; Hu, Rui; Zhang, Tiebang, E-mail: tiebang

The microstructure and solidification behavior of high Nb containing TiAl alloys with the composition of Ti-46Al-8Nb-xC (x = 0.1, 0.7, 1.4, 2.5 at.%) prepared by arc-melting method have been investigated in this work. The results give evidence that the addition of carbon changes the solidification behavior from solidification via the β phase to the peritectic solidification. And carbon in solid solution enriches in the α{sub 2} phase and increases the microhardness. As the carbon content increases to 1.4 at.%, plate-shape morphology carbides Ti{sub 2}AlC (H phase) precipitate from the TiAl matrix which leads to the refinement microstructure. By aging atmore » 1173 K for 24 h after quenching treatment, fine needle-like and granular shape Ti{sub 3}AlC (P phase) carbides are observed in the matrix of Ti-46Al-8Nb-2.5C alloy, which distribute along the lamellar structure or around the plate-shape Ti{sub 2}AlC. Transmission electron microscope observation shows that the Ti{sub 3}AlC carbides precipitate at dislocations. The phase transformation in-situ observations indicate that the Ti{sub 2}AlC carbides partly precipitate during the solid state phase transformation process. - Highlights: •Carbon changes the solidification behavior from β phase to peritectic solidification. •Dislocations in solution treated γ phase act as nucleation sites of Ti{sub 3}AlC precipitations. •Ti{sub 3}AlC precipitates as fine needle-like or granular shape in the solution treated matrix. •Ti{sub 2}AlC carbides precipitate during the solid state phase transformation process.« less

Interfacial Microstructure and Its Influence on Resistivity of Thin Layers Copper Cladding Steel Wires

NASA Astrophysics Data System (ADS)

Li, Hongjuan; Ding, Zhimin; Zhao, Ruirong

2018-04-01

The interfacial microstructure and resistivity of cold-drawn and annealed thin layers copper cladding steel (CCS) wires have been systematically investigated by the methods of scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), and resistivity testing. The results showed that the Cu and Fe atoms near interface diffused into each other matrixes. The Fe atoms diffused into Cu matrixes and formed a solid solution. The mechanism of solid solution is of substitution type. When the quantity of Fe atoms exceeds the maximum solubility, the supersaturated solid solution would form Fe clusters and decompose into base Cu and α-Fe precipitated phases under certain conditions. A few of α-Fe precipitates was observed in the copper near Cu/Fe interfaces of cold-drawn CCS wires, with 1-5 nm in size. A number of α-Fe precipitates of 1-20 nm in size can be detected in copper near Cu/Fe interfaces of CCS wires annealed at 850°C. When annealing temperature was less than 750°C, the resistivity of CCS wires annealed was lower than that of cold-drawn CCS wires. However, when annealing temperature was above 750°C, the resistivity of CCS wires was greater than that of cold-drawn CCS wires and increased with rising the annealing temperature. The relationship between nanoscale α-Fe precipitation and resistivity of CCS wires has been well discussed.

Changes in the Spectral Features of Zinc Phthalocyanine Induced by Nitrogen Dioxide Gas in Solution and in Solid Polymer Nanofiber Media.

PubMed

Zugle, Ruphino; Tetteh, Samuel

2017-03-01

The changes in the spectral features of zinc phthalocyanine in the visible domain as a result of its interaction with nitrogen dioxide gas were assessed in this work. This was done both in solution and when the phthalocyanine was incorporated into a solid polystyrene polymer nanofiber matrix. The spectral changes were found to be spontaneous and marked in both cases suggesting a rapid response criterion for the detection of the gas. In particular, the functionalised nano-fabric material could serve as a practical fire alarm system as it rapidly detects the nitrogen dioxide gas generated during burning.

Reduction of Plutonium in Acidic Solutions by Mesoporous Carbons

DOE PAGES

Parsons-Moss, Tashi; Jones, Stephen; Wang, Jinxiu; ...

2015-12-19

Batch contact experiments with several porous carbon materials showed that carbon solids spontaneously reduce the oxidation state of plutonium in 1-1.5 M acid solutions, without significant adsorption. The final oxidation state and rate of Pu reduction varies with the solution matrix, and also depends on the surface chemistry and surface area of the carbon. It was demonstrated that acidic Pu(VI) solutions can be reduced to Pu(III) by passing through a column of porous carbon particles, offering an easy alternative to electrolysis with a potentiostat.

Effects of hydrogen on thermal creep behaviour of Zircaloy fuel cladding

NASA Astrophysics Data System (ADS)

Suman, Siddharth; Khan, Mohd Kaleem; Pathak, Manabendra; Singh, R. N.

2018-01-01

Zirconium alloys are extensively used for nuclear fuel cladding. Creep is one of the most likely degradation mechanisms for fuel cladding during reactor operating and repository conditions. Fuel cladding tubes undergo waterside corrosion during service and hydrogen is produced as a result of it-a fraction of which is picked up by cladding. Hydrogen remains in solid solution up to terminal solid solubility and it precipitates as brittle hydride phase in the zirconium metal matrix beyond this limiting concentration. Hydrogen, either in solid solution or as precipitated hydride, alters the creep behaviour of zirconium alloys. The present article critically reviews the influence of hydrogen on thermal creep behaviour of zirconium alloys, develops the systematic understanding of this multifaceted phenomenon, and delineates the thrust areas which require further investigations.

Simple method to assess stability of immobilized peptide ligands against proteases.

PubMed

Giudicessi, Silvana L; Salum, María L; Saavedra, Soledad L; Martínez-Ceron, María C; Cascone, Osvaldo; Erra-Balsells, Rosa; Camperi, Silvia A

2017-09-01

Although peptides are used as affinity chromatography ligands, they could be digested by proteases. Usually, peptide stability is evaluated in solution, which differs from the resin-bounded peptide behavior. Furthermore, the study of the degradation products requires purification steps before analysis. Here, we describe an easy method to assess immobilized peptide stability. Sample peptides were synthesized on hydroxymethylbenzamide-ChemMatrix resin. Peptidyl-resin beads were then incubated with solutions containing proteases. Peptides were detached from the solid support with ammonia vapor and analyzed by matrix-assisted laser desorption/ionization and electrospray ionization mass spectrometry, allowing the detection of the whole peptides as well as their C-terminal degradation products. The method allowed a fast evaluation of peptide ligand stability in solid phase towards proteases that may be present in the crude sample before their use as ligands in affinity chromatography. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd.

Microstructural and microchemical studies of phase stability in V-O solid solution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ghosh, Chanchal, E-mail: chanchal@igcar.gov.in

2017-02-15

Over the last couple of decades vanadium and V-based alloys have received significant attention as a potential structural material for fusion power applications because of their favourable mechanical properties under irradiation and at elevated temperatures. They are also considered as the advanced options of storage materials for hydrogen and its isotopes. However, the higher affinity of V for O, C and N poses critical challenges in its engineering applications since they lead to degradation of mechanical properties. They can further interact with the matrix to produce metallic oxy-carbo-nitride precipitates. To a certain limit, these precipitates are beneficial and can bemore » exploited to enhance the mechanical behaviour of the alloy through suitable microstructural design. However, this requires a prior knowledge of the interaction between the alloy and the impurity solutes. In the present work vanadium specific experiments have been designed and carried out to bring out the V-interstitial solute interaction by charging oxygen in the near surface region of vanadium. Microstructural and microchemical behaviour of the V-O solid solution has been studied through HRTEM (high resolution transmission electron microscopy) and HAADF (high angle annular dark field) coupled with EELS. Quantitative electron microscopy has been carried out to study structural modification of the alloy in atomic level caused by O charging. - Highlights: •Controlled experiments were carried out in pulsed laser ablation set-up to promote V-O interaction. • As a consequence of O dissolution, V transformed into a bct structure which is otherwise a bcc structure. •In V-O solid solution, dissolved O in the V matrix introduces significant amount of lattice strain. • Present work can be extended for introducing interstitial O in other pure transition metals and their alloys.« less

Polyimide Composites from 'Salt-Like' Solution Precursors

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Hou, Tan H.; Weiser, Erik S.; SaintClair, Terry L.

2001-01-01

Four NASA Langley-developed polyimide matrix resins, LaRC(TM)-IA, LaRC(TM)-IAX, LaRC(TM)-8515 and LaRC(TM)-PETI-5, were produced via a 'saltlike' process developed by Unitika Ltd. The salt-like solutions (65% solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC multipurpose tape machine. Process parameters were determined and composite panels fabricated. The temperature dependent volatile depletion rates, the thermal crystallization behavior and the resin rheology were characterized. Composite molding cycles were developed which consistently yielded well consolidated, void-free laminated parts. Composite mechanical properties such as the short beam shear strength; the longitudinal and transverse flexural strength and flexural modulus; the longitudinal compression strength and modulus; and the open hole compression strength and compression after impact strength were measured at room temperature and elevated temperatures. The processing characteristics and the composite mechanical properties of the four intermediate modulus carbon fiber/polyimide matrix composites were compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (30-35% solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of the polyimide composites.

Theoretical models for supercritical fluid extraction.

PubMed

Huang, Zhen; Shi, Xiao-Han; Jiang, Wei-Juan

2012-08-10

For the proper design of supercritical fluid extraction processes, it is essential to have a sound knowledge of the mass transfer mechanism of the extraction process and the appropriate mathematical representation. In this paper, the advances and applications of kinetic models for describing supercritical fluid extraction from various solid matrices have been presented. The theoretical models overviewed here include the hot ball diffusion, broken and intact cell, shrinking core and some relatively simple models. Mathematical representations of these models have been in detail interpreted as well as their assumptions, parameter identifications and application examples. Extraction process of the analyte solute from the solid matrix by means of supercritical fluid includes the dissolution of the analyte from the solid, the analyte diffusion in the matrix and its transport to the bulk supercritical fluid. Mechanisms involved in a mass transfer model are discussed in terms of external mass transfer resistance, internal mass transfer resistance, solute-solid interactions and axial dispersion. The correlations of the external mass transfer coefficient and axial dispersion coefficient with certain dimensionless numbers are also discussed. Among these models, the broken and intact cell model seems to be the most relevant mathematical model as it is able to provide realistic description of the plant material structure for better understanding the mass-transfer kinetics and thus it has been widely employed for modeling supercritical fluid extraction of natural matters. Copyright © 2012 Elsevier B.V. All rights reserved.

Laser performance of Coumarin 540A dye molecules in polymeric host media with different viscosities: From liquid solution to solid polymer matrix

DOE Office of Scientific and Technical Information (OSTI.GOV)

Costela, A.; Garcia-Moreno, I.; Barroso, J.

1998-01-01

Photophysical parameters and lasing properties of Coumarin 540A dye molecules are studied in solutions of increasing viscosity, from liquid solutions in 1,4-dioxane to solid solutions in poly(methyl methacrylate). The fluorescence quantum yield and lasing efficiencies decrease as the viscosity of the solution increases, reflecting the strong influence of the rigidity of the medium on the radiative processes. The photodegradation mechanisms acting on the fluorophores are analyzed by following the dependence of laser induced fluorescence and laser output on the number of pump laser pulses. The fluorescence redistribution after pattern photobleaching technique is used, and Fick{close_quote}s second law is applied tomore » study the diffusion of dye molecules in the highly viscous polymer solutions. The diffusion coefficients of the dye molecules as a function of the increased viscosity of the medium are determined. {copyright} {ital 1998 American Institute of Physics.}« less

Investigations of Some Liquid Matrixes for Analyte Quantification by MALDI

NASA Astrophysics Data System (ADS)

Moon, Jeong Hee; Park, Kyung Man; Ahn, Sung Hee; Lee, Seong Hoon; Kim, Myung Soo

2015-06-01

Sample inhomogeneity is one of the obstacles preventing the generation of reproducible mass spectra by MALDI and to their use for the purpose of analyte quantification. As a potential solution to this problem, we investigated MALDI with some liquid matrixes prepared by nonstoichiometric mixing of acids and bases. Out of 27 combinations of acids and bases, liquid matrixes could be produced from seven. When the overall spectral features were considered, two liquid matrixes using α-cyano-4-hydroxycinnamic acid as the acid and 3-aminoquinoline and N,N-diethylaniline as bases were the best choices. In our previous study of MALDI with solid matrixes, we found that three requirements had to be met for the generation of reproducible spectra and for analyte quantification: (1) controlling the temperature by fixing the total ion count, (2) plotting the analyte-to-matrix ion ratio versus the analyte concentration as the calibration curve, and (3) keeping the matrix suppression below a critical value. We found that the same requirements had to be met in MALDI with liquid matrixes as well. In particular, although the liquid matrixes tested here were homogeneous, they failed to display spot-to-spot spectral reproducibility unless the first requirement above was met. We also found that analyte-derived ions could not be produced efficiently by MALDI with the above liquid matrixes unless the analyte was sufficiently basic. In this sense, MALDI processes with solid and liquid matrixes should be regarded as complementary techniques rather than as competing ones.

Investigations of Some Liquid Matrixes for Analyte Quantification by MALDI.

PubMed

Moon, Jeong Hee; Park, Kyung Man; Ahn, Sung Hee; Lee, Seong Hoon; Kim, Myung Soo

2015-10-01

Sample inhomogeneity is one of the obstacles preventing the generation of reproducible mass spectra by MALDI and to their use for the purpose of analyte quantification. As a potential solution to this problem, we investigated MALDI with some liquid matrixes prepared by nonstoichiometric mixing of acids and bases. Out of 27 combinations of acids and bases, liquid matrixes could be produced from seven. When the overall spectral features were considered, two liquid matrixes using α-cyano-4-hydroxycinnamic acid as the acid and 3-aminoquinoline and N,N-diethylaniline as bases were the best choices. In our previous study of MALDI with solid matrixes, we found that three requirements had to be met for the generation of reproducible spectra and for analyte quantification: (1) controlling the temperature by fixing the total ion count, (2) plotting the analyte-to-matrix ion ratio versus the analyte concentration as the calibration curve, and (3) keeping the matrix suppression below a critical value. We found that the same requirements had to be met in MALDI with liquid matrixes as well. In particular, although the liquid matrixes tested here were homogeneous, they failed to display spot-to-spot spectral reproducibility unless the first requirement above was met. We also found that analyte-derived ions could not be produced efficiently by MALDI with the above liquid matrixes unless the analyte was sufficiently basic. In this sense, MALDI processes with solid and liquid matrixes should be regarded as complementary techniques rather than as competing ones.

Microstructure and Hardness of Mg - 9Li - 6Al Alloy After Different Variants of Solid Solution Treatment

NASA Astrophysics Data System (ADS)

Zheng, Haipeng; Fei, Pengfei; Wu, Ruizhi; Hou, Legan; Zhang, Milin

2018-03-01

The microstructure and the hardness of cast magnesium alloy Mg - 9% Li - 6% Al are studied after a treatment for solid solution at 300, 350, and 450°C for 0.5 - 5 h. The phase composition of the alloy is represented by α-Mg, β-Li, thin-plate and faceted particles of an AlLi phase, and particles of a MgLi2Al θ-phase. The θ-phase dissolves in the matrix in the initial stage of the solution treatment, which causes growth in the hardness of the alloy. At a temperature above 350°C the AlLi phase dissolves giving way to short rod-like precipitates of a θ-phase, which remain steady in the process of solution treatment. The hardness of the alloy deceases in this stage for this reason.

Ceramic Matrix Composites by Liquid Infiltration

DTIC Science & Technology

1988-01-01

28 List of Tables Page Table I Solubility of ZrCl4 in Various Solvents-----------8 Table II Experimental Matrix of Precursor Formation -------- 10...unreactive, solvent. 1 The solubility of ZrCl4 in acetonitrile is approximately 25% by weight. Dissolution is accompanied by evolution of heat and the solution...is very fluid. Evaporation of the solvent yields an off-white solid residue which appears to be a one to two complex or adduct of ZrCl4 with CH3CN

Formation of soft magnetic high entropy amorphous alloys composites containing in situ solid solution phase

NASA Astrophysics Data System (ADS)

Wei, Ran; Sun, Huan; Chen, Chen; Tao, Juan; Li, Fushan

2018-03-01

Fe-Co-Ni-Si-B high entropy amorphous alloys composites (HEAACs), which containing high entropy solid solution phase in amorphous matrix, show good soft magnetic properties and bending ductility even in optimal annealed state, were successfully developed by melt spinning method. The crystallization phase of the HEAACs is solid solution phase with body centered cubic (BCC) structure instead of brittle intermetallic phase. In addition, the BCC phase can transformed into face centered cubic (FCC) phase with temperature rise. Accordingly, Fe-Co-Ni-Si-B high entropy alloys (HEAs) with FCC structure and a small amount of BCC phase was prepared by copper mold casting method. The HEAs exhibit high yield strength (about 1200 MPa) and good plastic strain (about 18%). Meanwhile, soft magnetic characteristics of the HEAs are largely reserved from HEAACs. This work provides a new strategy to overcome the annealing induced brittleness of amorphous alloys and design new advanced materials with excellent comprehensive properties.

The origin of ultrahigh piezoelectricity in relaxor-ferroelectric solid solution crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Fei; Zhang, Shujun; Yang, Tiannan

The discovery of ultrahigh piezoelectricity in relaxor-ferroelectric solid solution single crystals is a breakthrough in ferroelectric materials. A key signature of relaxor-ferroelectric solid solutions is the existence of polar nanoregions, a nanoscale inhomogeneity, that coexist with normal ferroelectric domains. Despite two decades of extensive studies, the contribution of polar nanoregions to the underlying piezoelectric properties of relaxor ferroelectrics has yet to be established. Here we quantitatively characterize the contribution of polar nanoregions to the dielectric/piezoelectric responses of relaxor-ferroelectric crystals using a combination of cryogenic experiments and phase-field simulations. The contribution of polar nanoregions to the room-temperature dielectric and piezoelectric propertiesmore » is in the range of 50–80%. A mesoscale mechanism is proposed to reveal the origin of the high piezoelectricity in relaxor ferroelectrics, where the polar nanoregions aligned in a ferroelectric matrix can facilitate polarization rotation. This mechanism emphasizes the critical role of local structure on the macroscopic properties of ferroelectric materials.« less

The origin of ultrahigh piezoelectricity in relaxor-ferroelectric solid solution crystals

DOE PAGES

Li, Fei; Zhang, Shujun; Yang, Tiannan; ...

2016-12-19

The discovery of ultrahigh piezoelectricity in relaxor-ferroelectric solid solution single crystals is a breakthrough in ferroelectric materials. A key signature of relaxor-ferroelectric solid solutions is the existence of polar nanoregions, a nanoscale inhomogeneity, that coexist with normal ferroelectric domains. Despite two decades of extensive studies, the contribution of polar nanoregions to the underlying piezoelectric properties of relaxor ferroelectrics has yet to be established. Here we quantitatively characterize the contribution of polar nanoregions to the dielectric/piezoelectric responses of relaxor-ferroelectric crystals using a combination of cryogenic experiments and phase-field simulations. The contribution of polar nanoregions to the room-temperature dielectric and piezoelectric propertiesmore » is in the range of 50–80%. A mesoscale mechanism is proposed to reveal the origin of the high piezoelectricity in relaxor ferroelectrics, where the polar nanoregions aligned in a ferroelectric matrix can facilitate polarization rotation. This mechanism emphasizes the critical role of local structure on the macroscopic properties of ferroelectric materials.« less

New strategy and easy fabrication of solid-state supercapacitor based on polypyrrole and nitrile rubber.

PubMed

Lee, Sangyool; Lee, Youngkwan; Cho, Mi-Suk; Nam, Jae-Do

2008-09-01

Solid state redox supercapacitors were fabricated using a solid polymer electrolyte, nitrile butadiene rubber (NBR)-KCI and chemically deposited polypyrrole (PPy) as the conducting polymer electrodes on both surfaces of a NBR film. The optimal conditions for the preparation of the PPy/NBR electrode were confirmed as functions of the uptake of pyrrole monomer into the NBR matrix as well as the immersion time in an oxidant solution. The morphology of the PPy-NBR-KCI capacitor was observed using scanning electron microscopy. The performance of the capacitors was characterized using a galvanostatic charge-discharge technique.

Calculation of the solvus temperature of metastable phases in the Al-Mg-Si alloys

NASA Astrophysics Data System (ADS)

Vasilyev, A. A.; Gruzdev, A. S.; Kuz'min, N. L.

2011-09-01

A procedure has been proposed for the self-consistent calculation of the solvus temperatures of metastable phase precipitates in Al-Mg-Si alloys and the specific energy of their interface with the aluminum matrix. The procedure is based on the results of experimental studies on the kinetics of formation of these precipitates during decomposition of supersaturated solid solutions of quenched Al-Mg-Si alloys, which were carried out by measuring the Young's modulus and electrical resistivity. On the basis of the obtained set of solvus temperatures of the β″-phase, an empirical formula has been proposed for calculating this temperature as a function of the chemical composition of the initial solid solution.

Atomistic Simulation of High-Density Uranium Fuels

DOE PAGES

Garcés, Jorge Eduardo; Bozzolo, Guillermo

2011-01-01

We apply an atomistic modeling approach to deal with interfacial phenomena in high-density uranium fuels. The effects of Si, as additive to Al or as U-Mo-particles coating, on the behavior of the Al/U-Mo interface is modeled by using the Bozzolo-Ferrante-Smith (BFS) method for alloys. The basic experimental features characterizing the real system are identified, via simulations and atom-by-atom analysis. These include (1) the trend indicating formation of interfacial compounds, (2) much reduced diffusion of Al into U-Mo solid solution due to the high Si concentration, (3) Si depletion in the Al matrix, (4) an unexpected interaction between Mo and Simore » which inhibits Si diffusion to deeper layers in the U-Mo solid solution, and (5) the minimum amount of Si needed to perform as an effective diffusion barrier. Simulation results related to alternatives to Si dispersed in the Al matrix, such as the use of C coating of U-Mo particles or Zr instead of the Al matrix, are also shown. Recent experimental results confirmed early theoretical proposals, along the lines of the results reported in this work, showing that atomistic computational modeling could become a valuable tool to aid the experimental work in the development of nuclear fuels.« less

Treatment of toxic metal aqueous solutions: encapsulation in a phosphate-calcium aluminate matrix.

PubMed

Fernández, J M; Navarro-Blasco, I; Duran, A; Sirera, R; Alvarez, J I

2014-07-01

Polyphosphate-modified calcium aluminate cement matrices were prepared by using aqueous solutions polluted with toxic metals as mixing water to obtain waste-containing solid blocks with improved management and disposal. Synthetically contaminated waters containing either Pb or Cu or Zn were incorporated into phosphoaluminate cement mortars and the effects of the metal's presence on setting time and mechanical performance were assessed. Sorption and leaching tests were also executed and both retention and release patterns were investigated. For all three metals, high uptake capacities as well as percentages of retention larger than 99.9% were measured. Both Pb and Cu were seen to be largely compatible with this cementitious matrix, rendering the obtained blocks suitable for landfilling or for building purposes. However, Zn spoilt the compressive strength values because of its reaction with hydrogen phosphate anions, hindering the development of the binding matrix. Copyright © 2014 Elsevier Ltd. All rights reserved.

Nature of diffraction fringes originating in the core of core-shell nanoparticle Cu/SiO2 and formation mechanism of the structures

NASA Astrophysics Data System (ADS)

Radnaev, A. R.; Kalashnikov, S. V.; Nomoev, A. V.

2016-05-01

This article is devoted to the analysis of the reasons for the occurrence of diffraction fringes in the cores of the core-shell nanoparticles Cu/SiO2. Moiré and diffraction fringes are observed while studying the nanoparticle cores under a transmission electron microscope. The formation of diffraction fringes is closely connected to the mechanism of nanoparticle formation under study and appears to be its consequence, letting us develop a hypothesis of metastable phase formation in nanoparticle cores. In our opinion, the emergence of diffraction fringes in cores of copper is connected to clasterisation in solid solution oversaturated with silicon α-Cu with the diffused interphase state. Only copper and oxygen (oxygen is presented as oxides in such types of copper as M0 - up to 0.01%; and M1 - up to 0.03%), Copper and silicon with oxygen in a stoichiometric proportion that is only sufficient for silicon dioxide formation (SiO2), Copper and silicon with oxygen in an amount that is sufficient not only for silicon dioxide formation, but also for the dissolution of silicon in the α-Cu solid solution, The amount of silicon in the alloy is not sufficient for the total fixation of oxygen contained in copper, Copper, oxygen and silicon whose contamination is greater than 8 wt.%. In the first case, the top-cut of oxygen in α-Cu solid solution is 0.03% at the temperature of 1066 °C. At slow cooling, secondary recrystallisation leads to the formation of equilibrium Cu2O on the line of the ultimate solubility (Figure 1a - line of maximum solubility of oxygen in copper). In the case of fast cooling fixation of oversaturated, single-phase, non-equilibrium α-Cu, solid solution (heat-treated) takes place, which contains saluted oxygen in an interstice crystal lattice of copper.Room temperature for nonferrous alloys (metals) is sufficient for the diffusive mobility of atoms, but insufficient for the formation of an equilibrium phase and stable phase of Cu2O. This is why diffusion of oxygen atoms in certain areas (clusters) with their increased diffusion of oxygen atoms in certain areas (clusters) with their increased number has been suggested [4]. At the same time, there is a boundary between the stable phase of α-Cu and 'pre-precipitations' containing oxygen, but not having the full value oxide: red copper ore, Cu2O (Figure 1b - solvus of suggested metastable phase). In this case, diffraction fringes can be treated as 'pre-precipitations' in the form of Guinier-Preston zones with diffuse interfaces and a stable α-Cu phase.In the second case, all oxygen and silicon after condensation and crystallisation are fixed in the form of amorphous SiO2 on the core surface of copper. As far as there are no atoms of saluted oxygen or silicon in copper, there are no conditions for the formation of non-equilibrium structures. Consequently, the diffraction pattern of nanoparticle cores is not observed (Figure 2a).In the third case, in the presence of quite a large amount of silicon in the stoichiometric drop, the process of copper oxide formation is not possible, because all the oxygen is used for the production of silicon dioxide since the sensitivity of oxygen to silicon is higher than to copper. This can be explained by the difference in Gibbs energy for the oxidising reaction of components. At the temperature of 25 °C it is 29.0 J/(g mol) - for copper, and 80.8 J/(g mol) for silicon. Silicon dioxide occurring due to the oxygen content in copper will be displaced on the surface of the drop in the form of ash, forming the SiO2 shell [24]. The reason lies in the lower specific density of silicon (approximately 2.2 g/cm3) compared to copper (8.92 g/cm3). This is why, in our case, it is appropriate to study the system where there is no influence of oxygen on the crystallisation of the Cu-Si system [5]. In the cores of such nanoparticles, prominent diffraction fringes can be observed in the α-Cu core (Figure 3b).Analysis of the Cu-Si phase diagram (Figure 3) shows that the maximum solubility of silicon α-Cu at the temperature 552 °C comprises 4.65 wt.% Si. This part of the Cu-Si phase diagram containing up to 8 wt.% silicon represents a classical example of the well-studied phase diagram of Al-Cu components, with the formation of Guinier-Preston zones in the quenched aluminium alloy [25].Single-phase solid solution of silicon α-Cu is fixed at fast cooling in our case. During its formation, cooling and natural ageing of the nanoparticle core, and redistribution of silicon into certain areas, takes place, forming metastable clusters in the matrix with high silicon content. They seem to be 'pre-precipitations' of the γ-phase of copper, though they really are not. In our opinion, diffraction fringes observed in these particles appear to be metastable phases according to Guinier-Preston zone type, i.e. α-Cu area with excessive silicon content.For nonferrous alloys, room temperature is sufficient for diffusive mobility of atoms of the saluted component [19]. Clusters are formed both at the time of cooling and in the long-term process (i.e. natural ageing). Provided that it is not a new phase, but rather the area of the initial matrix α-Cu solid solution enriched with dissolved silicon, such areas may be treated as Guinier-Preston zones. In contrast to intermediate phases with qualitatively new structures, characterised by their own lattices, Guinier-Preston zones have the same lattice as the matrix solution, but are deformed because of the difference in the atomic diameters of the solute and solvent. There is no clear boundary between the zone and solid solution by which it is surrounded. Compared to concentration fluctuations that appear continuously and are diffused by thermal motion, Guinier-Preston zones are stable for a long time (at low temperatures, for an intermediate amount of time). Experiments have shown that, with the increase of ageing duration, zone sizes are also increased. Furthermore, larger zones grow due to dissolution of the smaller ones, i.e. the same way as in coagulation of crystal grains in the solid state (i.e. collective crystallisation) [19]. The number of the zones at the given ageing temperature does not depend on the alloy composition.In some alloys, Guinier-Preston zones appear immediately after heat treatment or even during the cooling after heat treatment. At the same time, intermediate phases and stable phases appear after the incubation interval. All these facts show that Guinier-Preston zones are different to intermediate and stable phases. This is why Guinier-Preston zones are often called 'pre-precipitations' to differentiate them from real precipitations of intermediate and stable phases with a qualitatively new structure [19].Unlike such a structured approach that treats Guinier-Preston zones as 'pre-precipitations' from a thermodynamic point of view, they can be treated as independent stable phases, intermediate between the matrix solution and the stable phase. Consequently, these zones can be treated as the second phase that is in metastable equilibrium with the matrix solution.Moreover, a Guinier-Preston zone in the dual Cu-Si system with limited solubility of silicon in solid state can have its own line limit of solubility km (Figure 3). Metastable phases with a high content of silicon in the α-Cu matrix crystalline lattice appear below this line.Provided that the Guinier-Preston zone is treated as a phase, at the moment of its origin, the change of the free energy of the alloy is as follows: ΔU = -ΔUtot + ΔUsurf + ΔUel (Utot - total energy of the system, Usurf - surface energy of the crystal, Uel - elastic energy component). Because of the coherence property of the zone and the matrix, the ΔUsurf component can be neglected as its value is very small. Then, at relatively high oversaturation, the energy barrier for the origin of the Guinier-Preston zone should be relatively small, which explains the occurrence of clusters immediately after heat treatment or even at the moment of cooling and following natural ageing.The fact that Guinier-Preston zones can easily appear throughout the whole volume of the matrix solid solution and give the structure of equable decay with high density is of high practical value for us (Figure 2b).Thus, diffraction fringes in copper cores of core-shell nanoparticles should be treated as the second metastable phase, which is in equilibrium with the matrix solid solution. Similar to the exfoliation curve km in the solid solution α-Cu, the solvus curve for γ-Cu with intermediate 'pre-precipitations' can be built. The structure of the boundary with the matrix differentiates Guinier-Preston zones from other intermediate phases. These zones are fully coherent extractions, which is why their boundary with the matrix is poorly defined.As the rate accuracy of basal spacing with the method of electronic diffraction does not exceed 1 Å, according to the data it is not possible to evaluate accurately the change dα-Cu in diffraction fringes of the nanoparticle core; phase nonuniformity of structures has been suggested [26]. This is why it is necessary to treat such structures as solid solutions of α-Cu matrix, with the presence of metastable phases with the deformed crystal lattice.In the fourth case, formation of core-shell nanoparticle Cu/SiO2 happens much like in the third case, but due to the fact the amount of silicon is insufficient for the total fixation of oxygen and copper, a transition zone containing Cu2O is formed. Moiré in such particles are observed at the possible placing of double diffraction from two or more crystals of solid solution α-Cu (Figure 4a) [3]. The nanoparticle according to SAED analysis is very much like a 'sandwich': core α-Cu (Figure 4b, basal spacing d(111) ≈ 2.0 Å, corresponding to the tabular data for Cu), transition zone - copper oxide Cu2O (Figure 5a, basal spacing d(111) ≈ 2.4 Å) and shell - amorphous silicon dioxide, according to the EDAX data, the content of oxygen in this area is greater than 12% [11]. High copper oxide (CuO) was discovered only on the surface of the nanoparticle shell SiO2 (Figure 5b, basal spacing d(111) ≈ 2.5 Å).In the fifth case, when the silicon content is from 8.3-8.5 wt.% to 13 wt.%, copper with silicon in solid state at room temperature forms a continuous series of solid solutions of copper α, γ, ɛ and η. Silicon containing more than 13 wt.% copper undergoes eutectic decomposition only at (η″ + Si) [5]; structurally, such a solution contains eutectics in eutectics. In the obtained powder of nanoparticles, there are no modifications of solid solutions of copper, except for α-Cu.

Fungal nanoscale metal carbonates and production of electrochemical materials.

PubMed

Li, Qianwei; Gadd, Geoffrey Michael

2017-09-01

Fungal biomineralization of carbonates results in metal removal from solution or immobilization within a solid matrix. Such a system provides a promising method for removal of toxic or valuable metals from solution, such as Co, Ni, and La, with some carbonates being of nanoscale dimensions. A fungal Mn carbonate biomineralization process can be applied for the synthesis of novel electrochemical materials. © 2017 The Authors. Microbial Biotechnology published by John Wiley & Sons Ltd and Society for Applied Microbiology.

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

PubMed Central

Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

2018-01-01

Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

Dispersoid reinforced alloy powder and method of making

DOEpatents

Anderson, Iver E [Ames, IA; Terpstra, Robert L [Ames, IA

2012-06-12

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomized particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.

Dispersoid reinforced alloy powder and method of making

DOEpatents

Anderson, Iver E.; Terpstra, Robert L.

2010-04-20

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomized particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.

Capillary-Channeled Polymer (C-CP) Fibers as a Stationary Phase for Sample Clean-Up of Protein Solutions for Matrix-Assisted Laser/Desorption Ionization Mass Spectrometry

NASA Astrophysics Data System (ADS)

Manard, Benjamin T.; Marcus, R. Kenneth

2012-08-01

Capillary-channeled polymer (C-CP) fibers are employed in a micropipette tip format to affect a stationary phase for the solid phase extraction (SPE) of proteins from buffer solutions prior to MALDI-MS analysis. Proteins readily adsorb to the polypropylene (PP) C-CP fibers while buffer species are easily washed off the tips using DI-H2O. Elution of the solutes is achieved with an aliquot of 50:50 ACN:H2O, which is compatible with the subsequent spotting on the MALDI target with the matrix solution. Lysozyme and cytochrome c are used as test species, with a primary buffer composition of 100 mM Tris-HCl. In this case, direct MALDI-MS produces no discernible protein signals. SPE on the C-CP fibers yields high fidelity mass spectra for 1 μL sample volumes. Limits of detection for cytochrome c in 100 mM Tris-HCl are on the order of 40 nM. Extraction of cytochrome c from buffer concentrations of up to 1 M Tris-HCl, provides signal recoveries that are suppressed by only ~50 % versus neat protein solutions. Finally, extraction of 3.1 μM cytochrome c from a synthetic urine matrix exhibits excellent recovery.

Tribological Properties of Aluminium Alloy Composites Reinforced with Multi-Layer Graphene—The Influence of Spark Plasma Texturing Process

PubMed Central

Kostecki, Marek; Woźniak, Jarosław; Cygan, Tomasz; Petrus, Mateusz; Olszyna, Andrzej

2017-01-01

Self-lubricating composites are designed to obtain materials that reduce energy consumption, improve heat dissipation between moving bodies, and eliminate the need for external lubricants. The use of a solid lubricant in bulk composite material always involves a significant reduction in its mechanical properties, which is usually not an optimal solution. The growing interest in multilayer graphene (MLG), characterised by interesting properties as a component of composites, encouraged the authors to use it as an alternative solid lubricant in aluminium matrix composites instead of graphite. Aluminium alloy 6061 matrix composite reinforced with 2–15 vol % of MLG were synthesised by the spark plasma sintering process (SPS) and its modification, spark plasma texturing (SPT), involving deformation of the pre-sintered body in a larger diameter matrix. It was found that the application of the SPT method improves the density and hardness of the composites, resulting in improved tribological properties, particularly in the higher load regime. PMID:28796172

The principle of minimal episteric distortion of the water matrix and its steering role in protein folding

NASA Astrophysics Data System (ADS)

Fernández, Ariel

2013-08-01

A significant episteric ("around a solid") distortion of the hydrogen-bond structure of water is promoted by solutes with nanoscale surface detail and physico-chemical complexity, such as soluble natural proteins. These structural distortions defy analysis because the discrete nature of the solvent at the interface is not upheld by the continuous laws of electrostatics. This work derives and validates an electrostatic equation that governs the episteric distortions of the hydrogen-bond matrix. The equation correlates distortions from bulk-like structural patterns with anomalous polarization components that do not align with the electrostatic field of the solute. The result implies that the interfacial energy stored in the orthogonal polarization correlates with the distortion of the water hydrogen-bond network. The result is validated vis-à-vis experimental data on protein interfacial thermodynamics and is interpreted in terms of the interaction energy between the electrostatic field of the solute and the dipole moment induced by the anomalous polarization of interfacial water. Finally, we consider solutes capable of changing their interface through conformational transitions and introduce a principle of minimal episteric distortion (MED) of the water matrix. We assess the importance of the MED principle in the context of protein folding, concluding that the native fold may be identified topologically with the conformation that minimizes the interfacial tension or disruption of the water matrix.

[Multiply upconversion emission in oxyfluoride ceramics].

PubMed

Xiao, Si-guo; Yang, Xiao-liang; Liu, Zhen-wei

2003-02-01

Oxyfluoride ceramics with the host composition of SiO2 and PbF2 have been prepared. X-ray diffraction analysis of the ceramics revealed that fluoride type beta-PbF2 solid solution regions are precipitated in the glass matrix. Rare earth ions in the beta-PbF2 solid solution show highly efficient upconversion performance due to the very small multi-phonon relaxation rates. Eight upconversion emission bands whose central wavelength are 846, 803, 665, 549, 523, 487, 456 and 411 nm have been observed when the sample was excited with 930 nm diode light. Four possible energy transfer processes between Er3+ and Yb3+ cause the electronic population of high energy level of Er3+ and realize the abound upconversion luminescence bands.

Dynamic transverse shear modulus for a heterogeneous fluid-filled porous solid containing cylindrical inclusions

NASA Astrophysics Data System (ADS)

Song, Yongjia; Hu, Hengshan; Rudnicki, John W.; Duan, Yunda

2016-09-01

An exact analytical solution is presented for the effective dynamic transverse shear modulus in a heterogeneous fluid-filled porous solid containing cylindrical inclusions. The complex and frequency-dependent properties of the dynamic shear modulus are caused by the physical mechanism of mesoscopic-scale wave-induced fluid flow whose scale is smaller than wavelength but larger than the size of pores. Our model consists of three phases: a long cylindrical inclusion, a cylindrical shell of poroelastic matrix material with different mechanical and/or hydraulic properties than the inclusion and an outer region of effective homogeneous medium of laterally infinite extent. The behavior of both the inclusion and the matrix is described by Biot's consolidation equations, whereas the surrounding effective medium which is used to describe the effective transverse shear properties of the inner poroelastic composite is assumed to be a viscoelastic solid whose complex transverse shear modulus needs to be determined. The determined effective transverse shear modulus is used to quantify the S-wave attenuation and velocity dispersion in heterogeneous fluid-filled poroelastic rocks. The calculation shows the relaxation frequency and relative position of various fluid saturation dispersion curves predicted by this study exhibit very good agreement with those of a previous 2-D finite-element simulation. For the double-porosity model (inclusions having a different solid frame than the matrix but the same pore fluid as the matrix) the effective shear modulus also exhibits a size-dependent characteristic that the relaxation frequency moves to lower frequencies by two orders of magnitude if the radius of the cylindrical poroelastic composite increases by one order of magnitude. For the patchy-saturation model (inclusions having the same solid frame as the matrix but with a different pore fluid from the matrix), the heterogeneity in pore fluid cannot cause any attenuation in the transverse shear modulus at all. A comparison with the case of spherical inclusions illustrates that the transverse shear modulus for the cylindrical inclusion exhibits more S-wave attenuation than spherical inclusions.

Ti2Al(C, N) Solid Solution Reinforcing TiAl-Based Composites: Evolution of a Core-Shell Structure, Interfaces, and Mechanical Properties.

PubMed

Song, Xiaojie; Cui, Hongzhi; Han, Ye; Ding, Lei; Song, Qiang

2018-05-16

In this work, Ti 2 Al(C, N) solid solution with lamellar structure-enhanced TiAl matrix composites was synthesized by vacuum arc melting, using bulk g-C 3 N 4 , Ti, and Al powders as raw materials. The phases, microstructures, interfaces, and mechanical properties were investigated. MAX phase of Ti 2 Al(C, N) solid solution with lamellar structure was formed. During the melting process, first, C 3 N 4 reacted with Ti to form Ti(C, N) by Ti + C 3 N 4 → Ti(C, N). Then Ti 2 Al(C, N) was formed by a peritectic reaction of TiAl(l) + Ti(C, N)(s) → Ti 2 Al(C, N). C 3 N 4 is the single reactant that provides C and N simultaneously to final product of Ti 2 Al(C, N). The interfaces of TiAl//Ti 2 Al(C, N) and Ti 2 Al(C, N)//Ti(C, N) display perfect orientation relationships with low misfit values. The microhardness, compressive strength, and strain of best-performing TiAl-10 mol % Ti 2 Al(C, N) composite were improved by 45%, 55.7%, and 50% compared with the TiAl alloy, respectively. Uniformly distributed Ti 2 Al(C, N) and unreacted Ti(C, N) particles contributed to the grain refinement and reinforcement of the TiAl matrix. Laminated tearing, particle pull-out, and the crack-arresting of Ti 2 Al(C, N) are crucial for the improvement in compressive strength and plasticity of the composites.

Steady State Transportation Cooling in Porous Media Under Local, Non-Thermal Equilibrium Fluid Flow

NASA Technical Reports Server (NTRS)

Rodriquez, Alvaro Che

2002-01-01

An analytical solution to the steady-state fluid temperature for 1-D (one dimensional) transpiration cooling has been derived. Transpiration cooling has potential use in the aerospace industry for protection against high heating environments for re-entry vehicles. Literature for analytical treatments of transpiration cooling has been largely confined to the assumption of thermal equilibrium between the porous matrix and fluid. In the present analysis, the fundamental fluid and matrix equations are coupled through a volumetric heat transfer coefficient and investigated in non-thermal equilibrium. The effects of varying the thermal conductivity of the solid matrix and the heat transfer coefficient are investigated. The results are also compared to existing experimental data.

High temperature coercive field behavior of Fe-Zr powder

NASA Astrophysics Data System (ADS)

Mishra, Debabrata; Perumal, A.; Srinivasan, A.

2009-04-01

We report the investigation of high temperature coercive field behavior of Fe80Zr20 nanocrystalline alloy powder having two-phase microstructure prepared by mechanical alloying process. Thermomagnetization measurement shows the presence of two different magnetic phase transitions corresponding to the amorphous matrix and nonequilibrium Fe(Zr) solid solution. Temperature dependent coercivity exhibits a sharp increase in its value close to the Curie temperature of the amorphous matrix. This feature is attributed to the loss of intergranular ferromagnetic exchange coupling between the nanocrystallites due to the paramagnetic nature of the amorphous matrix. The temperature dependent coercive field behavior is ascribed to the variations in both the effective anisotropy and the exchange stiffness constant with temperature.

Nanocrystal-polymer nanocomposite electrochromic device

DOEpatents

Milliron, Delia; Runnerstrom, Evan; Helms, Brett; Llordes, Anna; Buonsanti, Raffaella; Garcia, Guillermo

2015-12-08

Described is an electrochromic nanocomposite film comprising a solid matrix of an oxide based material, the solid matrix comprising a plurality of transparent conducting oxide (TCO) nanostructures dispersed in the solid matrix and a lithium salt dispersed in the solid matrix. Also described is a near infrared nanostructured electrochromic device having a functional layer comprising the electrochromic nanocomposite film.

Liquid electrode plasma-optical emission spectrometry combined with solid-phase preconcentration for on-site analysis of lead.

PubMed

Barua, Suman; Rahman, Ismail M M; Alam, Iftakharul; Miyaguchi, Maho; Sawai, Hikaru; Maki, Teruya; Hasegawa, Hiroshi

2017-08-15

A relatively rapid and precise method is presented for the determination of lead in aqueous matrix. The method consists of analyte quantitation using the liquid electrode plasma-optical emission spectrometry (LEP-OES) coupled with selective separation/preconcentration by solid-phase extraction (SPE). The impact of operating variables on the retention of lead in SPEs such as pH, flow rate of the sample solution; type, volume, flow rate of the eluent; and matrix effects were investigated. Selective SPE-separation/preconcentration minimized the interfering effect due to manganese in solution and limitations in lead-detection in low-concentration samples by LEP-OES. The LEP-OES operating parameters such as the electrical conductivity of sample solution; applied voltage; on-time, off-time, pulse count for applied voltage; number of measurements; and matrix effects have also been optimized to obtain a distinct peak for the lead at λ max =405.8nm. The limit of detection (3σ) and the limit of quantification (10σ) for lead determination using the technique were found as 1.9 and 6.5ng mL -1 , respectively. The precision, as relative standard deviation, was lower than 5% at 0.1μg mL -1 Pb, and the preconcentration factor was found to be 187. The proposed method was applied to the analysis of lead contents in the natural aqueous matrix (recovery rate:>95%). The method accuracy was verified using certified reference material of wastewaters: SPS-WW1 and ERM-CA713. The results from LEP-OES were in good agreement with inductively coupled plasma optical emission spectrometry measurements of the same samples. The application of the method is rapid (≤5min, without preconcentration) with a reliable detection limit at trace levels. Copyright © 2017 Elsevier B.V. All rights reserved.

Theory for solubility in static systems

NASA Astrophysics Data System (ADS)

Gusev, Andrei A.; Suter, Ulrich W.

1991-06-01

A theory for the solubility of small particles in static structures has been developed. The distribution function of the solute in a frozen solid has been derived in analytical form for the quantum and the quasiclassical cases. The solubility at infinitesimal gas pressure (Henry's constant) as well as the pressure dependence of the solute concentration at elevated pressures has been found from the statistical equilibrium between the solute in the static matrix and the ideal-gas phase. The distribution function of a solute containing different particles has been evaluated in closed form. An application of the theory to the sorption of methane in the computed structures of glassy polycarbonate has resulted in a satisfactory agreement with experimental data.

Investigation of Different Colloidal Porous Silicon Solutions and Their Composite Solid Matrix Rods by Optical Techniques

NASA Astrophysics Data System (ADS)

Khan, M. Naziruddin; Aldalbahi, Ali; Almohammedi, Abdullah

2018-03-01

Colloidal porous silicon (PSi) in different solvents was synthesized by simple chemical etching. Colloidal solutions were then prepared using different quantities of silicon wafer pieces (Pcs) and chloroplatinic (Pt) acid in catalyst solution. The effect on the properties of the colloidal solutions and composite rods were investigated using various optical characterization techniques. Absorption and photoluminescence (PL) intensity of the colloidal PSi solutions are observed to depend on the quantity of wafer Pcs, the Pt-solution, and the porosity formation on the wafer surface. The morphological structure of the PSi in a solvent and the solid-rod environments were studied using field-emission scanning electron microscopy (FE-SEM) and were observed to have different structures. A mono-oriented structure of PSi exists in tetrahydrofuran, which has stereo orientation in dioxane and dimethylsulfoxide (approximately 5-8 nm as confirmed using high resolution transmission electron microscopy). Subsequently, some colloidal PSi solutions were directly embedded in three types of sol-gel-based matrices, silica, ormosils (or organically modified silica) and polymer, which easily generated solid rods. Spontaneous emission (SE) of the PSi solutions and their composite rods were examined using a high power picosecond 355 nm laser source. The emitted PL and SE signals of the colloidal PSi solutions were dependent on the Pt volume, nature of the solvent, quantity of Si wafer piece, and pumping energy. The response of SE signals from the PSi composites rods is an interesting phenomenon, and such nanocomposites may be used for future research on light amplification.

Investigation of Different Colloidal Porous Silicon Solutions and Their Composite Solid Matrix Rods by Optical Techniques

NASA Astrophysics Data System (ADS)

Khan, M. Naziruddin; Aldalbahi, Ali; Almohammedi, Abdullah

2018-07-01

Colloidal porous silicon (PSi) in different solvents was synthesized by simple chemical etching. Colloidal solutions were then prepared using different quantities of silicon wafer pieces (Pcs) and chloroplatinic (Pt) acid in catalyst solution. The effect on the properties of the colloidal solutions and composite rods were investigated using various optical characterization techniques. Absorption and photoluminescence (PL) intensity of the colloidal PSi solutions are observed to depend on the quantity of wafer Pcs, the Pt-solution, and the porosity formation on the wafer surface. The morphological structure of the PSi in a solvent and the solid-rod environments were studied using field-emission scanning electron microscopy (FE-SEM) and were observed to have different structures. A mono-oriented structure of PSi exists in tetrahydrofuran, which has stereo orientation in dioxane and dimethylsulfoxide (approximately 5-8 nm as confirmed using high resolution transmission electron microscopy). Subsequently, some colloidal PSi solutions were directly embedded in three types of sol-gel-based matrices, silica, ormosils (or organically modified silica) and polymer, which easily generated solid rods. Spontaneous emission (SE) of the PSi solutions and their composite rods were examined using a high power picosecond 355 nm laser source. The emitted PL and SE signals of the colloidal PSi solutions were dependent on the Pt volume, nature of the solvent, quantity of Si wafer piece, and pumping energy. The response of SE signals from the PSi composites rods is an interesting phenomenon, and such nanocomposites may be used for future research on light amplification.

Dispersoid reinforced alloy powder and method of making

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anderson, Iver E.; Terpstra, Robert L.

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomizedmore » particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.« less

Dispersoid reinforced alloy powder and method of making

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anderson, Iver E.; Terpstra, Robert L.

2017-10-10

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomizedmore » particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.« less

Extraction of acetanilides in rice using ionic liquid-based matrix solid phase dispersion-solvent flotation.

PubMed

Zhang, Liyuan; Wang, Changyuan; Li, Zuotong; Zhao, Changjiang; Zhang, Hanqi; Zhang, Dongjie

2018-04-15

Ionic liquid-based matrix solid phase dispersion-solvent flotation coupled with high performance liquid chromatography was developed for the determination of the acetanilide herbicides, including metazachlor, propanil, alachlor, propisochlor, pretilachlor, and butachlor in rice samples. Some experimental parameters, including the type of dispersant, the mass ratio of dispersant to sample, pH of sample solution, the type of extraction solvent, the type of ionic liquid, flotation time, and flow rate of N 2 were optimized. The average recoveries of the acetanilide herbicides at spiked concentrations of 50, 125, and 250 µg/kg ranged from 89.4% to 108.7%, and relative standard deviations were equal to or lower than 7.1%, the limits of quantification were in the range of 38.0 to 84.7 µg/kg. Copyright © 2017 Elsevier Ltd. All rights reserved.

Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials

DOE PAGES

Gao, Jun; Manard, Benjamin Thomas; Castro, Alonso; ...

2017-02-02

Advances in sample nebulization and injection technology have significantly reduced the volume of solution required for trace impurity analysis in plutonium and uranium materials. Correspondingly, we have designed and tested a novel chip-based microfluidic platform, containing a 100-µL or 20-µL solid-phase microextraction column, packed by centrifugation, which supports nuclear material mass and solution volume reductions of 90% or more compared to standard methods. Quantitative recovery of 28 trace elements in uranium was demonstrated using a UTEVA chromatographic resin column, and trace element recovery from thorium (a surrogate for plutonium) was similarly demonstrated using anion exchange resin AG MP-1. Of ninemore » materials tested, compatibility of polyvinyl chloride (PVC), polypropylene (PP), and polytetrafluoroethylene (PTFE) chips with the strong nitric acid media was highest. Finally, the microcolumns can be incorporated into a variety of devices and systems, and can be loaded with other solid-phase resins for trace element assay in high-purity metals.« less

Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gao, Jun; Manard, Benjamin Thomas; Castro, Alonso

Advances in sample nebulization and injection technology have significantly reduced the volume of solution required for trace impurity analysis in plutonium and uranium materials. Correspondingly, we have designed and tested a novel chip-based microfluidic platform, containing a 100-µL or 20-µL solid-phase microextraction column, packed by centrifugation, which supports nuclear material mass and solution volume reductions of 90% or more compared to standard methods. Quantitative recovery of 28 trace elements in uranium was demonstrated using a UTEVA chromatographic resin column, and trace element recovery from thorium (a surrogate for plutonium) was similarly demonstrated using anion exchange resin AG MP-1. Of ninemore » materials tested, compatibility of polyvinyl chloride (PVC), polypropylene (PP), and polytetrafluoroethylene (PTFE) chips with the strong nitric acid media was highest. Finally, the microcolumns can be incorporated into a variety of devices and systems, and can be loaded with other solid-phase resins for trace element assay in high-purity metals.« less

Molecular-Level Control of Ciclopirox Olamine Release from Poly(ethylene oxide)-Based Mucoadhesive Buccal Films: Exploration of Structure-Property Relationships with Solid-State NMR.

PubMed

Urbanova, Martina; Gajdosova, Marketa; Steinhart, Miloš; Vetchy, David; Brus, Jiri

2016-05-02

Mucoadhesive buccal films (MBFs) provide an innovative way to facilitate the efficient site-specific delivery of active compounds while simultaneously separating the lesions from the environment of the oral cavity. The structural diversity of these complex multicomponent and mostly multiphase systems as well as an experimental strategy for their structural characterization at molecular scale with atomic resolution were demonstrated using MBFs of ciclopirox olamine (CPX) in a poly(ethylene oxide) (PEO) matrix as a case study. A detailed description of each component of the CPX/PEO films was followed by an analysis of the relationships between each component and the physicochemical properties of the MBFs. Two distinct MBFs were identified by solid-state NMR spectroscopy: (i) at low API (active pharmaceutical ingredient) loading, a nanoheterogeneous solid solution of CPX molecularly dispersed in an amorphous PEO matrix was created; and (ii) at high API loading, a pseudoco-crystalline system containing CPX-2-aminoethanol nanocrystals incorporated into the interlamellar space of a crystalline PEO matrix was revealed. These structural differences were found to be closely related to the mechanical and physicochemical properties of the prepared MBFs. At low API loading, the polymer chains of PEO provided sufficient quantities of binding sites to stabilize the CPX that was molecularly dispersed in the highly amorphous semiflexible polymer matrix. Consequently, the resulting MBFs were soft, with low tensile strength, plasticity, and swelling index, supporting rapid drug release. At high CPX content, however, the active compounds and the polymer chains simultaneously cocrystallized, leaving the CPX to form nanocrystals grown directly inside the spherulites of PEO. Interfacial polymer-drug interactions were thus responsible not only for the considerably enhanced plasticity of the system but also for the exclusive crystallization of CPX in the thermodynamically most stable polymorphic form, Form I, which exhibited reduced dissolution kinetics. The bioavailability of CPX olamine formulated as PEO-based MBFs can thus be effectively controlled by inducing the complete dispersion and/or microsegregation and nanocrystallization of CPX olamine in the polymer matrix. Solid-state NMR spectroscopy is an efficient tool for exploring structure-property relationships in these complex pharmaceutical solids.

Coupling between magnetic and optical properties of stable Au-Fe solid solution nanoparticles

NASA Astrophysics Data System (ADS)

de Julián Fernández, C.; Mattei, G.; Paz, E.; Novak, R. L.; Cavigli, L.; Bogani, L.; Palomares, F. J.; Mazzoldi, P.; Caneschi, A.

2010-04-01

Au-Fe nanoparticles constitute one of the simplest prototypes of a multifunctional nanomaterial that can exhibit both magnetic and optical (plasmonic) properties. This solid solution, not feasible in the bulk phase diagram in thermal equilibrium, can be formed as a nanostructure by out-of-equilibrium processes. Here, the novel magnetic, optical and magneto-optical properties of ion-implanted Au-Fe solid solution nanoparticles dispersed in a SiO2 matrix are investigated and correlated. The surface plasmon resonance of the Au-Fe nanoparticles with almost equicomposition is strongly damped when compared to pure Au and to Au-rich Au-Fe nanoparticles. In all cases, the Au atoms are magnetically polarized, as measured by x-ray magnetic circular dichroism, and ferromagnetically coupled with Fe atoms. Although the chemical stability of Au-Fe nanoparticles is larger than that of Fe nanoparticles, both the magnetic moment per Fe atom and the order temperature are smaller. These results suggest that electronic and magnetic properties are more influenced by the hybridization of the electronic bands in the Au-Fe solid solution than by size effects. On the other hand, the magneto-optical transitions allowed in the vis-nIR spectral regions are very similar. In addition, we also observe, after studying the properties of thermally treated samples, that the Au-Fe alloy is stabilized, not by surface effects, but by the combination of the out-of-equilibrium nature of the ion implantation technique and by changes in the properties due to size effects.

Coupling between magnetic and optical properties of stable Au-Fe solid solution nanoparticles.

PubMed

de Julián Fernández, C; Mattei, G; Paz, E; Novak, R L; Cavigli, L; Bogani, L; Palomares, F J; Mazzoldi, P; Caneschi, A

2010-04-23

Au-Fe nanoparticles constitute one of the simplest prototypes of a multifunctional nanomaterial that can exhibit both magnetic and optical (plasmonic) properties. This solid solution, not feasible in the bulk phase diagram in thermal equilibrium, can be formed as a nanostructure by out-of-equilibrium processes. Here, the novel magnetic, optical and magneto-optical properties of ion-implanted Au-Fe solid solution nanoparticles dispersed in a SiO(2) matrix are investigated and correlated. The surface plasmon resonance of the Au-Fe nanoparticles with almost equicomposition is strongly damped when compared to pure Au and to Au-rich Au-Fe nanoparticles. In all cases, the Au atoms are magnetically polarized, as measured by x-ray magnetic circular dichroism, and ferromagnetically coupled with Fe atoms. Although the chemical stability of Au-Fe nanoparticles is larger than that of Fe nanoparticles, both the magnetic moment per Fe atom and the order temperature are smaller. These results suggest that electronic and magnetic properties are more influenced by the hybridization of the electronic bands in the Au-Fe solid solution than by size effects. On the other hand, the magneto-optical transitions allowed in the vis-nIR spectral regions are very similar. In addition, we also observe, after studying the properties of thermally treated samples, that the Au-Fe alloy is stabilized, not by surface effects, but by the combination of the out-of-equilibrium nature of the ion implantation technique and by changes in the properties due to size effects.

Matrix effects in inductively coupled plasma mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Xiaoshan

1995-07-07

The inductively coupled plasma is an electrodeless discharge in a gas (usually Ar) at atmospheric pressure. Radio frequency energy generated by a RF power source is inductively coupled to the plasma gas through a water cooled load coil. In ICP-MS the "Fassel" TAX quartz torch commonly used in emission is mounted horizontally. The sample aerosol is introduced into the central flow, where the gas kinetic temperature is about 5000 K. The aerosol is vaporized, atomized, excited and ionized in the plasma, and the ions are subsequently extracted through two metal apertures (sampler and skimmer) into the mass spectrometer. In ICP-MS,more » the matrix effects, or non-spectroscopic interferences, can be defined as the type of interferences caused by dissolved concomitant salt ions in the solution. Matrix effects can be divided into two categories: (1) signal drift due to the deposition of solids on the sampling apertures; and/or (2) signal suppression or enhancement by the presence of the dissolved salts. The first category is now reasonably understood. The dissolved salts, especially refractory oxides, tend to deposit on the cool tip of the sampling cone. The clogging of the orifices reduces the ion flow into the ICP-MS, lowers the pressure in the first stage of ICP-MS, and enhances the level of metal oxide ions. Because the extent of the clogging increases with the time, the signal drifts down. Even at the very early stage of the development of ICP-MS, matrix effects had been observed. Houk et al. found out that the ICP-MS was not tolerant to solutions containing significant amounts of dissolved solids.« less

Easy-Going On-Spectrometer Optimisation of Phase Modulated Homonuclear Decoupling Sequences in Solid-State NMR

NASA Astrophysics Data System (ADS)

Grimminck, Dennis L. A. G.; Vasa, Suresh K.; Meerts, W. Leo; Kentgens, P. M.

2011-06-01

A global optimisation scheme for phase modulated proton homonuclear decoupling sequences in solid-state NMR is presented. Phase modulations, parameterised by DUMBO Fourier coefficients, were optimized using a Covariance Matrix Adaptation Evolution Strategies algorithm. Our method, denoted EASY-GOING homonuclear decoupling, starts with featureless spectra and optimises proton-proton decoupling, during either proton or carbon signal detection. On the one hand, our solutions closely resemble (e)DUMBO for moderate sample spinning frequencies and medium radio-frequency (rf) field strengths. On the other hand, the EASY-GOING approach resulted in a superior solution, achieving significantly better resolved proton spectra at very high 680 kHz rf field strength. N. Hansen, and A. Ostermeier. Evol. Comput. 9 (2001) 159-195 B. Elena, G. de Paepe, L. Emsley. Chem. Phys. Lett. 398 (2004) 532-538

Matrix isolation technique for the study of some factors affecting the partitioning of trace elements. [using vibrational spectroscopy

NASA Technical Reports Server (NTRS)

Grzybowski, J. M.; Allen, R. O.

1974-01-01

The factors that affect the preferred positions of cations in ionic solid solutions were investigated utilizing vibrational spectroscopy. Solid solutions of the sulfate and chromate ions codoped with La(+3) and Ca(+2) in a KBr host lattice were examined as a function of the polyvalent cation concentration. The cation-anion pairing process was found to be random for Ca(+2), whereas the formation of La(+3)-SO4(-2) ion pairs with a C2 sub v bonding geometry is highly preferential to any type of La(+3)-CrO4(-2) ion pair formation. The relative populations of ion pair site configurations are discussed in terms of an energy-entropy competition model which can be applied to the partition of trace elements during magmatic processes.

Synthesis of Al₂Ca Dispersoids by Powder Metallurgy Using a Mg-Al Alloy and CaO Particles.

PubMed

Fujita, Junji; Umeda, Junko; Kondoh, Katsuyoshi

2017-06-28

The elemental mixture of Mg-6 wt %Al-1 wt %Zn-0.3 wt %Mn (AZ61B) alloy powder and CaO particles was consolidated by an equal-channel angular bulk mechanical alloying (ECABMA) process to form a composite precursor. Subsequently, the precursor was subjected to a heat treatment to synthesize fine Al₂Ca particles via a solid-state reaction between the Mg-Al matrix and CaO additives. Scanning electron microscopy-energy-dispersive spectroscopy (SEM-EDS) and electron probe micro-analysis on the precursor indicated that 4.7-at % Al atoms formed a supersaturated solid solution in the α-Mg matrix. Transmission electron microscopy-EDS and X-ray diffraction analyses on the AZ61B composite precursor with 10-vol % CaO particles obtained by heat treatment confirmed that CaO additives were thermally decomposed in the Mg-Al alloy, and the solid-soluted Ca atoms diffused along the α-Mg grain boundaries. Al atoms also diffused to the grain boundaries because of attraction to the Ca atoms resulting from a strong reactivity between Al and Ca. As a result, needle-like (Mg,Al)₂Ca intermetallics were formed as intermediate precipitates in the initial reaction stage during the heat treatment. Finally, the precipitates were transformed into spherical Al₂Ca particles by the substitution of Al atoms for Mg atoms in (Mg,Al)₂Ca after a long heat treatment.

Photo-physical properties and triplet-triplet absorption of platinum(II) acetylides in solid PMMA matrices

NASA Astrophysics Data System (ADS)

Glimsdal, Eirik; Westlund, Robert; Lindgren, Mikael

2009-05-01

Because of their strong nonlinear optical properties, Platinum(II) acetylides are investigated as potential chromophores for optical power limiting (OPL) applications. The strong excited state absorption and efficient intersystem crossing to the triplet states in these materials are desired properties for good OPL performance. We recently reported on OPL and photo-physical properties of Pt(II)-acetylide chromophores in solution, modified with thiophenyl or triazole groups. [R. Westlund et al. J. Mater. Chem. 18, 166 (2008); E. Glimsdal et al. Proc. SPIE 6740, 67400M (2007)] The chromophores were later incorporated into poly(methyl-methacrylate) (PMMA) glasses. A variety of doped organic solids were prepared, reaching concentrations of up to 13 wt% of the guest molecule. Raman spectra of the doped solid devices proved that the chemical structure of the nonlinear dyes remains intact upon the polymerization of the solid matrix. Luminescence spectra confirm that the basic photo-physical properties (absorption, emission and inter-system crossing) observed for the solute molecules in THF are maintained also in the solid state. In particular, the phosphorescence lifetime stays in the order of μs to ms, just as in the oxygen evacuated liquid samples. Also, the wavelength dependence and time-dynamics of the triplet absorption spectra of the dyes, dissolved in THF solution and dispersed in solid PMMA matrices, were investigated and compared. Ground state UV absorption spectra between 300 and 420 nm have corresponding broad band visible triplet-triplet absorption between 400 and 800 nm. The triplet state extinction coefficients were determined to be in the order of 104 M-1cm-1.

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review.

PubMed

Rahman, Md Musfiqur; Abd El-Aty, A M; Kim, Sung-Woo; Shin, Sung Chul; Shin, Ho-Chul; Shim, Jae-Han

2017-01-01

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

PubMed

Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

2016-05-01

A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Long-living nanobubbles of dissolved gas in aqueous solutions of salts and erythrocyte suspensions.

PubMed

Bunkin, Nikolai F; Ninham, Barry W; Ignatiev, Pavel S; Kozlov, Valery A; Shkirin, Alexey V; Starosvetskij, Artem V

2011-03-01

Results of experiments combining laser modulation interference microscopy and Mueller matrix scatterometry show that macroscopic scatterers of light are present in liquids free of external solid impurities. Experimental data on distilled water and aqueous NaCl solutions of various concentrations as well as physiological saline solution are reported. The experimental data can be interpreted by using a model of micron-scale clusters composed of polydisperse air nanobubbles having effective radii of 70-100 nm. Their concentration increases with the growth of ionic content. We hypothesize that under certain conditions those clusters of nanobubbles can affect the erythrocyte structure. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of poly(N-vinylpyrrolidone)-stabilized ZnO colloid nanoparticles

PubMed Central

Gutul, Tatyana; Condur, Nadejda; Ursaki, Veaceslav; Goncearenco, Evgenii; Vlazan, Paulina

2014-01-01

Summary We propose a method for the synthesis of a colloidal ZnO solution with poly(N-vinylpyrrolidone) (PVP) as stabilizer. Stable colloidal solutions with good luminescence properties are obtained by using PVP as stabilizer in the synthesis of ZnO nanoparticles by a sol–gel method assisted by ultrasound. Nanoparticles with sizes of 30–40 nm in a PVP matrix are produced as a solid product. The colloidal ZnO/PVP/methanol solution, apart from the most intense PL band at 356 nm coming from the PVP, exhibits a strong PL band at 376 nm (3.30 eV) which corresponds to the emission of the free exciton recombination in ZnO nanoparticles. PMID:24778966

Effects of fiber and interfacial layer architectures on the thermoplastic response of metal matrix composites

NASA Technical Reports Server (NTRS)

Pindera, Marek-Jerzy; Freed, Alan D.; Arnold, Steven M.

1992-01-01

Examined here is the effect of fiber and interfacial layer morphologies on thermal fields in metal matrix composites (MMCs). A micromechanics model based on an arbitrarily layered concentric cylinder configuration is used to calculate thermal stress fields in MMCs subjected to spatially uniform temperature changes. The fiber is modelled as a layered material with isotropic or orthotropic elastic layers, whereas the surrounding matrix, including interfacial layers, is treated as a strain-hardening, elastoplastic, von Mises solid with temperature-dependent parameters. The solution to the boundary-value problem of an arbitrarily layered concentric cylinder under the prescribed thermal loading is obtained using the local/global stiffness matrix formulation originally developed for stress analysis of multilayered elastic media. Examples are provided that illustrate how the morphology of the SCS6 silicon carbide fiber and the use of multiple compliant layers at the fiber/matrix interface affect the evolution of residual stresses in SiC/Ti composites during fabrication cool-down.

Method for molding ceramic powders

DOEpatents

Janney, Mark A.

1990-01-01

A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant for the metal-containing powder, and a monomer solution. The monomer solution includes at least one multifunctional monomer, a free-radical initiator, and an organic solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, whereafter the product may be sintered.

Method for molding ceramic powders

DOEpatents

Janney, M.A.

1990-01-16

A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant for the metal-containing powder, and a monomer solution. The monomer solution includes at least one multifunctional monomer, a free-radical initiator, and an organic solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, where after the product may be sintered.

Supercritical fluid precipitation of ketoprofen in novel structured lipid carriers for enhanced mucosal delivery--a comparison with solid lipid particles.

PubMed

Gonçalves, V S S; Matias, A A; Rodríguez-Rojo, S; Nogueira, I D; Duarte, C M M

2015-11-10

Structured lipid carriers based on mixture of solid lipids with liquid lipids are the second generation of solid lipid particles, offering the advantage of improved drug loading capacity and higher storage stability. In this study, structured lipid carriers were successfully prepared for the first time by precipitation from gas saturated solutions. Glyceryl monooleate (GMO), a liquid glycerolipid, was selected in this work to be incorporated into three solid glycerolipids with hydrophilic-lipophilic balance (HLB) ranging from 1 to 13, namely Gelucire 43/01™, Geleol™ and Gelucire 50/13™. In general, microparticles with a irregular porous morphology and a wide particle size distribution were obtained. The HLB of the individual glycerolipids might be a relevant parameter to take into account during the processing of solid:liquid lipid blends. As expected, the addition of a liquid lipid into a solid lipid matrix led to increased stability of the lipid carriers, with no significant modifications in their melting enthalpy after 6 months of storage. Additionally, Gelucire 43/01™:GMO particles were produced with different mass ratios and loaded with ketoprofen. The drug loading capacity of the structured lipid carriers increased as the GMO content in the particles increased, achieving a maximum encapsulation efficiency of 97% for the 3:1 mass ratio. Moreover, structured lipid carriers presented an immediate release of ketoprofen from its matrix with higher permeation through a mucous-membrane model, while solid lipid particles present a controlled release of the drug with less permeation capacity. Copyright © 2015. Published by Elsevier B.V.

Controlling the Localization of Liquid Droplets in Polymer Matrices by Evaporative Lithography.

PubMed

Zhao, Huaixia; Xu, Jiajia; Jing, Guangyin; Prieto-López, Lizbeth Ofelia; Deng, Xu; Cui, Jiaxi

2016-08-26

Localized inclusions of liquids provide solid materials with many functions, such as self-healing, secretion, and tunable mechanical properties, in a spatially controlled mode. However, a strategy to control the distribution of liquid droplets in solid matrices directly obtained from a homogeneous solution has not been reported thus far. Herein, we describe an approach to selectively localize liquid droplets in a supramolecular gel directly obtained from its solution by using evaporative lithography. In this process, the formation of droplet-embedded domains occurs in regions of free evaporation where the non-volatile liquid is concentrated and undergoes a phase separation to create liquid droplets prior to gelation, while a homogeneous gel matrix is formed in the regions of hindered evaporation. The different regions of a coating with droplet embedment patterns display different secretion abilities, enabling the control of the directional movement of water droplets. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Fei; Zhang, Shujun; Yang, Tiannan

The discovery of ultrahigh piezoelectricity in relaxor-ferroelectric solid solution single crystals is a breakthrough in ferroelectric materials. A key signature of relaxor-ferroelectric solid solutions is the existence of polar nanoregions, a nanoscale inhomogeneity, that coexist with normal ferroelectric domains. Despite two decades of extensive studies, the contribution of polar nanoregions to the underlying piezoelectric properties of relaxor ferroelectrics has yet to be established. Here we quantitatively characterize the contribution of polar nanoregions to the dielectric/piezoelectric responses of relaxor-ferroelectric crystals using a combination of cryogenic experiments and phase-field simulations. The contribution of polar nanoregions to the room-temperature dielectric and piezoelectric propertiesmore » is in the range of 50–80%. A mesoscale mechanism is proposed to reveal the origin of the high piezoelectricity in relaxor ferroelectrics, where the polar nanoregions aligned in a ferroelectric matrix can facilitate polarization rotation. This mechanism emphasizes the critical role of local structure on the macroscopic properties of ferroelectric materials.« less

Utilization of chemically treated municipal solid waste (spent coffee bean powder) as reinforcement in cellulose matrix for packaging applications.

PubMed

Thiagamani, Senthil Muthu Kumar; Nagarajan, Rajini; Jawaid, Mohammad; Anumakonda, Varadarajulu; Siengchin, Suchart

2017-11-01

As the annual production of the solid waste generable in the form of spent coffee bean powder (SCBP) is over 6 million tons, its utilization in the generation of green energy, waste water treatment and as a filler in biocomposites is desirable. The objective of this article is to analyze the possibilities to valorize coffee bean powder as a filler in cellulose matrix. Cellulose matrix was dissolved in the relatively safer aqueous solution mixture (8% LiOH and 15% Urea) precooled to -12.5°C. To the cellulose solution (SCBP) was added in 5-25wt% and the composite films were prepared by regeneration method using ethyl alcohol as a coagulant. Some SCBP was treated with aq. 5% NaOH and the composite films were also prepared using alkali treated SCBP as a filler. The films of composites were uniform with brown in color. The cellulose/SCBP films without and with alkali treated SCBP were characterized by FTIR, XRD, optical and polarized optical microscopy, thermogravimetric analysis (TGA) and tensile tests. The maximum tensile strength of the composite films with alkali treated SCBP varied between (106-149MPa) and increased with SCBP content when compared to the composites with untreated SCBP. The thermal stability of the composite was higher at elevated temperatures when alkali treated SCBP was used. Based on the improved tensile properties and photo resistivity, the cellulose/SCBP composite films with alkali treated SCBP may be considered for packaging and wrapping of flowers and vegetables. Copyright © 2017 Elsevier Ltd. All rights reserved.

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry.

PubMed

Grate, Jay W; Gonzalez, Jhanis J; O'Hara, Matthew J; Kellogg, Cynthia M; Morrison, Samuel S; Koppenaal, David W; Chan, George C-Y; Mao, Xianglei; Zorba, Vassilia; Russo, Richard E

2017-09-08

Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standards.

Curcumin-Eudragit® E PO solid dispersion: A simple and potent method to solve the problems of curcumin.

PubMed

Li, Jinglei; Lee, Il Woo; Shin, Gye Hwa; Chen, Xiguang; Park, Hyun Jin

2015-08-01

Using a simple solution mixing method, curcumin was dispersed in the matrix of Eudragit® E PO polymer. Water solubility of curcumin in curcumin-Eudragit® E PO solid dispersion (Cur@EPO) was greatly increased. Based on the results of several tests, curcumin was demonstrated to exist in the polymer matrix in amorphous state. The interaction between curcumin and the polymer was investigated through Fourier transform infrared spectroscopy and (1)H NMR which implied that OH group of curcumin and carbonyl group of the polymer involved in the H bonding formation. Cur@EPO also provided protection function for curcumin as verified by the pH challenge and UV irradiation test. The pH value influenced curcumin release profile in which sustained release pattern was revealed. Additionally, in vitro transdermal test was conducted to assess the potential of Cur@EPO as a vehicle to deliver curcumin through this alternative administration route. Copyright © 2015 Elsevier B.V. All rights reserved.

Rapid solidification of high-conductivity copper alloys. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Bloom, Theodore Atlas

1989-01-01

The main objective was to develop improved copper alloys of high strength and high thermal and electric conductivity. Chill block melt spinning was used to produce binary alloys of Cu-Cr and Cu-Zr, and ternary alloys of Cu-Cr-Ag. By quenching from the liquid state, up to 5 atomic percent of Cr and Zr were retained in metastable extended solid solution during the rapid solidification process. Eutectic solidification was avoided and the full strengthening benefits of the large volume fraction of precipitates were realized by subsequent aging treatment. The very low solid solubility of Cr and Zr in Cu result in a high conductivity Cu matrix strengthened by second phase precipitates. Tensile properties on as-cast and aged ribbons were measured at room and elevated temperatures. Precipitate coarsening of Cr in Cu was studied by changes in electrical resistance during aging. X-ray diffraction was used to measure the lattice parameter and the degree of supersaturation of the matrix. The microstructures were characterized by optical and electron microscopy.

Laser-induced oxidation of cholesterol observed during MALDI-TOF mass spectrometry.

PubMed

McAvey, Kevin M; Guan, Bing; Fortier, Chanel A; Tarr, Matthew A; Cole, Richard B

2011-04-01

Conditions for the detection of three odd-electron cholesterol oxidation peaks were determined and these peaks were shown to be artifacts of the matrix-assisted laser desorption time of flight (MALDI-TOF) process. Matrix choice, solvent, laser intensity and cholesterol concentration were systematically varied to characterize the conditions leading to the highest signals of the radical cation peaks, and it was found that initial cholesterol solution concentration and resultant density of solid cholesterol on the MALDI target were important parameters in determining signal intensities. It is proposed that hydroxyl radicals, generated as a result of laser irradiation of the employed 2,5-dihydroxybenzoic acid (DHB) matrix, initiate cholesterol oxidation on the MALDI target. An attempt to induce the odd-electron oxidation peaks by means of adding an oxidizing agent succeeded using an acetonitrile solution of DHB, cholesterol, and cumene hydroperoxide. Moreover, addition of free radical scavengers reduced the abundances of some oxidation products under certain conditions. These results are consistent with the mechanism of oxidation proposed herein involving laser-induced hydroxyl radical production followed by attack on neutral cholesterol. Hydroxyl radical production upon irradiation of dithranol matrix may also be responsible for generation of the same radical peaks observed from cholesterol in dithranol by an analogous mechanism. © American Society for Mass Spectrometry, 2011

The occurrence and behavior of radium in saline formation water of the U.S. Gulf Coast region.

USGS Publications Warehouse

Kraemer, T.F.; Reid, D.F.

1984-01-01

Ra was measured in deep saline formation waters produced from a variety of US Gulf Coast subsurface environments, including oil and gas reservoirs, and water-producing geopressured aquifers. A strong positive correlation was found between formation-water salinity and Ra activity, resulting from the interaction of formation water with aquifer matrix. Ra isotopes enter the fluid phase after being produced by the decay of parent elements U and Th on and within the solid matrix. The processes believed to be primarily responsible for transfering Ra from matrix to formation water are chemical leaching and alpha -particle recoil. Factors controlling the observed salinity-Ra relationship may be one or a combination of the following: 1) ion exchange; 2) increased solubility of matrix silica surrounding Ra atoms, coupled with a salinity-controlled rate of re-equilibration of silica between solution and quartz grains; and 3) the equilibration of Ra in solution with detrital baryte within the aquifer. No difference was found in the brine-Ra relation in water produced from oil or gas wells and water produced from wells penetrating only water-bearing aquifers, although the relation was more highly correlated for water-bearing aquifers than hydrocarbon-containing reservoirs.-P.Br.

The occurrence and behavior of radium in saline formation water of the U.S. Gulf Coast region

USGS Publications Warehouse

Kraemer, T.F.; Reid, D.F.

1984-01-01

Radium has been measured in deep saline formation waters produced from a variety of U.S. Gulf Coast subsurface environments, including oil reservoirs, gas reservoirs and water-producing geopressured aquifers. A strong positive correlation has been found between formation-water salinity and Ra activity, resulting from the interaction of formation water with aquifer matrix. Ra isotopes enter the fluid phase after being produced by the decay of parent elements U and Th, which are located at sites on and within the solid matrix. Processes that are belived to be primarily responsible for transferring Ra from matrix to formation water are chemical leaching and alpha-particle recoil. Factors controlling the observed salinity-Ra relationship may be one or a combination of the following factors: (a) ion exchange; (b) increased solubility of matrix silica surrounding Ra atoms, coupled with a salinity-controlled rate of reequilibration of silica between solution and quartz grains; and (c) the equilibration of Ra in solution with detrial barite within the aquifer. No difference was found in the brine-Ra relation in water produced from oil or gas wells and water produced from wells penetrating only water-bearing aquifers, although the relation was more highly correlated for water-bearing aquifers than hydrocarbon-containing reservoirs. ?? 1984.

Investigations of systems ThO 2-MO 2-P 2O 5 (M=U, Ce, Zr, Pu). Solid solutions of thorium-uranium (IV) and thorium-plutonium (IV) phosphate-diphosphates

NASA Astrophysics Data System (ADS)

Dacheux, N.; Podor, R.; Brandel, V.; Genet, M.

1998-02-01

In the framework of nuclear waste management aiming at the research of a storage matrix, the chemistry of thorium phosphates has been completely re-examined. In the ThO 2-P 2O 5 system a new compound thorium phosphate-diphosphate Th 4(PO 4) 4P 2O 7 has been synthesized. The replacement of Th 4+ by a smaller cation like U 4+ and Pu 4+ in the thorium phosphate-diphosphate (TPD) lattice has been achieved. Th 4- xU x(PO 4) 4P 2O 7 and Th 4- xPu x(PO 4) 4P 2O 7 solid solutions have been synthesized through wet and dry processes with 0< x<3.0 for uranium and 0< x<1.0 for plutonium. From the variation of the unit cell parameters, an upper x value equal to 1.67 has been estimated for the thorium-plutonium (IV) phosphate-diphosphate solid solutions. Two other tetravalent cations, Ce 4+ and Zr 4+, cannot be incorporated in the TPD lattice: cerium (IV) because of its reduction into Ce (III) at high temperature, and zirconium probably because of its too small radius compared to thorium.

La-Sr-Ni-Co-O based perovskite-type solid solutions as catalyst precursors in the CO 2 reforming of methane

NASA Astrophysics Data System (ADS)

Valderrama, Gustavo; Kiennemann, Alain; Goldwasser, Mireya R.

La 1- xSr xNi 0.4Co 0.6O 3 and La 0.8Sr 0.2Ni 1- yCo yO 3 solid solutions with perovskite-type structure were synthesized by the sol-gel resin method and used as catalytic precursors in the dry reforming of methane with CO 2 to syngas, between 873 and 1073 K at atmospheric pressure under continuous flow of reactant gases with CH 4/CO 2 = 1 ratio. These quaternary oxides were characterized by X-ray diffraction (XRD), BET specific surface area and temperature-programmed reduction (TPR) techniques. XRD analyses of the more intense diffraction peaks and cell parameter measurements showed formation of La-Sr-Ni-Co-O solid solutions with La 0.9Sr 0.1CoO 3 and/or La 0.9Sr 0.1NiO 3 as the main crystallographic phases present on the solids depending on the degree of substitution. TPR analyses showed that Sr doping decreases the temperature of reduction via formation of intermediary species producing Ni 0, Co 0 with particle sizes in the range of nanometers over the SrO and La 2O 3 phases. These metallic nano particles highly dispersed in the solid matrix are responsible for the high activity shown during the reaction and avoid carbon formation. The presence of Sr in doping quantities also promotes the secondary reactions of carbon formation and water-gas shift in a very small extension during the dry reforming reaction.

Constrained Sintering in Fabrication of Solid Oxide Fuel Cells

PubMed Central

Lee, Hae-Weon; Park, Mansoo; Hong, Jongsup; Kim, Hyoungchul; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook

2016-01-01

Solid oxide fuel cells (SOFCs) are inevitably affected by the tensile stress field imposed by the rigid substrate during constrained sintering, which strongly affects microstructural evolution and flaw generation in the fabrication process and subsequent operation. In the case of sintering a composite cathode, one component acts as a continuous matrix phase while the other acts as a dispersed phase depending upon the initial composition and packing structure. The clustering of dispersed particles in the matrix has significant effects on the final microstructure, and strong rigidity of the clusters covering the entire cathode volume is desirable to obtain stable pore structure. The local constraints developed around the dispersed particles and their clusters effectively suppress generation of major process flaws, and microstructural features such as triple phase boundary and porosity could be readily controlled by adjusting the content and size of the dispersed particles. However, in the fabrication of the dense electrolyte layer via the chemical solution deposition route using slow-sintering nanoparticles dispersed in a sol matrix, the rigidity of the cluster should be minimized for the fine matrix to continuously densify, and special care should be taken in selecting the size of the dispersed particles to optimize the thermodynamic stability criteria of the grain size and film thickness. The principles of constrained sintering presented in this paper could be used as basic guidelines for realizing the ideal microstructure of SOFCs. PMID:28773795

Ductile tungsten-nickel alloy and method for making same

DOEpatents

Snyder, Jr., William B.

1976-01-01

The present invention is directed to a ductile, high-density tungsten-nickel alloy which possesses a tensile strength in the range of 100,000 to 140,000 psi and a tensile elongation of 3.1 to 16.5 percent in 1 inch at 25.degree.C. This alloy is prepared by the steps of liquid phase sintering a mixture of tungsten-0.5 to 10.0 weight percent nickel, heat treating the alloy at a temperature above the ordering temperature of approximately 970.degree.C. to stabilize the matrix phase, and thereafter rapidly quenching the alloy in a suitable liquid to maintain the matrix phase in a metastable, face-centered cubic, solid- solution of tungsten in nickel.

Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid-phase dispersion extraction of bioactive flavonoids from toothpaste, plant, and saliva.

PubMed

Cao, Wan; Cao, Jun; Ye, Li-Hong; Xu, Jing-Jing; Hu, Shuai-Shuai; Peng, Li-Qing

2015-12-01

This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Understanding the generation and maintenance of supersaturation during the dissolution of amorphous solid dispersions using modulated DSC and 1H NMR.

PubMed

Baghel, Shrawan; Cathcart, Helen; O'Reilly, Niall J

2018-01-30

In this study, the dissolution behaviour of dipyridamole (DPM) and cinnarizine (CNZ) spray-dried amorphous solid dispersions (ASDs) using polyvinyl pyrrolidone (PVP) and polyacrylic acid (PAA) as a carrier matrix were evaluated and compared. The drug concentrations achieved from the dissolution of PVP and PAA solid dispersions were significantly greater than the equilibrium solubility of crystalline DPM and CNZ in phosphate buffer pH 6.8 (PBS 6.8). The maximum drug concentration achieved by dissolution of PVP and PAA solid dispersions did not exceed the theoretically calculated apparent solubility of amorphous DPM and CNZ. However, the degree of supersaturation of DPM and CNZ increased considerably as the polymer weight fraction within the solid dispersion increased. In addition, the supersaturation profile of DPM and CNZ were studied in the presence and absence of the polymers. PAA was found to maintain a higher level of supersaturation compared to PVP. The enhanced drug solution concentration following dissolution of ASDs can be attributed to the reduced crystal growth rates of DPM and CNZ at an equivalent supersaturation. We have also shown that, for drugs having high crystallization tendency and weak drug-polymer interaction, the feasible way to increase dissolution might be increase the polymer weight fraction in the ASD. Solution 1 H NMR spectra were used to understand dissolution mechanism and to identify drug-polymer interaction. The change in electron densities of proton attached to different groups in DPM and CNZ suggested drug-polymer interaction in solution. The relative intensities of peak shift and nature of interaction between drug and polymer in different systems are different. These different effects suggest that DPM and CNZ interacts in a different way with PVP and PAA in solution which goes some way towards explaining the different polymeric effect, particularly in terms of inhibition of drug recrystallization and dissolution of DPM and CNZ ASDs. These results established that the different drug/polymer interactions in the solid state and in solution give rise to the variation in dissolution profile observed for different systems. Copyright © 2017 Elsevier B.V. All rights reserved.

A New Type of Self-lubricated Thermal Spray Coatings: Liquid Lubricants Embedded in a Metal Matrix

NASA Astrophysics Data System (ADS)

Espallargas, N.; Armada, S.

2015-01-01

Oils and greases are commonly used for lubricating, rotating and sliding systems such as bearings, gears, connectors, etc. The maintenance of such lubricated systems in some applications where access is difficult (e.g., offshore wind farms and subsea equipment) increases the operational costs. In some cases, it can be thought that the use of solid lubricants (MoS2, PTFE, graphite, etc.) embedded in coatings could be a solution for such applications; however, the mechanical and dynamic conditions of most of the systems are not appropriate for solid lubricants. Despite this, solid lubricants such as PTFE and MoS2 have been largely employed in different industries, especially in those applications where liquid lubricants cannot be used and when the dynamic conditions allow for it. Self-lubricated coatings have been a major topic of interest in thermal spray in the last decades. Although the use of liquid lubricants is desirable whenever it is possible, limited research has been addressed toward the development of self-lubricated coatings containing liquid lubricants. One of the main reasons for this is due to the complexity of embedding liquid lubricant reservoirs inside the coating matrix. In the present work, a new type of liquid-solid self-lubricated coatings is presented, being the matrix a metal alloy. Three thermal spray techniques used were as follows: arc-spray, plasma spray, and HVOAF. The metal matrices were two stainless steel types and liquid lubricant-filled capsules with different liquid contents were used. No degradation of the capsules during spraying was observed and the coatings containing capsules were able to keep a low coefficient of friction. The optimal performance is found for the coatings obtained at the lowest spraying temperature and velocity.

A novel approach for the fabrication of all-inorganic nanocrystal solids: Semiconductor matrix encapsulated nanocrystal arrays

NASA Astrophysics Data System (ADS)

Moroz, Pavel

Growing fossil fuels consumption compels researchers to find new alternative pathways to produce energy. Along with new materials for the conversion of different types of energy into electricity innovative methods for efficient processing of energy sources are also introduced. The main criteria for the success of such materials and methods are the low cost and compelling performance. Among different types of materials semiconductor nanocrystals are considered as promising candidates for the role of the efficient and cheap absorbers for solar energy applications. In addition to the anticipated cost reduction, the integration of nanocrystals (NC) into device architectures is inspired by the possibility of tuning the energy of electrical charges in NCs via nanoparticle size. However, the stability of nanocrystals in photovoltaic devices is limited by the stability of organic ligands which passivate the surface of semiconductors to preserve quantum confinement. The present work introduces a new strategy for low-temperature processing of colloidal nanocrystals into all-inorganic films: semiconductor matrix encapsulated nanocrystal arrays (SMENA). This methodology goes beyond the traditional ligand-interlinking scheme and relies on the encapsulation of morphologically-defined nanocrystal arrays into a matrix of a wide-band gap semiconductor, which preserves optoelectronic properties of individual nanoparticles. Fabricated solids exhibit excellent thermal stability, which is attributed to the heteroepitaxial structure of nanocrystal-matrix interfaces. The main characteristics and properties of these solids were investigated and compared with ones of traditionally fabricated nanocrystal films using standard spectroscopic, optoelectronic and electronic techniques. As a proof of concept, we. We also characterized electron transport phenomena in different types of nanocrystal films using all-optical approach. By measuring excited carrier lifetimes in either ligand-linked or matrix-encapsulated PbS nanocrystal films containing a tunable fraction of insulating ZnS domains, we uniquely distinguish the dynamics of charge scattering on defects from other processes of exciton dissociation. The measured times are subsequently used to estimate the diffusion length and the carrier mobility for each film type within hopping transport regime. It is demonstrated that nanocrystal films encapsulated into semiconductor matrices exhibit a lower probability of charge scattering than nanocrystal solids cross-linked with either 3-mercaptopropionic acid or 1,2-ethanedithiol molecular linkers. The suppression of carrier scattering in matrix-encapsulated nanocrystal films is attributed to a relatively low density of surface defects at nanocrystal/matrix interfaces. High stability and low density of defects made it possible to fabricate infrared-emitting nanocrystal solids. Presently, an important challenge facing the development of nanocrystal infrared emitters concerns the fact that both the emission quantum yield and the stability of colloidal nanoparticles become compromised when nanoparticle solutions are processed into solids. Here, we address this issue by developing an assembly technique that encapsulates infrared-emitting PbS NCs into crystalline CdS matrices, designed to preserve NC emission characteristics upon film processing. Here, the morphology of these matrices was designed to suppress the nonradiative carrier decay, whereby increasing the exciton lifetime up to 1 mus, and boosting the emission quantum yield to an unprecedented 3.7% for inorganically encapsulated PbS NC solids.

Simultaneous use of solution NMR and X-ray data in REFMAC5 for joint refinement/detection of structural differences.

PubMed

Rinaldelli, Mauro; Ravera, Enrico; Calderone, Vito; Parigi, Giacomo; Murshudov, Garib N; Luchinat, Claudio

2014-04-01

The program REFMAC5 from CCP4 was modified to allow the simultaneous use of X-ray crystallographic data and paramagnetic NMR data (pseudocontact shifts and self-orientation residual dipolar couplings) and/or diamagnetic residual dipolar couplings. Incorporation of these long-range NMR restraints in REFMAC5 can reveal differences between solid-state and solution conformations of molecules or, in their absence, can be used together with X-ray crystallographic data for structural refinement. Since NMR and X-ray data are complementary, when a single structure is consistent with both sets of data and still maintains reasonably `ideal' geometries, the reliability of the derived atomic model is expected to increase. The program was tested on five different proteins: the catalytic domain of matrix metalloproteinase 1, GB3, ubiquitin, free calmodulin and calmodulin complexed with a peptide. In some cases the joint refinement produced a single model consistent with both sets of observations, while in other cases it indicated, outside the experimental uncertainty, the presence of different protein conformations in solution and in the solid state.

A facile method to prepare "green" nano-phosphors with a large Stokes-shift and solid-state enhanced photophysical properties based on surface-modified gold nanoclusters.

PubMed

Cheng, C H; Huang, H Y; Talite, M J; Chou, W C; Yeh, J M; Yuan, C T

2017-12-15

Colloidal nano-materials, such as quantum dots (QDs) have been applied to light-conversion nano-phosphors due to their unique tunable emission. However, most of the QDs involve toxic elements and are synthesized in a hazardous solvent. In addition, conventional QD nano-phosphors with a small Stokes shift suffered from reabsorption losses and aggregation-induced quenching in the solid state. Here, we demonstrate a facile, matrix-free method to prepare eco-friendly nano-phosphors with a large Stokes shift based on aqueous thiolate-stabilized gold nanoclusters (GSH-AuNCs) with simple surface modifications. Our method is just to drop GSH-AuNCs solution on the aluminum foil and then surface-modified AuNCs (Al-GSH-AuNCs) can be spontaneously precipitated out of the aqueous solution. Compared with pristine GSH-AuNCs in solution, the Al-GSH-AuNCs exhibit enhanced solid-state PL quantum yields, lengthened PL lifetime, and spectral blue shift, which can be attributed to the aggregation-induced emission enhancement facilitated by surface modifications. Such surface-treatment induced aggregation of AuNCs can restrict the surface-ligand motion, leading to the enhancement of PL properties in the solid state. In addition, the Al-GSH-AuNCs nano-phosphors with a large Stokes shift can mitigate the aggregation-induced PL quenching and reabsorption losses, which would be potential candidates for "green" nano-phosphors. Copyright © 2017 Elsevier Inc. All rights reserved.

Predictive model to describe water migration in cellular solid foods during storage.

PubMed

Voogt, Juliën A; Hirte, Anita; Meinders, Marcel B J

2011-11-01

Water migration in cellular solid foods during storage causes loss of crispness. To improve crispness retention, physical understanding of this process is needed. Mathematical models are suitable tools to gain this physical knowledge. Water migration in cellular solid foods involves migration through both the air cells and the solid matrix. For systems in which the water migration distance is large compared with the cell wall thickness of the solid matrix, the overall water flux through the system is dominated by the flux through the air. For these systems, water migration can be approximated well by a Fickian diffusion model. The effective diffusion coefficient can be expressed in terms of the material properties of the solid matrix (i.e. the density, sorption isotherm and diffusion coefficient of water in the solid matrix) and the morphological properties of the cellular structure (i.e. water vapour permeability and volume fraction of the solid matrix). The water vapour permeability is estimated from finite element method modelling using a simplified model for the cellular structure. It is shown that experimentally observed dynamical water profiles of bread rolls that differ in crust permeability are predicted well by the Fickian diffusion model. Copyright © 2011 Society of Chemical Industry.

Stabilization of superionic α-Agl at room temperature in a glass matrix

NASA Astrophysics Data System (ADS)

Tatsumisago, Masahiro; Shinkuma, Yoshikane; Minami, Tsutomu

1991-11-01

SINCE the discovery1 that the high-temperature phase of silver iodide (α-AgI) has an ionic conductivity comparable to that of the best liquid electrolytes, solid electrolytes have attracted wide interest. Possible applications of these materials range from solid-state batteries to electrochromic displays and sensors2. Although α-AgI displays conductivities of more than 10 S cm-1 (ref. 3), owing to the almost liquid-like mobility of Ag+ ions, the crystal transforms below 147 °C to the β-phase with a conductivity of only ~10-5 S cm-1 at room temperature. Efforts to achieve good conductivities at lower temperatures have focused on the addition of a second component to AgI to form solid solutions or new compounds such as RbAg4I5 and Ag2HgI4 (refs 4-7). Here we report our success in depressing the α-->β transformation temperature so as to stabilize α-AgI itself at room temperature. We use a melt-quenching technique to prepare crystallites of α-AgI frozen into a silver borate glass matrix. The quenched material showed diffraction peaks characteristic of α-AgI and displayed ionic conductivities of about 10-1 S cm-1. Further development of these glass/crystal composites may make the high ionic conductivity of α-AgI available for room-temperature solid-state applications.

Method for molding ceramic powders using a water-based gel casting

DOEpatents

Janney, Mark A.; Omatete, Ogbemi O.

1991-07-02

A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant, and a monomer solution. The monomer solution includes at least one monofunctional monomer and at least one difunctional monomer, a free-radical initiator, and a aqueous solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product any be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, whereafter the product may be sintered.

Method for molding ceramic powders using a water-based gel casting process

DOEpatents

Jenny, Mark A.; Omalete, Ogbemi O.

1992-09-08

A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant, and a monomer solution. The monomer solution includes at least one monofunctional monomer and at least one difunctional monomer, a free-radical initiator, and a aqueous solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, whereafter the product may be sintered.

Kinetics of transformation of deformation processed gold-matrix composite

NASA Astrophysics Data System (ADS)

Wongpreedee, Kageeporn

Gold matrix Ḏeformation-processed M&barbelow;etal M&barbelow;etal C&barbelow;omposites (DMMC) have been developed that have better strength and conductivity than conventional gold alloys. However, DMMC possess metastable two-phase microstructures, and their strength and conductivity decrease after prolonged exposure to elevated temperatures. The kinetics of the transformation from the metastable two-phase microstructure to the equilibrium single-phase solid solution is of interest. This document describes a study of the elevated temperature stability of Au DMMC's and the relationship between microstructure and resistivity of three compositions: Au-7 vol %Ag, Au-14 vol %Ag, and Au-vol 7%Pt. DMMC samples were prepared by a powder metallurgy technique and mechanical processes. The smallest final diameter of these wires was 120 mum. Avrami and Arrhenius relations were used to evaluate the kinetic transformation. The extensive deformation used to produce these composites reshaped the initially equi-axed powder particles into a nanofilamentary composite. Electrical resistivity measurements were used to determine the degree of transformation from the initial metastable nano-filamentary composite to the equilibrium solid solution condition. These measurements indicated that this transformation in Au-14 at%Ag, Au-7 at %Ag Au and Au-7 at %Pt DMMC wires proceeded with activation energies of 141, 156, and 167 kJ/mol, respectively. It is thought that these empirically determined activation energies differ from those determined in single crystal, planar interface Au-Ag and Au-Pt diffusion couples due to chemical potential, surface curvature, and strain effects. The DMMC systems reach the equilibrium solid solution condition faster than single crystal, planar interface systems for two reasons: (1) far more defects (dislocations, grain boundaries, vacancies from non-conservative dislocation motion, etc.) are present in the Au-Ag and Au-Pt DMMC composites, and (2) the small radius of curvature of the Ag and Pt filaments increases the chemical potential for diffusion in the DMMC.

Macroscopic modelling of multiperiodic composites

NASA Astrophysics Data System (ADS)

Woźniak, Czesław

By a multiperiodic composite we mean a composite solid in which all constituents are periodically distributed in a matrix but a representative element (unit cell) may not exist. The aim of this Note is to propose a nonasymptotic approach to the formation of averaged (macroscopic) models of multiperiodic composites. The approach is based on the concept of tolerance averaging, which in [2] was applied to the modelling of periodic composites. The derived model, in contrast to homogenization, describes the effect of microstructure size on the overall solid behaviour and yields necessary conditions for the physical correctness of solutions to special problems. To cite this article: C. Woźniak, C. R. Mecanique 330 (2002) 267-272.

Stationary light pulse in solids with long-lived spin coherence

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang Xiaojun; Wang Haihua; Wang Lei

We present a detailed analysis of stationary light pulses (SLP's) for the case of inhomogeneous broadening in both optical and spin transitions, which is normally found in solid materials with long-lived spin coherence. By solving the Langevin equations of motion for the density matrix elements under the integral over the entire range of the inhomogeneous broadenings, the necessary conditions for creating the SLP in a solid are obtained. Then the decay and diffusion processes that the SLP undergoes are analyzed. The characteristics of such processes are studied based on the analytic solution of the SLP with a slowly varying envelope.more » The dependence of SLP lifetime on inhomogeneous broadenings of spin and optical transitions, which can be regarded as the laser linewidth in the repump scheme, has been discussed.« less

Solid-phase assays for small molecule screening using sol-gel entrapped proteins.

PubMed

Lebert, Julie M; Forsberg, Erica M; Brennan, John D

2008-04-01

With compound libraries exceeding one million compounds, the ability to quickly and effectively screen these compounds against relevant pharmaceutical targets has become crucial. Solid-phase assays present several advantages over solution-based methods. For example, a higher degree of miniaturization can be achieved, functional- and affinity-based studies are possible, and a variety of detection methods can be used. Unfortunately, most protein immobilization methods are either too harsh or require recombinant proteins and thus are not amenable to delicate proteins such as kinases and membrane-bound receptors. Sol-gel encapsulation of proteins in an inorganic silica matrix has emerged as a novel solid-phase assay platform. In this minireview, we discuss the development of sol-gel derived protein microarrays and sol-gel based monolithic bioaffinity columns for the high-throughput screening of small molecule libraries and mixtures.

Investigation of solvent-free MALDI-TOFMS sample preparation methods for the analysis of organometallic and coordination compounds.

PubMed

Hughes, Laura; Wyatt, Mark F; Stein, Bridget K; Brenton, A Gareth

2009-01-15

An investigation of various solvent-free matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) sample preparation methods for the characterization of organometallic and coordination compounds is described. Such methods are desirable for insoluble materials, compounds that are only soluble in disadvantageous solvents, or complexes that dissociate in solution, all of which present a major "difficulty" to most mass spectrometry techniques. First-row transition metal acetylacetonate complexes, which have been characterized previously by solution preparation MALDI-TOFMS, were used to evaluate the various solvent-free procedures. These procedures comprise two distinct steps: the first being the efficient "solids mixing" (the mixing of sample and matrix), and the second being the effective transfer of the sample/matrix mixture to the MALDI target plate. This investigation shows that vortex mixing is the most efficient first step and that smearing using a microspatula is the most effective second step. In addition, the second step is shown to be much more critical than the first step in obtaining high-quality data. Case studies of truly insoluble materials highlight the importance of these techniques for the wider chemistry community.

Atmospheric pressure laser desorption/ionization using a 6-7 µm-band mid-infrared tunable laser and liquid water matrix.

PubMed

Hiraguchi, Ryuji; Hazama, Hisanao; Masuda, Katsuyoshi; Awazu, Kunio

2015-01-01

Due to the characteristic absorption peaks in the IR region, various molecules can be used as a matrix for infrared matrix-assisted laser desorption/ionization (IR-MALDI). Especially in the 6-7 µm-band IR region, solvents used as the mobile phase for liquid chromatography have absorption peaks that correspond to their functional groups, such as O-H, C=O, and CH3. Additionally, atmospheric pressure (AP) IR-MALDI, which is applicable to liquid-state samples, is a promising technique to directly analyze untreated samples. Herein we perform AP-IR-MALDI mass spectrometry of a peptide, angiotensin II, using a mid-IR tunable laser with a tunable wavelength range of 5.50-10.00 µm and several different matrices. The wavelength dependences of the ion signal intensity of [M + H](+) of the peptide are measured using a conventional solid matrix, α-cyano-4-hydroxycinnamic acid (CHCA) and a liquid matrix composed of CHCA and 3-aminoquinoline. Other than the O-H stretching and bending vibration modes, the characteristic absorption peaks are useful for AP-IR-MALDI. Peptide ions are also observed from an aqueous solution of the peptide without an additional matrix, and the highest peak intensity of [M + H](+) is at 6.00 µm, which is somewhat shorter than the absorption peak wavelength of liquid water corresponding to the O-H bending vibration mode. Moreover, long-lasting and stable ion signals are obtained from the aqueous solution. AP-IR-MALDI using a 6-7 µm-band IR tunable laser and solvents as the matrix may provide a novel on-line interface between liquid chromatography and mass spectrometry. Copyright © 2015 John Wiley & Sons, Ltd.

Solution Treatment Effect on Tensile, Impact and Fracture Behaviour of Trace Zr Added Al-12Si-1Mg-1Cu Piston Alloy

NASA Astrophysics Data System (ADS)

Kaiser, Md. Salim

2018-04-01

The effects of T6 solution treatment on tensile, impact and fracture properties of cast Al-12Si-1Mg-1Cu piston alloys with trace of zirconium were investigated. Cast alloys were given precipitation strengthening treatment having a sequence of homogenizing, solutionizing, quenching and ageing. Both cast and solutionized samples are isochronally aged for 90 min at different temperatures up to 300 °C. Tensile and impact properties of the differently processed alloys have been studied to understand the precipitation strengthening of the alloys. Fractograpy of the alloys were observed to understand the mode of fracture. It is observed that the improvement in tensile properties in the aged alloys through heat treatment is mainly attributed to the formation of the Al2Cu and Mg2Si precipitates within the Al matrix. Solution treatment improves the tensile strength for the reason that during solution treatment some alloying elements are re-dissolved to produce a solute-rich solid solution. Impact energy decreases with ageing temperature due to formation of GP zones, β' and β precipitates. The fractography shows large and small dimple structure and broken or cracked primary Si, particles. Microstructure study of alloys revealed that the solution treatment improved distribution of silicon grains. The addition of Zr produces an improvement in the tensile properties as a result of its grain refining action and grain coarsening resistance in the matrix at a higher temperature.

Phase Behavior of Ritonavir Amorphous Solid Dispersions during Hydration and Dissolution.

PubMed

Purohit, Hitesh S; Taylor, Lynne S

2017-12-01

The aim of this research was to study the interplay of solid and solution state phase transformations during the dissolution of ritonavir (RTV) amorphous solid dispersions (ASDs). RTV ASDs with polyvinylpyrrolidone (PVP), polyvinylpyrrolidone vinyl acetate (PVPVA) and hydroxypropyl methylcellulose acetate succinate (HPMCAS) were prepared at 10-50% drug loading by solvent evaporation. The miscibility of RTV ASDs was studied before and after exposure to 97% relative humidity (RH). Non-sink dissolution studies were performed on fresh and moisture-exposed ASDs. RTV and polymer release were monitored using ultraviolet-visible spectroscopy. Techniques including fluorescence spectroscopy, confocal imaging, scanning electron microscopy (SEM), atomic force microscopy (AFM), differential scanning calorimetry (DSC) and nanoparticle tracking analysis (NTA) were utilized to monitor solid and the solution state phase transformations. All RTV-PVP and RTV-PVPVA ASDs underwent moisture-induced amorphous-amorphous phase separation (AAPS) on high RH storage whereas RTV-HPMCAS ASDs remained miscible. Non-sink dissolution of PVP- and PVPVA-based ASDs at low drug loadings led to rapid RTV and polymer release resulting in concentrations in excess of amorphous solubility, liquid-liquid phase separation (LLPS) and amorphous nanodroplet formation. High drug loading PVP- and PVPVA-based ASDs did not exhibit LLPS upon dissolution as a consequence of extensive AAPS in the hydrated ASD matrix. All RTV-HPMCAS ASDs led to LLPS upon dissolution. RTV ASD dissolution is governed by a competition between the dissolution rate and the rate of phase separation in the hydrated ASD matrix. LLPS was observed for ASDs where the drug release was polymer controlled and only ASDs that remained miscible during the initial phase of dissolution led to LLPS. Techniques such as fluorescence spectroscopy, confocal imaging and SEM were useful in understanding the phase behavior of ASDs upon hydration and dissolution and were helpful in elucidating the mechanism of generation of amorphous nanodroplets.

Preparation of Si and O co-solution strengthened Ti alloys by using rice husks as SiO2 resource and quantitative descriptions on their strengthening effects

NASA Astrophysics Data System (ADS)

Jia, Lei; Chen, Jiang-xian; Lu, Zhen-lin; Li, Shu-feng; Umeda, Junko; Kondoh, Katsuyoshi

2018-04-01

Ti alloys strengthened by both Si and O solutes were prepared by powder metallurgy method from pure Ti and amorphous SiO2 powder obtained by combusting rice husks. At the same time, Ti alloys singly strengthened by Si or O were also prepared for studying the strengthening effect of Si and O solutes. Results showed that amorphous SiO2 powder originated from rice husks could almost fully dissolve into pure Ti matrix when the content was not higher than 1.0 wt%, while higher content of SiO2 addition resulted in the formation of Ti5Si3 intermetallics. Si and O elements leaded to negative and positive distortion of Ti lattice, and the influencing degrees were ‑0.02 and +0.014 Å/wt% for lattice constant a, while ‑0.05 and +0.046 Å/wt% for constant c, respectively. Solid solution of Si and O would also result in the increase of hardness, which was 98.5 and 209.43 HV/wt%, respectively. When Si and O were co-exsited in Ti matrix, the negative and positive distortion cancelled each other, while the strengthening effect did not cancel but enhance each other.

On the Representation of Aquifer Compressibility in General Subsurface Flow Codes: How an Alternate Definition of Aquifer Compressibility Matches Results from the Groundwater Flow Equation

NASA Astrophysics Data System (ADS)

Birdsell, D.; Karra, S.; Rajaram, H.

2016-12-01

The governing equations for subsurface flow codes in deformable porous media are derived from the fluid mass balance equation. One class of these codes, which we call general subsurface flow (GSF) codes, does not explicitly track the motion of the solid porous media but does accept general constitutive relations for porosity, density, and fluid flux. Examples of GSF codes include PFLOTRAN, FEHM, STOMP, and TOUGH2. Meanwhile, analytical and numerical solutions based on the groundwater flow equation have assumed forms for porosity, density, and fluid flux. We review the derivation of the groundwater flow equation, which uses the form of Darcy's equation that accounts for the velocity of fluids with respect to solids and defines the soil matrix compressibility accordingly. We then show how GSF codes have a different governing equation if they use the form of Darcy's equation that is written only in terms of fluid velocity. The difference is seen in the porosity change, which is part of the specific storage term in the groundwater flow equation. We propose an alternative definition of soil matrix compressibility to correct for the untracked solid velocity. Simulation results show significantly less error for our new compressibility definition than the traditional compressibility when compared to analytical solutions from the groundwater literature. For example, the error in one calculation for a pumped sandstone aquifer goes from 940 to <70 Pa when the new compressibility is used. Code users and developers need to be aware of assumptions in the governing equations and constitutive relations in subsurface flow codes, and our newly-proposed compressibility function should be incorporated into GSF codes.

On the Representation of Aquifer Compressibility in General Subsurface Flow Codes: How an Alternate Definition of Aquifer Compressibility Matches Results from the Groundwater Flow Equation

NASA Astrophysics Data System (ADS)

Birdsell, D.; Karra, S.; Rajaram, H.

2017-12-01

The governing equations for subsurface flow codes in deformable porous media are derived from the fluid mass balance equation. One class of these codes, which we call general subsurface flow (GSF) codes, does not explicitly track the motion of the solid porous media but does accept general constitutive relations for porosity, density, and fluid flux. Examples of GSF codes include PFLOTRAN, FEHM, STOMP, and TOUGH2. Meanwhile, analytical and numerical solutions based on the groundwater flow equation have assumed forms for porosity, density, and fluid flux. We review the derivation of the groundwater flow equation, which uses the form of Darcy's equation that accounts for the velocity of fluids with respect to solids and defines the soil matrix compressibility accordingly. We then show how GSF codes have a different governing equation if they use the form of Darcy's equation that is written only in terms of fluid velocity. The difference is seen in the porosity change, which is part of the specific storage term in the groundwater flow equation. We propose an alternative definition of soil matrix compressibility to correct for the untracked solid velocity. Simulation results show significantly less error for our new compressibility definition than the traditional compressibility when compared to analytical solutions from the groundwater literature. For example, the error in one calculation for a pumped sandstone aquifer goes from 940 to <70 Pa when the new compressibility is used. Code users and developers need to be aware of assumptions in the governing equations and constitutive relations in subsurface flow codes, and our newly-proposed compressibility function should be incorporated into GSF codes.

In situ molecular NMR picture of bioavailable calcium stabilized as amorphous CaCO3 biomineral in crayfish gastroliths

PubMed Central

Akiva-Tal, Anat; Kababya, Shifi; Balazs, Yael S.; Glazer, Lilah; Berman, Amir; Sagi, Amir; Schmidt, Asher

2011-01-01

Bioavailable calcium is maintained by some crustaceans, in particular freshwater crayfish, by stabilizing amorphous calcium carbonate (ACC) within reservoir organs—gastroliths, readily providing the Ca2+ needed to build a new exoskeleton. Despite the key scientific and biomedical importance of the in situ molecular-level picture of biogenic ACC and its stabilization in a bioavailable form, its description has eluded efforts to date. Herein, using multinuclear NMR, we accomplish in situ molecular-level characterization of ACC within intact gastroliths of the crayfish Cherax quadricarinatus. In addition to the known CaCO3, chitin scaffold and inorganic phosphate (Pi), we identify within the gastrolith two primary metabolites, citrate and phosphoenolpyruvate (PEP) and quantify their abundance by applying solution NMR techniques to the gastrolith “soluble matrix.” The long-standing question on the physico-chemical state of ACC stabilizing, P-bearing moieties within the gastrolith is answered directly by the application of solid state rotational-echo double-resonance (REDOR) and transferred-echo double-resonance (TEDOR) NMR to the intact gastroliths: Pi and PEP are found molecularly dispersed throughout the ACC as a solid solution. Citrate carboxylates are found < 5 Å from a phosphate (intermolecular C⋯P distance), an interaction that must be mediated by Ca2+. The high abundance and extensive interactions of these molecules with the ACC matrix identify them as the central constituents stabilizing the bioavailable form of calcium. This study further emphasizes that it is imperative to characterize the intact biogenic CaCO3. Solid state NMR spectroscopy is shown to be a robust and accessible means of determining composition, internal structure, and molecular functionality in situ. PMID:21873244

Study of the effects of heat-treatment of hydroxyapatite synthesized in gelatin matrix

NASA Astrophysics Data System (ADS)

Zaits, A. V.; Golovanova, O. A.; Kuimova, M. V.

2017-01-01

In the study, the isothermal thermogravimetric analysis (TGA) of hydroxyapatite synthesized in gelatin matrix (HAG) has been performed. 3 wt.% HAG samples were synthesized from the solution simulating the human extracellular fluid (SBF). X-ray diffraction and IR spectroscopy were used to determine the composition. During the experiment, increase in the calcination temperature up to 200°C-800°C was found to cause weight loss. The study of phase composition revealed that heat treatment does not affect the phase composition of the solid phase, which is composed of hydroxylapatite (HA). The prepared HAG (3 wt.% gelatin) samples are shown to have low thermal stability; the degradation of the samples occurs at 400° C.

Study of the effects of heat-treatment of hydroxyapatite synthesized in gelatin matrix

NASA Astrophysics Data System (ADS)

Zaits, A. V.; Golovanova, O. A.; Kuimova, M. V.

2017-01-01

In the study, the isothermal thermogravimetric analysis (TGA) of hydroxyapatite synthesized in gelatin matrix (HAG) has been performed. 3 wt.% HAG samples were synthesized from the solution simulating the human extracellular fluid (SBF). X-ray diffraction and IR spectroscopy were used to determine the composition. During the experiment, increase in the calcination temperature up to 200°C-800°C was found to cause weight loss. The study of phase composition revealed that heat treatment does not affect the phase composition of the solid phase, which is composed of hydroxylapatite (HA). The prepared HAG (3 wt.% gelatin) samples are shown to have low thermal stability; the degradation of the samples occurs at 400°C.

From Mixed-Metal MOFs to Carbon-Coated Core-Shell Metal Alloy@Metal Oxide Solid Solutions: Transformation of Co/Ni-MOF-74 to CoxNi1-x@CoyNi1-yO@C for the Oxygen Evolution Reaction.

PubMed

Sun, Dengrong; Ye, Lin; Sun, Fangxiang; García, Hermenegildo; Li, Zhaohui

2017-05-01

Calcination of the mixed-metal species Co/Ni-MOF-74 leads to the formation of carbon-coated Co x Ni 1-x @Co y Ni 1-y O with a metal core diameter of ∼3.2 nm and a metal oxide shell thickness of ∼2.4 nm embedded uniformly in the ligand-derived carbon matrix. The close proximity of Co and Ni in the mixed-metal Co/Ni-MOF-74 promotes the metal alloying and the formation of a solid solution of metal oxide during the calcination process. The presence of the tightly coated carbon shell prohibits particle agglomeration and stabilizes the Co x Ni 1-x @Co y Ni 1-y O nanoparticles in small size. The Co x Ni 1-x @Co y Ni 1-y O@C derived from Co/Ni-MOF-74 nanocomposites show superior performance for the oxygen evolution reaction (OER). The use of mixed-metal MOFs as precursors represents a powerful strategy for the fabrication of metal alloy@metal oxide solid solution nanoparticles in small size. This method also holds great promise in the development of multifunctional carbon-coated complex core-shell metal/metal oxides owing to the diversified MOF structures and their flexible chemistry.

Synthesis and the luminescent properties of the Nd3+ ions doped three kinds of fluoride nanocrystals in organic solvents

NASA Astrophysics Data System (ADS)

Chen, Zhuo; Tian, Changyong; Bo, Shuhui; Liu, Xinhou; Zhen, Zhen

2015-10-01

Oleic acid (OA)-modified LaF3:Nd, NaYF4:Nd and CaF2:Nd nanocrystals (NCs) with the different Nd3+ ion concentration (2% and 5%) have been prepared. The structure and morphology of NCs were identified by XRD, TEM, FT-IR and TGA. The size of OA-modified NC is a mean diameter of 5-10 nm and can be dispersed in common organic solvents to form a transparent solution. The optical loss of NCs in organic solvent is the first time to discuss in this work. The luminescence properties of NCs were also characterized and studied by fluorescence spectrometer. The nanoparticles in solid and in the solution all exhibited the strong emission at the 1060 nm when the materials were excited around 800 nm. Compared with the LaF3 and CaF2 matrix, NaYF4 as the host can protect the Nd3+ ions more efficiently away from the nonradiative transitions. The longest luminescent lifetime of the solid NaYF4:2%Nd NCs was up to 136 μs, and the little difference of the fluorescence lifetime existed between the NCs in solid state and in solution. The low optical loss in organic solvent indicated that the Nd3+ ions-doped fluoride NCs are promising materials for optical amplification fields.

Intrinsic properties and strengthening mechanism of monocrystalline Ni-containing ternary concentrated solid solutions

DOE PAGES

Jin, K.; Gao, Y. F.; Bei, H.

2017-04-07

Ternary single-phase concentrated solid solution alloys (SP-CSAs), so-called "medium entropy alloys", not only possess notable mechanical and physical properties but also form a model system linking the relatively simple binary alloys to the complex high entropy alloys. Our knowledge of their intrinsic properties is vital to understand the material behavior and to prompt future applications. To this end, three model alloys NiCoFe, NiCoCr, and NiFe-20Cr have been selected and grown as single crystals. We measured their elastic constants using an ultrasonic method, and several key materials properties, such as shear modulus, bulk modulus, elastic anisotropy, and Debye temperatures have beenmore » derived. Furthermore, nanoindentation tests have been performed on these three alloys together with Ni, NiCo and NiFe on their (100) surface, to investigate the strengthening mechanisms. NiCoCr has the highest hardness, NiFe, NiCoFe and NiFe-20Cr share a similar hardness that is apparently lower than NiCoCr; NiCo has the lowest hardness in the alloys, which is similar to elemental Ni. The Labusch-type solid solution model has been applied to interpret the nanoindentation data, with two approaches used to calculate the lattice mismatch. Finally, by adopting an interatomic spacing matrix method, the Labusch model can reasonably predict the hardening effects for the whole set of materials.« less

Impact of Extraction Parameters on the Recovery of Lipolytic Activity from Fermented Babassu Cake

PubMed Central

Silva, Jaqueline N.; Godoy, Mateus G.; Gutarra, Melissa L. E.; Freire, Denise M. G.

2014-01-01

Enzyme extraction from solid matrix is as important step in solid-state fermentation to obtain soluble enzymes for further immobilization and application in biocatalysis. A method for the recovery of a pool of lipases from Penicillium simplicissimum produced by solid-state fermentation was developed. For lipase recovery different extraction solution was used and phosphate buffer containing Tween 80 and NaCl showed the best results, yielding lipase activity of 85.7 U/g and 65.7 U/g, respectively. The parameters with great impacts on enzyme extraction detected by the Plackett-Burman analysis were studied by Central Composite Rotatable experimental designs where a quadratic model was built showing maximum predicted lipase activity (160 U/g) at 25°C, Tween 80 0.5% (w/v), pH 8.0 and extraction solution 7 mL/g, maintaining constant buffer molarity of 0.1 M and 200 rpm. After the optimization process a 2.5 fold increase in lipase activity in the crude extract was obtained, comparing the intial value (64 U/g) with the experimental design (160 U/g), thus improving the overall productivity of the process. PMID:25090644

Ultra-thin Solid-State Li-Ion Electrolyte Membrane Facilitated by a Self-Healing Polymer Matrix.

PubMed

Whiteley, Justin M; Taynton, Philip; Zhang, Wei; Lee, Se-Hee

2015-11-18

Thin solid membranes are formed by a new strategy, whereby an in situ derived self-healing polymer matrix that penetrates the void space of an inorganic solid is created. The concept is applied as a separator in an all-solid-state battery with an FeS2 -based cathode and achieves tremendous performance for over 200 cycles. Processing in dry conditions represents a paradigm shift for incorporating high active-material mass loadings into mixed-matrix membranes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analytical Solution for the Critical Velocity of Pushing/Engulfment Transition

NASA Technical Reports Server (NTRS)

Catalina, Adrian V.; Stefanescu, Doru M.; Sen, Subhayu

2004-01-01

The distribution of ceramic particles in a metal matrix composite material depends primarily on the interaction of the particles with the solid/liquid interface during the solidification process. A numerical model that describes the evolution of the shape of the solid/liquid interface in the proximity of a foreign particle will presented in this paper. The model accounts for the influence of the temperature gradient and the Gibbs-Thomson and disjoining pressure effects. It shows that for the systems characterized by k(sub p) < k(sub L) the disjoining pressure causes the interface curvature to change its sign in the close-contact particle/interface region. It also shows that the increase of the temperature gradient diminishes the effect of the disjoining pressure. The analysis of the numerical results obtained for a large range of processing conditions and materials parameters has led to the development of an analytical solution for the critical velocity of pushing/engulfinent transition. The theoretical results will be discussed and compared with the experimental measurements performed under microgravity conditions.

Isolation and reversible dimerization of a selenium-selenium three-electron σ-bond.

PubMed

Zhang, Senwang; Wang, Xingyong; Su, Yuanting; Qiu, Yunfan; Zhang, Zaichao; Wang, Xinping

2014-06-11

Three-electron σ-bonding that was proposed by Linus Pauling in 1931 has been recognized as important in intermediates encountered in many areas. A number of three-electron bonding systems have been spectroscopically investigated in the gas phase, solution and solid matrix. However, X-ray diffraction studies have only been possible on simple noble gas dimer Xe∴Xe and cyclic framework-constrained N∴N radical cations. Here, we show that a diselena species modified with a naphthalene scaffold can undergo one-electron oxidation using a large and weakly coordinating anion, to afford a room-temperature-stable radical cation containing a Se∴Se three-electron σ-bond. When a small anion is used, a reversible dimerization with phase and marked colour changes is observed: radical cation in solution (blue) but diamagnetic dimer in the solid state (brown). These findings suggest that more examples of three-electron σ-bonds may be stabilized and isolated by using naphthalene scaffolds together with large and weakly coordinating anions.

On the superposition of strengthening mechanisms in dispersion strengthened alloys and metal-matrix nanocomposites: Considerations of stress and energy

NASA Astrophysics Data System (ADS)

Ferguson, J. B.; Schultz, Benjamin F.; Venugopalan, Dev; Lopez, Hugo F.; Rohatgi, Pradeep K.; Cho, Kyu; Kim, Chang-Soo

2014-03-01

Yield strength improvement in dispersion strengthened alloys and nano particle-reinforced composites by well-known strengthening mechanisms such as solid solution, grain refinement, coherent and incoherent dispersed particles, and increased dislocation density resulting from work-hardening can all be described individually. However, there is no agreed upon description of how these mechanisms combine to determine the yield strength. In this work, we propose an analytical yield strength prediction model combining arithmetic and quadratic addition approaches based on the consideration of two types of yielding mechanisms; stress-activated and energy-activated. Using data available in the literature for materials of differing grain sizes, we consider the cases of solid solutions and coherent precipitates to show that they follow stress-activated behavior. Then, we applied our model with some empirical parameters to precipitationhardenable materials of various grain sizes in both coherent and incoherent precipitate conditions, which demonstrated that grain boundary and Orowan-strengthening can be treated as energy-activated mechanisms.

The numerical approach adopted in toba computer code for mass and heat transfer dynamic analysis of metal hydride hydrogen storage beds

DOE Office of Scientific and Technical Information (OSTI.GOV)

El Osery, I.A.

1983-12-01

Modelling studies of metal hydride hydrogen storage beds is a part of an extensive R and D program conducted in Egypt on hydrogen energy. In this context two computer programs; namely RET and RET1; have been developed. In RET computer program, a cylindrical conduction bed model is considered and an approximate analytical solution is used for solution of the associated mass and heat transfer problem. This problem is solved in RET1 computer program numerically allowing more flexibility in operating conditions but still limited to cylindrical configuration with only two alternatives for heat exchange; either fluid is passing through tubes imbeddedmore » in the solid alloy matrix or solid rods are surrounded by annular fluid tubes. The present computer code TOBA is more flexible and realistic. It performs the mass and heat transfer dynamic analysis of metal hydride storage beds using a variety of geometrical and operating alternatives.« less

Processing and fabrication of mixed uranium/refractory metal carbide fuels with liquid-phase sintering

NASA Astrophysics Data System (ADS)

Knight, Travis W.; Anghaie, Samim

2002-11-01

Optimization of powder processing techniques were sought for the fabrication of single-phase, solid-solution mixed uranium/refractory metal carbide nuclear fuels - namely (U, Zr, Nb)C. These advanced, ultra-high temperature nuclear fuels have great potential for improved performance over graphite matrix, dispersed fuels tested in the Rover/NERVA program of the 1960s and early 1970s. Hypostoichiometric fuel samples with carbon-to-metal ratios of 0.98, uranium metal mole fractions of 5% and 10%, and porosities less than 5% were fabricated. These qualities should provide for the longest life and highest performance capability for these fuels. Study and optimization of processing methods were necessary to provide the quality assurance of samples for meaningful testing and assessment of performance for nuclear thermal propulsion applications. The processing parameters and benefits of enhanced sintering by uranium carbide liquid-phase sintering were established for the rapid and effective consolidation and formation of a solid-solution mixed carbide nuclear fuel.

Influence of thickness and permeability of endothelial surface layer on transmission of shear stress in capillaries

NASA Astrophysics Data System (ADS)

Zhang, SongPeng; Zhang, XiangJun; Tian, Yu; Meng, YongGang; Lipowsky, Herbert

2015-07-01

The molecular coating on the surface of microvascular endothelium has been identified as a barrier to transvascular exchange of solutes. With a thickness of hundreds of nanometers, this endothelial surface layer (ESL) has been treated as a porous domain within which fluid shear stresses are dissipated and transmitted to the solid matrix to initiate mechanotransduction events. The present study aims to examine the effects of the ESL thickness and permeability on the transmission of shear stress throughout the ESL. Our results indicate that fluid shear stresses rapidly decrease to insignificant levels within a thin transition layer near the outer boundary of the ESL with a thickness on the order of ten nanometers. The thickness of the transition zone between free fluid and the porous layer was found to be proportional to the square root of the Darcy permeability. As the permeability is reduced ten-fold, the interfacial fluid and solid matrix shear stress gradients increase exponentially two-fold. While the interfacial fluid shear stress is positively related to the ESL thickness, the transmitted matrix stress is reduced by about 50% as the ESL thickness is decreased from 500 to 100 nm, which may occur under pathological conditions. Thus, thickness and permeability of the ESL are two main factors that determine flow features and the apportionment of shear stresses between the fluid and solid phases of the ESL. These results may shed light on the mechanisms of force transmission through the ESL and the pathological events caused by alterations in thickness and permeability of the ESL.

Implications of Chirality of Drugs and Excipients in Physical Pharmacy.

NASA Astrophysics Data System (ADS)

Duddu, Sarma P.

1993-01-01

The interactions of enantiomers of a chiral drug with other chemical entities, which may lead to changes and stereoselective differences in the physicochemical properties of the drug, were investigated. The various interactions described below employed ephedrine, pseudoephedrine and some of their salts, and to a minor extent, propranolol hydrochloride. The interaction of ephedrinium or pseudoephedrinium with the achiral anion, salicylate, yielded crystalline salts with the notable exception of homochiral ephedrine. Racemic ephedrinium salicylate exists as a centrosymmetric crystal (P2_1/n) whereas racemic pseudoephedrinium salicylate is a mixture of homochiral crystals (P2 _1). The inability of ephedrinium to exist as a homochiral salicylate salt is attributed to a high energy conformation of the ephedrinium cation, following conformational analysis. Arising from conformationally favorable interactions, the crystallization of racemic ephedrinium salicylate from aqueous solutions was utilized to improve the enantiomeric purity of a partially resolved mixture of ephedrine from 60% to 82% in one crystallization step. Interaction of the opposite enantiomers of ephedrine and pseudoephedrine in the solid, liquid, solution and vapor state produced the respective racemic compounds. The formation of racemic ephedrine in the solid state as predominantly second order (k = 392 mol^{-1} hr^{-1}), probably mediated by the vapor phase. The formation of racemic pseudoephedrine was predominantly diffusion-controlled in the solid state via an intermediate non-crystalline phase. The interaction with traces of the opposite enantiomer during crystallization of (RS)-(-)-ephedrinium 2-naphthalenesulfonate and (SS)-(+)-pseudoephedrinium salicylate changed pharmaceutically important solid state properties, including dissolution rate. Uptake of the enantiomeric impurity was measured by a new, sensitive HPLC method. The enantiomeric impurity, at mole fractions <= 0.0027 greatly increased the lattice disorder, i.e. entropy, measured calorimetrically. The release of propranolol hydrochloride from a sustained-release matrix containing HPMC and racemic propranolol hydrochloride was stereoselective, though variable, suggesting a differential interaction of the two enantiomers with the hydrated chiral matrix. Thus, the interaction of a chiral drug with other chemical entities leads to significant, interpretable changes in the physicochemical properties of the drug, which may have important implications in the design and development of reliable and effective solid dosage forms.

Heat treatment giving a stable high temperature micro-structure in cast austenitic stainless steel

DOEpatents

Anton, Donald L.; Lemkey, Franklin D.

1988-01-01

A novel micro-structure developed in a cast austenitic stainless steel alloy and a heat treatment thereof are disclosed. The alloy is based on a multicomponent Fe-Cr-Mn-Mo-Si-Nb-C system consisting of an austenitic iron solid solution (.gamma.) matrix reinforced by finely dispersed carbide phases and a heat treatment to produce the micro-structure. The heat treatment includes a prebraze heat treatment followed by a three stage braze cycle heat treatment.

Chemical weathering rates of a soil chronosequence on granitic alluvium: III. Hydrochemical evolution and contemporary solute fluxes and rates

USGS Publications Warehouse

White, A.F.; Schulz, M.S.; Vivit, D.V.; Blum, A.E.; Stonestrom, David A.; Harden, J.W.

2005-01-01

Although long-term changes in solid-state compositions of soil chronosequences have been extensively investigated, this study presents the first detailed description of the concurrent hydrochemical evolution and contemporary weathering rates in such sequences. The most direct linkage between weathering and hydrology over 3 million years of soil development in the Merced chronosequence in Central California relates decreasing permeability and increasing hydrologic heterogeneity to the development of secondary argillic horizons and silica duripans. In a highly permeable, younger soil (40 kyr old), pore water solutes reflect seasonal to decadal-scale variations in rainfall and evapotranspiration (ET). This climate signal is strongly damped in less permeable older soils (250 to 600 kyr old) where solutes increasingly reflect weathering inputs modified by heterogeneous flow. Elemental balances in the soils are described in terms of solid state, exchange and pore water reservoirs and input/output fluxes from precipitation, ET, biomass, solute discharge and weathering. Solute mineral nutrients are strongly dependent on biomass variations as evidenced by an apparent negative K weathering flux reflecting aggradation by grassland plants. The ratios of solute Na to other base cations progressively increase with soil age. Discharge fluxes of Na and Si, when integrated over geologic time, are comparable to solid-state mass losses in the soils, implying similar past weathering conditions. Similarities in solute and sorbed Ca/Mg ratios reflect short-term equilibrium with the exchange reservoir. Long-term consistency in solute ratios, when contrasted against progressive decreases in solid-state Ca/Mg, requires an additional Ca source, probably from dry deposition. Amorphous silica precipitates from thermodynamically-saturated pore waters during periods of high evapotranspiration and result in the formation of duripans in the oldest soils. The degree of feldspar and secondary gibbsite and kaolinite saturation varies both spatially and temporally due to the seasonality of plant-respired CO2 and a decrease in organically complexed Al. In deeper pore waters, K-feldspar is in equilibrium and plagioclase is about an order of magnitude undersaturated. Hydrologic heterogeneity produces a range of weathering gradients that are constrained by solute distributions and matrix and macropore flow regimes. Plagioclase weathering rates, based on precipitation-corrected Na gradients, vary between 3 and 7 ?? 10-16 mol m-2 s-1. These rates are similar to previously determined solid-state rates but are several orders of magnitude slower than for experimental plagioclase dissolution indicating strong inhibitions to natural weathering, partly due to near-equilibrium weathering reactions. Copyright ?? 2005 Elsevier Ltd.

Flash Vacuum Pyrolysis: Techniques and Reactions.

PubMed

Wentrup, Curt

2017-11-20

Flash vacuum pyrolysis (FVP) had its beginnings in the 1940s and 1950s, mainly through mass spectrometric detection of pyrolytically formed free radicals. In the 1960s many organic chemists started performing FVP experiments with the purpose of isolating new and interesting compounds and understanding pyrolysis processes. Meanwhile, many different types of apparatus and techniques have been developed, and it is the purpose of this review to present the most important methods as well as a survey of typical reactions and observations that can be achieved with the various techniques. This includes preparative FVP, chemical trapping reactions, matrix isolation, and low temperature spectroscopy of reactive intermediates and unstable molecules, the use of online mass, photoelectron, microwave, and millimeterwave spectroscopies, gas-phase laser pyrolysis, pulsed pyrolysis with supersonic jet expansion, very low pressure pyrolysis for kinetic investigations, solution-spray and falling-solid FVP for involatile compounds, and pyrolysis over solid supports and reagents. Moreover, the combination of FVP with matrix isolation and photochemistry is a powerful tool for investigations of reaction mechanism. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrafine Ceramic Grains Embedded in Metallic Glass Matrix: Achieving Superior Wear Resistance via Increase in Both Hardness and Toughness.

PubMed

Yang, Lina; Wen, Mao; Dai, Xuan; Cheng, Gang; Zhang, Kan

2018-05-09

As structural materials, crystalline or metallic glass materials have attracted scientific and practical interests. However, some mechanisms involving critical size and shear bands have adverse effects on their mechanical properties. Here, we counter these two effects by introducing a special structure with ultrafine ceramic grains (with a diameter of ∼2.0 nm) embedded into a metallic glass matrix, wherein the grains are mainly composed of a Ta-W-N solid solution structure in nature, surrounded by a W-based amorphous matrix that contains Ta and N atoms. Such a structure is in situ formed during preparation, which combines the merits of both phases to achieve simultaneous increase in hardness and toughness relative to references (pure TaN and W) and thus superior wear resistance. Even more remarkable, a favorable variation of increased hardness but reduced elasticity modulus can be induced by this structure. Intrinsically, ultrafine ceramic grains (free of dislocations), embedded in the metallic glass matrix, could prevent shear band propagation within the glass matrix and further improve the hardness of the matrix material. In return, such glass matrix allows for stiffness neutralization and structural relaxation to reduce the elasticity modulus of ceramic grains. This study will offer a new guidance to fabricate ultrahigh-performance metal-based composites.

Parallel computation using boundary elements in solid mechanics

NASA Technical Reports Server (NTRS)

Chien, L. S.; Sun, C. T.

1990-01-01

The inherent parallelism of the boundary element method is shown. The boundary element is formulated by assuming the linear variation of displacements and tractions within a line element. Moreover, MACSYMA symbolic program is employed to obtain the analytical results for influence coefficients. Three computational components are parallelized in this method to show the speedup and efficiency in computation. The global coefficient matrix is first formed concurrently. Then, the parallel Gaussian elimination solution scheme is applied to solve the resulting system of equations. Finally, and more importantly, the domain solutions of a given boundary value problem are calculated simultaneously. The linear speedups and high efficiencies are shown for solving a demonstrated problem on Sequent Symmetry S81 parallel computing system.

Theoretical analysis for the specific heat and thermal parameters of solid C60

NASA Astrophysics Data System (ADS)

Soto, J. R.; Calles, A.; Castro, J. J.

1997-08-01

We present the results of a theoretical analysis for the thermal parameters and phonon contribution to the specific heat in solid C60. The phonon contribution to the specific heat is calculated through the solution of the corresponding dynamical matrix, for different points in the Brillouin zone, and the construccion of the partial and generalized phonon density of states. The force constants are obtained from a first principle calculation, using a SCF Hartree-Fock wave function from the Gaussian 92 program. The thermal parameters reported are the effective temperatures and vibrational amplitudes as a function of temperature. Using this model we present a parametization scheme in order to reproduce the general behaviour of the experimental specific heat for these materials.

Defining the Role of Solid Stress and Matrix Stiffness in Cancer Cell Proliferation and Metastasis

PubMed Central

Kalli, Maria; Stylianopoulos, Triantafyllos

2018-01-01

Solid tumors are characterized by an abnormal stroma that contributes to the development of biomechanical abnormalities in the tumor microenvironment. In particular, these abnormalities include an increase in matrix stiffness and an accumulation of solid stress in the tumor interior. So far, it is not clearly defined whether matrix stiffness and solid stress are strongly related to each other or they have distinct roles in tumor progression. Moreover, while the effects of stiffness on tumor progression are extensively studied compared to the contribution of solid stress, it is important to ascertain the biological outcomes of both abnormalities in tumorigenesis and metastasis. In this review, we discuss how each of these parameters is evolved during tumor growth and how these parameters are influenced by each other. We further review the effects of matrix stiffness and solid stress on the proliferative and metastatic potential of cancer and stromal cells and summarize the in vitro experimental setups that have been designed to study the individual contribution of these parameters. PMID:29594037

DOE Office of Scientific and Technical Information (OSTI.GOV)

Secchieri, M.; Benassi, C.A.; Pastore, S.

A method for the quail-quantitative evaluation of pentachlorophenol (PCP) in solid matrixes has been developed. The procedure is based on solid-liquid extraction of solid samples (leather or wood), followed by purification on a cyanopropyl column and determination of the preservative by second derivative UV spectroscopy considering the PCP A peak-through value (304-297 nm). The method allows rapid PCP determination in the concentration range 1-40 micrograms/mL; any matrix interference is avoided by the purification step and recoveries of the preservative were 99.12% (RSD% 0.13) for the leather matrix and 98.03 (RSD% 0.17) for the wood matrix.

Analysis of biogenic carbonates by inductively coupled plasma-mass spectrometry (ICP-MS). Flow injection on-line solid-phase preconcentration for trace element determination in fish otoliths.

PubMed

Arslan, Z; Paulson, A J

2002-04-01

The aragonite deposits within the ear bones (otoliths) of teleost fish retain a chemical signal reflecting the life history of fish (similar to rings of trees) and the nature of fish habitats. Otoliths dissolved in acid solutions contain high concentrations of calcium and a variety of proteins. Elimination of matrix salts and organic interferences during preconcentration is essential for accurate determination of trace elements in otolith solutions by inductively coupled plasma-quadrupole mass spectrometry. An iminodiacetate-based chelating resin (Toyopearl AF-Chelate 650 M) has been used for on-line preconcentration and matrix separation for the determination of 31 transition and rare elements. Successful preconcentration of the elements was achieved at pH 5 by on-line buffering, except Mn which required pH 8.8. Sample solutions were loaded on to the column for 1 min at 3.2 mL min(-1), and then eluted directly into the mass spectrometer with 4% v/v nitric acid. This procedure enabled up to 25-fold preconcentration with successful removal of the calcium matrix. The effect of heat-assisted oxidation with concentrated nitric acid was investigated to eliminate the organic matrix. It was found that heating to dryness after dissolution and further mineralization with the acid significantly improved the retention of the transition elements. The method was validated by analysis of a certified reference material produced from saggittal otoliths of emperor snapper ( Lutjanus sebae), and then applied to the determination of trace metal concentrations in juvenile bluefin tuna ( Thunnus thynnus) from the Western Pacific Ocean.

Molecular interactions in high conductive gel electrolytes based on low molecular weight gelator.

PubMed

Bielejewski, Michał; Łapiński, Andrzej; Demchuk, Oleg

2017-03-15

Organic ionic gel (OIG) electrolytes, also known as gel electrolytes or ionogels are one example of modern functional materials with the potential to use in wide range of electrochemical applications. The functionality of OIGs arises from the thermally reversible solidification of electrolytes or ionic liquids and their superior ionic conductivity. To understand and to predict the properties of these systems it is important to get the knowledge about the interactions on molecular level between the solid gelator matrix and the electrolyte solution. This paper reports the spectroscopic studies (FT-IR, UV-Vis and Raman) of the gel electrolyte based on low molecular weight gelator methyl-4,6-O-(p-nitrobenzylidene)-α-d-glucopyranoside and solution of quaternary ammonium salt, tetramethylammonium bromide. The solidification process was based on sol-gel technique. Below characteristic temperature, defined as gel to sol phase transition temperature, T gs , the samples were solid-like and showed high conductivity values of the same order as observed for pure liquid electrolytes. The investigations were performed for a OIGs in a wide range of molar concentrations of the electrolyte solution. Copyright © 2016 Elsevier Inc. All rights reserved.

Separation, preconcentration and inductively coupled plasma-mass spectrometric (ICP-MS) determination of thorium(IV), titanium(IV), iron(III), lead(II) and chromium(III) on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin.

PubMed

Aydin, Funda Armagan; Soylak, Mustafa

2010-01-15

A simple and effective method is presented for the separation and preconcentration of Th(IV), Ti(IV), Fe(III), Pb(II) and Cr(III) by solid phase extraction on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin prior to their inductively coupled plasma-mass spectrometric determinations. The influence of analytical parameters including pH of the aqueous solution, flow rates of sample and eluent solutions and sample volume on the quantitative recoveries of analyte ions was investigated. Matrix effects caused by the presence of alkali, earth alkali and some metal ions in the analyzed solutions were investigated. The presented solid phase extraction method was applied to BCR-144R Sewage Sludge (domestic origin), BCR-141R Calcareous Loam Soil, NIST 1568a Rice Flour and NIST 1577b Bovine Liver certified reference materials (CRMs) for the determination of analyte ions and the results were in good agreement with the certified values. The separation procedure presented was also applied to the various natural water samples collected from Turkey with satisfactory results.

A porous flow approach to model thermal non-equilibrium applicable to melt migration

NASA Astrophysics Data System (ADS)

Schmeling, Harro; Marquart, Gabriele; Grebe, Michael

2018-01-01

We develop an approach for heat exchange between a fluid and a solid phase of a porous medium where the temperatures of the fluid and matrix are not in thermal equilibrium. The formulation considers moving of the fluid within a resting or deforming porous matrix in an Eulerian coordinate system. The approach can be applied, for example, to partially molten systems or to brine transport in porous rocks. We start from an existing theory for heat exchange where the energy conservation equations for the fluid and the solid phases are separated and coupled by a heat exchange term. This term is extended to account for the full history of heat exchange. It depends on the microscopic geometry of the fluid phase. For the case of solid containing hot, fluid-filled channels, we derive an expression based on a time-dependent Fourier approach for periodic half-waves. On the macroscopic scale, the temporal evolution of the heat exchange leads to a convolution integral along the flow path of the solid, which simplifies considerably in case of a resting matrix. The evolution of the temperature in both phases with time is derived by inserting the heat exchange term into the energy equations. We explore the effects of thermal non-equilibrium between fluid and solid by considering simple cases with sudden temperature differences between fluid and solid as initial or boundary conditions, and by varying the fluid velocity with respect to the resting porous solid. Our results agree well with an analytical solution for non-moving fluid and solid. The temperature difference between solid and fluid depends on the Peclet number based on the Darcy velocity. For Peclet numbers larger than 1, the temperature difference after one diffusion time reaches 5 per cent of \\tilde{T} or more (\\tilde{T} is a scaling temperature, e.g. the initial temperature difference). Thus, our results imply that thermal non-equilibrium can play an important role for melt migration through partially molten systems where melt focuses into melt channels near the transition to melt ascent by dykes. Our method is based on solving the convolution integration for the heat exchange over the full flow history, which is numerically expensive. We tested to replace the heat exchange term by an instantaneous, approximate term. We found considerable errors on the short timescale, but a good agreement on the long timescale if appropriate parameters for the approximate terms are used. We derived these parameters which may be implemented in fully dynamical two-phase flow formulations of melt migration in the Earth.

A novel anti-frictional multiphase layer produced by plasma nitriding of PVD titanium coated ZL205A aluminum alloy

NASA Astrophysics Data System (ADS)

Lu, C.; Yao, J. W.; Wang, Y. X.; Zhu, Y. D.; Guo, J. H.; Wang, Y.; Fu, H. Y.; Chen, Z. B.; Yan, M. F.

2018-02-01

The heat treatment (consisting of solid solution and aging), is integrated with the nitriding process of titanium coated ZL205A aluminum alloy to improve the surface and matrix mechanical properties simultaneously. Two-step duplex treatment is adopted to prepare the gradient multiphase layer on a magnesium-free ZL205A aluminum-copper based alloy. Firstly, pure titanium film is deposited on the aluminum alloy substrate using magnetron sputtering. Secondly, the Ti-coated specimen is nitrided at the solid solution temperature of the substrate alloying elements in a gas mixture of N2 and H2 and aged at 175 °C. The microstructure evolution, microhardness as well as the wear resistance of obtained multiphase layers are investigated by means of scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometer (EDS), microhardness tester and pin-on-disc tribometer. The multiphase layer, dominated by TiN0.3 or Al3Ti, is prepared with significantly increased layer depth after duplex treatment. The surface hardness of multiphase layer is remarkably improved from 23.7HV to 457HV. The core matrix hardness is also increased to 65HV after aging. The wear rate of the multiphase layer decreases about 55.22% and 49.28% in comparison with the aged and Ti coated specimens, respectively. The predominant wear mechanism for the multiphase layer is abrasive and oxidation, but severe adhesive wear for the aged and Ti coated specimens.

Radiation-induced microcrystal shape change as a mechanism of wasteform degradation

NASA Astrophysics Data System (ADS)

Ojovan, Michael I.; Burakov, Boris E.; Lee, William E.

2018-04-01

Experiments with actinide-containing insulating wasteforms such as devitrified glasses containing 244Cm, Ti-pyrochlore, single-phase La-monazite, Pu-monazite ceramics, Eu-monazite and zircon single crystals containing 238Pu indicate that mechanical self-irradiation-induced destruction may not reveal itself for many years (even decades). The mechanisms causing these slowly-occurring changes remain unknown therefore in addition to known mechanisms of wasteform degradation such as matrix swelling and loss of solid solution we have modelled the damaging effects of electrical fields induced by the decay of radionuclides in clusters embedded in a non-conducting matrix. Three effects were important: (i) electric breakdown; (ii) cluster shape change due to dipole interaction, and (iii) cluster shape change due to polarisation interaction. We reveal a critical size of radioactive clusters in non-conducting matrices so that the matrix material can be damaged if clusters are larger than this critical size. The most important parameters that control the matrix integrity are the radioactive cluster (inhomogeneity) size, specific radioactivity, and effective matrix electrical conductivity. We conclude that the wasteform should be as homogeneous as possible and even electrically conductive to avoid potential damage caused by electrical charges induced by radioactive decay.

Photoinduced crystallization of calcium carbonate from a homogeneous precursor solution in the presence of partially hydrolyzed poly(vinyl alcohol)

NASA Astrophysics Data System (ADS)

Nishio, Takashi; Naka, Kensuke

2015-04-01

Photoinduced crystallization of calcium carbonate (CaCO3) was demonstrated by the photodecarboxylation of ketoprofen (KP, 2-(3-benzoylphenyl)propionic acid) under alkaline conditions (pH 10). In this method, a homogeneous solution comprising KP, calcium chloride, ammonia, and partially hydrolyzed poly(vinyl alcohol) (PVAPS, degree of saponification: 86.5-89.0 mol %) was used as the precursor solution and was exposed to ultraviolet (UV) irradiation for different time periods. Thermogravimetric analysis of the obtained xerogels showed that increasing the UV irradiation time increased the amount of CaCO3 formed and the complete conversion of calcium ions to calcite was achieved after 50 min of UV irradiation. Furthermore, solid phase analyses suggested that nanometer-to-micron-sized calcite crystals were formed and dispersed in the obtained PVAPS matrix.

The Microstructure and Properties of Super Martensitic Stainless Steel Microalloyed with Tungsten and Copper

NASA Astrophysics Data System (ADS)

Ye, Dong; Li, Jun; Liu, Yu-Rong; Yong, Qi-Long; Su, Jie; Cao, Jian-Chun; Tao, Jing-Mei; Zhao, Kun-Yu

2011-06-01

The microstructure and properties of super martensitic stainless steel (SMSS) microalloyed with tungsten and copper were studied by means of optical microscopy, dilatometer, X-ray diffraction, and tensile tests. The results showed that the microstructure of SMSS, after quenching and tempering, was a typical biphase structure with tempered martensite and reversed austenite dispersedly distributed in the martensite matrix. W and Cu were added into the SMSS to reduce the transformation temperature (Ms) and improve the strength and hardness of the matrix by grain refining and solid solution strengthening. Thermocalc calculations confirmed that M23C6 compound and Laves phase were precipitated during tempering in the investigated steel. Compared with the traditional SMSS, the steel microalloyed with W and Cu performed better mechanical properties.

From solid solution to cluster formation of Fe and Cr in α-Zr

NASA Astrophysics Data System (ADS)

Burr, P. A.; Wenman, M. R.; Gault, B.; Moody, M. P.; Ivermark, M.; Rushton, M. J. D.; Preuss, M.; Edwards, L.; Grimes, R. W.

2015-12-01

To understand the mechanisms by which the re-solution of Fe and Cr additions increase the corrosion rate of irradiated Zr alloys, the solubility and clustering of Fe and Cr in model binary Zr alloys was investigated using a combination of experimental and modelling techniques - atom probe tomography (APT), x-ray diffraction (XRD), thermoelectric power (TEP) and density functional theory (DFT). Cr occupies both interstitial and substitutional sites in the α-Zr lattice; Fe favours interstitial sites, and a low-symmetry site that was not previously modelled is found to be the most favourable for Fe. Lattice expansion as a function of Fe and Cr content in the α-Zr matrix deviates from Vegard's law and is strongly anisotropic for Fe additions, expanding the c-axis while contracting the a-axis. Matrix content of solutes cannot be reliably estimated from lattice parameter measurements, instead a combination of TEP and APT was employed. Defect clusters form at higher solution concentrations, which induce a smaller lattice strain compared to the dilute defects. In the presence of a Zr vacancy, all two-atom clusters are more soluble than individual point defects and as many as four Fe or three Cr atoms could be accommodated in a single Zr vacancy. The Zr vacancy is critical for the increased apparent solubility of defect clusters; the implications for irradiation induced microstructure changes in Zr alloys are discussed.

Determination of Aroclor 1260 in soil samples by gas chromatography with mass spectrometry and solid-phase microextraction.

PubMed

Zhang, Mengliang; Jackson, Glen P; Kruse, Natalie A; Bowman, Jennifer R; Harrington, Peter de B

2014-10-01

A novel fast screening method was developed for the determination of polychlorinated biphenyls that are constituents of the commercial mixture, Aroclor 1260, in soil matrices by gas chromatography with mass spectrometry combined with solid-phase microextraction. Nonequilibrium headspace solid-phase microextraction with a 100 μm polydimethylsiloxane fiber was used to extract polychlorinated biphenyls from 0.5 g of soil matrix. The use of 2 mL of saturated potassium dichromate in 6 M sulfuric acid solution improved the reproducibility of the extractions and the mass transfer of the polychlorinated biphenyls from the soil matrix to the microextraction fiber via the headspace. The extraction time was 30 min at 100°C. The percent recoveries, which were evaluated using an Aroclor 1260 standard and liquid injection, were within the range of 54.9-65.7%. Two-way extracted ion chromatogram data were used to construct calibration curves. The relative error was <±15% and the relative standard deviation was <15%, which are respective measures of the accuracy and precision. The method was validated with certified soil samples and the predicted concentrations for Aroclor 1260 agreed with the certified values. The method was demonstrated to be linear from 10 to 1000 ng/g for Aroclor 1260 in dry soil. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multi-cut solutions in Chern-Simons matrix models

NASA Astrophysics Data System (ADS)

Morita, Takeshi; Sugiyama, Kento

2018-04-01

We elaborate the Chern-Simons (CS) matrix models at large N. The saddle point equations of these matrix models have a curious structure which cannot be seen in the ordinary one matrix models. Thanks to this structure, an infinite number of multi-cut solutions exist in the CS matrix models. Particularly we exactly derive the two-cut solutions at finite 't Hooft coupling in the pure CS matrix model. In the ABJM matrix model, we argue that some of multi-cut solutions might be interpreted as a condensation of the D2-brane instantons.

Solid-Phase Extraction Strategies to Surmount Body Fluid Sample Complexity in High-Throughput Mass Spectrometry-Based Proteomics

PubMed Central

Bladergroen, Marco R.; van der Burgt, Yuri E. M.

2015-01-01

For large-scale and standardized applications in mass spectrometry- (MS-) based proteomics automation of each step is essential. Here we present high-throughput sample preparation solutions for balancing the speed of current MS-acquisitions and the time needed for analytical workup of body fluids. The discussed workflows reduce body fluid sample complexity and apply for both bottom-up proteomics experiments and top-down protein characterization approaches. Various sample preparation methods that involve solid-phase extraction (SPE) including affinity enrichment strategies have been automated. Obtained peptide and protein fractions can be mass analyzed by direct infusion into an electrospray ionization (ESI) source or by means of matrix-assisted laser desorption ionization (MALDI) without further need of time-consuming liquid chromatography (LC) separations. PMID:25692071

Composite solid-state scintillators for neutron detection

DOEpatents

Dai, Sheng; Im, Hee-Jung; Pawel, Michelle D.

2006-09-12

Applicant's present invention is a composite scintillator for neutron detection comprising a matrix material fabricated from an inorganic sol-gel precursor solution homogeneously doped with a liquid scintillating material and a neutron absorbing material. The neutron absorbing material yields at least one of an electron, a proton, a triton, an alpha particle or a fission fragment when the neutron absorbing material absorbs a neutron. The composite scintillator further comprises a liquid scintillating material in a self-assembled micelle formation homogeneously doped in the matrix material through the formation of surfactant-silica composites. The scintillating material is provided to scintillate when traversed by at least one of an electron, a proton, a triton, an alpha particle or a fission fragment. The scintillating material is configured such that the matrix material surrounds the micelle formation of the scintillating material. The composite scintillator is fabricated and applied as a thin film on substrate surfaces, a coating on optical fibers or as a glass material.

Elevated-Temperature Deformation Properties of a HfC Modified Ti-48Al-2Mn-2Nb Matrix Particulate Composite

NASA Technical Reports Server (NTRS)

Whittenberger, J. D.; Farmer, S. C.; Bors, D. A.; Ray, R.; Lee, D. S.

1994-01-01

Rapid solidification techniques in combination with HIPing have been used to produce Ti-48Al-2Mn-2Nb and a Ti-48Al-2Mn-2Nb+15 wt% HfC composite. While the composite does contain several second phases within the gamma + alpha(sub 2) matrix, none was identified to be HfC. The elevated-temperature properties were determined by constant velocity compression and constant load tensile testing in air between 1000 and 1173 K. Such testing indicated that the elevated temperature strengths of the HfC-modified aluminide was superior to those of the unreinforced matrix with the best 1100 K temperature slow strain rate properties for both materials being achieved after high-temperature annealing prior to testing. Examination of the microstructures after deformation in combination with the measured stress exponents and activation energies suggest that creep resistance of the HfC-modified form is due to solid-solution strengthening from carbon and hafnium rather than the presence of second phases.

Chiroplasmonic magnetic gold nanocomposites produced by one-step aqueous method using κ-carrageenan.

PubMed

Lesnichaya, Marina V; Sukhov, Boris G; Aleksandrova, Galina P; Gasilova, Ekaterina R; Vakul'skaya, Tamara I; Khutsishvili, Spartak S; Sapozhnikov, Anatoliy N; Klimenkov, Igor V; Trofimov, Boris A

2017-11-01

Novel water-soluble chiroplasmonic nanobiocomposites with directly varied gold content were synthesized by a one-step redox method in water using a biocompatible polysaccharide κ-carrageenan (industrial product from algae) as both reducing and stabilizing matrix. The influence of the reactants ratio, temperature, and pH on the reaction was studied and the optimal reaction parameters were found. The structure and the properties of composite nanomaterials were examined in solid state and aqueous solutions by using complementary physical-chemical methods X-ray diffraction analysis, transmission electron microscopy, spectroscopy of electron paramagnetic resonance, atomic absorption and optical spectroscopy, polarimetry including optical rotatory dispersion with registration of interphase-crossbred Cotton effect of a chiral polysaccharide matrix on plasmonic chromophore of gold nanoparticles, dynamic and static light scattering. The new perspective multi-purpose nanocomposites demonstrate a complex of chiroplasmonic and magnetic properties, imparted by both nanoparticles and radicals enriched chiral polysaccharide matrix. Copyright © 2017 Elsevier Ltd. All rights reserved.

Dispersoid reinforced alloy powder and method of making

DOEpatents

Anderson, Iver E; Rieken, Joel

2013-12-10

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with an introduced reactive species than does the alloying element and wherein one or more atomizing parameters is/are modified to controllably reduce the amount of the reactive species, such as oxygen, introduced into the atomized particles so as to reduce anneal times and improve reaction (conversion) to the desired strengthening dispersoids in the matrix. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies are made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.

Quantitative fluorescence measurements performed on typical matrix molecules in matrix-assisted laser desorption/ionisation

NASA Astrophysics Data System (ADS)

Allwood, D. A.; Dyer, P. E.

2000-11-01

Fundamental photophysical parameters have been determined for several molecules that are commonly used as matrices, e.g. ferulic acid, within matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. Fluorescence quantum efficiencies ( φqe), singlet decay rates ( kl), vibrationless ground-singlet transition energies and average fluorescence wavelengths have been obtained from solid and solution samples by quantitative optical measurements. This new data will assist in modelling calculations of MALDI processes and in highlighting desirable characteristics of MALDI matrices. φqe may be as high as 0.59 whilst the radiative decay rate ( kf) appears to be within the (0.8-4)×10 8 s -1 range. Interestingly, α-cyano-4-hydroxycinnamic acid (α-CHC) has a very low φqe and fast non-radiative decay rate which would imply a rapid and efficient thermalisation of electronic excitation. This is in keeping with observations that α-CHC exhibits low threshold fluences for ion detection and the low fluences at which α-CHC tends to fragment.

Disintegration of the net-shaped grain-boundary phase by multi-directional forging and its influence on the microstructure and properties of Cu-Ni-Si alloy

NASA Astrophysics Data System (ADS)

Zhang, Jinlong; Lu, Zhenlin; Zhao, Yuntao; Jia, Lei; Xie, Hui; Tao, Shiping

2017-09-01

Cu-Ni-Si alloys with 90% Cu content and Ni to Si ratios of 5:1 were fabricated by fusion casting, and severe plastic deformation of the Cu-Ni-Si alloy was carried out by multi-direction forging (MDF). The results showed that the as-cast and homogenized Cu-Ni-Si alloys consisted of three phases, namely the matrix phase α-Cu (Ni, Si), the reticular grain boundary phase Ni31Si12 and the precipitated phase Ni2Si. MDF significantly destroyed the net-shaped grain boundary phase, the Ni31Si12 phase and refined the grain size of the Cu matrix, and also resulted in the dissolving of Ni2Si precipitates into the Cu matrix. The effect of MDF on the conductivity of the solid solution Cu-Ni-Si alloy was very significant, with an average increase of 165.16%, and the hardness of the Cu-Ni-Si alloy also increased obviously.

Friction Stir Processing of Copper-Coated SiC Particulate-Reinforced Aluminum Matrix Composite

PubMed Central

Huang, Chih-Wei; Aoh, Jong-Ning

2018-01-01

In the present work, we proposed a novel friction stir processing (FSP) to produce a locally reinforced aluminum matrix composite (AMC) by stirring copper-coated SiC particulate reinforcement into Al6061 alloy matrix. Electroless-plating process was applied to deposit the copper surface coating on the SiC particulate reinforcement for the purpose of improving the interfacial adhesion between SiC particles and Al matrix. The core-shell SiC structure provides a layer for the atomic diffusion between aluminum and copper to enhance the cohesion between reinforcing particles and matrix on one hand, the dispersion of fine copper in the Al matrix during FSP provides further dispersive strengthening and solid solution strengthening, on the other hand. Hardness distribution and tensile results across the stir zone validated the novel concept in improving the mechanical properties of AMC that was realized via FSP. Optical microscope (OM) and Transmission Electron Microscopy (TEM) investigations were conducted to investigate the microstructure. Energy dispersive spectrometer (EDS), electron probe micro-analyzer (EPMA), and X-ray diffraction (XRD) were explored to analyze the atomic inter-diffusion and the formation of intermetallic at interface. The possible strengthening mechanisms of the AMC containing Cu-coated SiC particulate reinforcement were interpreted. The concept of strengthening developed in this work may open a new way of fabricating of particulate reinforced metal matrix composites. PMID:29652846

Applications of inductively coupled plasma mass spectrometry and laser ablation inductively coupled plasma mass spectrometry in materials science

NASA Astrophysics Data System (ADS)

Becker, Johanna Sabine

2002-12-01

Inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) have been applied as the most important inorganic mass spectrometric techniques having multielemental capability for the characterization of solid samples in materials science. ICP-MS is used for the sensitive determination of trace and ultratrace elements in digested solutions of solid samples or of process chemicals (ultrapure water, acids and organic solutions) for the semiconductor industry with detection limits down to sub-picogram per liter levels. Whereas ICP-MS on solid samples (e.g. high-purity ceramics) sometimes requires time-consuming sample preparation for its application in materials science, and the risk of contamination is a serious drawback, a fast, direct determination of trace elements in solid materials without any sample preparation by LA-ICP-MS is possible. The detection limits for the direct analysis of solid samples by LA-ICP-MS have been determined for many elements down to the nanogram per gram range. A deterioration of detection limits was observed for elements where interferences with polyatomic ions occur. The inherent interference problem can often be solved by applying a double-focusing sector field mass spectrometer at higher mass resolution or by collision-induced reactions of polyatomic ions with a collision gas using an ICP-MS fitted with collision cell. The main problem of LA-ICP-MS is quantification if no suitable standard reference materials with a similar matrix composition are available. The calibration problem in LA-ICP-MS can be solved using on-line solution-based calibration, and different procedures, such as external calibration and standard addition, have been discussed with respect to their application in materials science. The application of isotope dilution in solution-based calibration for trace metal determination in small amounts of noble metals has been developed as a new calibration strategy. This review discusses new analytical developments and possible applications of ICP-MS and LA-ICP-MS for the quantitative determination of trace elements and in surface analysis for materials science.

Rapid Sintering of Li₂O-Nb₂O₅-TiO₂ Solid Solution by Air Pressure Control and Clarification of Its Mechanism.

PubMed

Nakano, Hiromi; Kamimoto, Konatsu; Yamamoto, Takahisa; Furuta, Yoshio

2018-06-11

We first successfully synthesized Li 1+ x − y Nb 1− x −3 y Ti x +4 y O₃ (LNT) solid solutions (0.13 ≤ x ≤ 0.18, 0 ≤ y ≤ 0.06) rapidly at 1373 K for one hour under 0.35 MPa by the controlling of air pressure using an air-pressure control atmosphere furnace. The composition is a formation area of a superstructure for LNT, in which the periodical intergrowth layer was formed in the matrix, and where it can be controlled by Ti content. Therefore, the sintering time depended on Ti content, and annealing was repeated for over 24 h until a homogeneous structure was formed using a conventional electric furnace. We clarified the mechanism of the rapid sintering using various microscale to nanoscale characterization techniques: X-ray diffraction, a scanning electron microscope, a transmission electron microscope (TEM), a Cs-corrected scanning TEM equipped with electron energy-loss spectroscopy, and X-ray absorption fine structure spectroscopy.

Elastic moduli and thermal expansion coefficients of medium-entropy subsystems of the CrMnFeCoNi high-entropy alloy

DOE PAGES

Laplanche, Guillaume; Gadaud, P.; Barsch, C.; ...

2018-02-23

Elastic moduli of a set of equiatomic alloys (CrFeCoNi, CrCoNi, CrFeNi, FeCoNi, MnCoNi, MnFeNi, and CoNi), which are medium-entropy subsystems of the CrMnFeCoNi high-entropy alloy were determined as a function of temperature over the range 293 K–1000 K. Thermal expansion coefficients were determined for these alloys over the temperature range 100 K–673 K. All alloys were single-phase and had the face-centered cubic (FCC) crystal structure, except CrFeNi which is a two-phase alloy containing a small amount of body-centered cubic (BCC) precipitates in a FCC matrix. The temperature dependences of thermal expansion coefficients and elastic moduli obtained here are useful formore » quantifying fundamental aspects such as solid solution strengthening, and for structural analysis/design. Furthermore, using the above results, the yield strengths reported in literature for these alloys were normalized by their shear moduli to reveal the influence of shear modulus on solid solution strengthening.« less

Improved strategies for postoligomerization synthesis of oligodeoxynucleotides bearing structurally defined adducts at the N2 position of deoxyguanosine.

PubMed

DeCorte, B L; Tsarouhtsis, D; Kuchimanchi, S; Cooper, M D; Horton, P; Harris, C M; Harris, T M

1996-01-01

Improved methodology has been developed for preparation of oligodeoxynucleotides bearing adducts on the N2 position of guanine in which the adduction reaction is carried out in homogeneous solution rather than while the oligonucleotide is immobilized on a solid matrix. The methodology utilizes a new synthon, 2-fluoro-O6-(trimethylsilylethyl)-2'-deoxyinosine (3). Nucleoside 3 is stable to the conditions of oligonucleotide synthesis, but the O6 protection is eliminated under very mild conditions following displacement of the 2-fluoro group by amine nucleophiles. Oligonucleotides containing 3 could be removed from the solid support by treatment with 0.1 M NaOH (8 h, rt) without disruption of 3. Reaction of the crude, partially deprotected oligonucleotide with (R)-2-amino-2-phenylethanol in homogeneous solution, followed by removal of the remaining protective groups with NH4OH (60 degrees C, 8 h) and then 0.1% acetic acid, gave the adducted oligonucleotide in good purity and yield. Alternatively, fully deprotected oligonucleotide containing 3 could be prepared by use of labile phenoxyacetyl-type protecting groups on the exocyclic amino groups.

Synthesis, fluorescence, TGA and crystal structure of thiazolyl-pyrazolines derived from chalcones

NASA Astrophysics Data System (ADS)

Suwunwong, T.; Chantrapromma, S.; Fun, H.-K.

2015-04-01

Thiazolyl-pyrazolines 3a-3d were synthesized in a three step procedure using chalcones as starting materials and characterized by FT-IR, UV-Vis, and 1H NMR techniques. The crystal structure of compound 3a was also determined by X-ray diffraction analysis. Compound 3a crystallized out in the orthorhombic P212121 space group with the unit cell dimensions: a = 5.2106(2) Å, b = 12.4341(5) Å, c = 33.3254(13) Å, α = β = γ = 90°, V = 2159.12(15) Å3, Z = 4, D cald = 1.372 M gm-3 and F(000) = 928. Fluorescence of 3a-3d were studied in solid state and acetonitrile solution. It was found that, these compounds exhibit the green fluorescence light (506-508 nm) in both solid and solution states. The pH stability on fluorescence property and the thermal gravimetric analysis of compound 3a were specifically carried out. It was revealed that 3a shows high thermal stability up to around 250°C and presenting high stability in various pH ranges in the acetonitrilewater matrix.

Effects of drug-carrier interactions on drug dissolution from binary and ternary matrices

NASA Astrophysics Data System (ADS)

Iqbal, Zafar

For nearly five decades, pharmaceutical researchers have studied solid solutions of drugs in polymers as a potential means to enhance the dissolution of drugs with poor aqueous solubility. This has become of greater importance in recent years because most new potential drug compounds (new chemical entities) exhibit poor water solubility and present great challenges to scientists who must design dosage forms from which the drugs are bioavailable. During the formulation of a solid solution, the drug undergoes physical but not chemical alterations that increase its chemical potential in the formulation relative to that of the pure drug in its stable form. This increased chemical potential is responsible for enhanced dissolution as well as physical instabilities, such as amorphous to crystalline conversions and precipitation within the solid state. The chemical potential is derived from the Gibbs free energy, so it is reasonable to explain the behavior of solid solution systems in terms of thermodynamics. Solid solutions and dispersions have been extensively studied by pharmaceutical scientists, both with regard to manufacturing aspects and the proposal of various models in attempts to explain the physical bases for how these systems work. Recently, Dave and Bellantone proposed a model based on the thermodynamic changes resulting from the formulation of binary solid solutions of a drug in the polymer PVP. Their model introduced a modification of the F-H theory, which was used to quantify the drug-polymer interaction energies and calculate the entropy of mixing of the drug and polymer. In this work, the model of Dave and Bellantone was extended to include three-component systems, consisting of one drug mixed in a carrier matrix consisting of mixture of two polymers or a polymer and a surfactant. For this research, solid solutions were formed using various drug weight fractions in the formulations. The study focused on the following points: (1) Prepare solid solution formulations and perform appropriate physical characterizations. (2) Characterize the increase in drug dissolution rates resulting from solid solution formulations. (3) Relate the initial dissolution rates to the drug solubility. (4) Explain the solubility enhancement from solid solution dosage in terms of the drug polymer interactions using the extended thermodynamic model. Two poorly water soluble drugs, levonorgestrel (LEVO) and ethinyl estradiol (EE) were formulated in seven solid solution preparations comprised of four carrier systems. Materials used as carriers included various combinations of the polymers PVP K-30, Copovidone (COP), Poloxamer 182, and the surfactant TweenRTM 20. Additionally, ibuprofen (IBU) was used in three formulations consisting of various combinations of PVP K-30, Copovidone and TweenRTM 20. Formulations with various drug weight fractions (0.5%--30%) were prepared using the solvent evaporation technique. Each formulation was tested for dissolution using intrinsic dissolution apparatus (USP). The solid solutions were compressed into tablets into the sample die that maintained a constant surface area during the dissolution process. DSC, XRD and NIRS scans identified that the crystalline peaks of the drug disappeared with the addition of the polymer for all ratios of EE, indicating the formation of solid solutions (to within the limits of detection of the equipment). This was also observed for the LEVO dispersions up to 10% drug loading. At higher drug loading, solutions were formed but some small degree crystallinity was also present. For each experiment, the initial dissolution rates were obtained from the slope of the mass dissolved vs. time plots taken at early times, and volume normalized initial dissolution rates RV were calculated by dividing the initial dissolution rate by the volume fraction of the drug in the formulation. Comparison of the RV values for the various formulations with a reference RV (typically that of the pure drug or of the formulation with the highest polymer content) allowed calculation of relative volume normalized dissolution rates (RNV). The various RNV were used in the thermodynamic model for data analyses and to determine the interactions between the drug and carrier molecules. It was generally seen that RNV increased with decreased drug fraction, and was adequately modeled by the equations derived from the extended thermodynamic model. It was concluded that the model proposed for the binary and ternary systems successfully represented the mechanism of drug-polymer interaction and the energy changes taken place within the dispersion systems. The dissolution data analysis and subsequent understanding of physical modifications in the dispersion systems characterized by XRD, NIRS and DSC further substantiated the findings. The understanding of the fundamental physical might help scientists to predict the effects of mixing various drugs and polymers, and the effects of varying ratios.

Stabilization of pH in solid-matrix hydroponic systems

NASA Technical Reports Server (NTRS)

Frick, J.; Mitchell, C. A.

1993-01-01

2-[N-morpholino]ethanesulfonic acid (MES) buffer or Amberlite DP-1 (cation-exchange resin beads) were used to stabilize substrate pH of passive-wicking, solid-matrix hydroponic systems in which small canopies of Brassica napus L. (CrGC 5-2, genome : ACaacc) were grown to maturity. Two concentrations of MES (5 or 10 mM) were included in Hoagland 1 nutrient solution. Alternatively, resin beads were incorporated into the 2 vermiculite : 1 perlite (v/v) growth medium at 6% or 12% of total substrate volume. Both strategies stabilized pH without toxic side effects on plants. Average seed yield rates for all four pH stabilization treatments (13.3 to 16.9 g m-2 day-1) were about double that of the control (8.2 g m-2 day-1), for which there was no attempt to buffer substrate pH. Both the highest canopy seed yield rate (16.9 g m-2 day-1) and the highest shoot harvest index (19.5%) occurred with the 6% resin bead treatment, even though the 10 mM MES and 12% bead treatments maintained pH within the narrowest limits. The pH stabilization methods tested did not significantly affect seed oil and protein contents.

Electrosprayed core-shell solid dispersions of acyclovir fabricated using an epoxy-coated concentric spray head.

PubMed

Liu, Zhe-Peng; Cui, Lei; Yu, Deng-Guang; Zhao, Zhuan-Xia; Chen, Lan

2014-01-01

A novel structural solid dispersion (SD) taking the form of core-shell microparticles for poorly water-soluble drugs is reported for the first time. Using polyvinylpyrrolidone (PVP) as a hydrophilic polymer matrix, the SDs were fabricated using coaxial electrospraying (characterized by an epoxy-coated concentric spray head), although the core fluids were unprocessable using one-fluid electrospraying. Through manipulating the flow rates of the core drug-loaded solutions, two types of core-shell microparticles with tunable drug contents were prepared. They had average diameters of 1.36±0.67 and 1.74±0.58 μm, and were essentially a combination of nanocomposites with the active ingredient acyclovir (ACY) distributed in the inner core, and the sweeter sucralose and transmembrane enhancer sodium dodecyl sulfate localized in the outer shell. Differential scanning calorimetry and X-ray diffraction results demonstrated that ACY, sodium dodecyl sulfate, and sucralose were well distributed in the PVP matrix in an amorphous state because of favorable second-order interactions. In vitro dissolution and permeation studies showed that the core-shell microparticle SDs rapidly freed ACY within 1 minute and promoted nearly eightfold increases in permeation rate across the sublingual mucosa compared with raw ACY powders.

Multiple Changes to Reusable Solid Rocket Motors, Identifying Hidden Risks

NASA Technical Reports Server (NTRS)

Greenhalgh, Phillip O.; McCann, Bradley Q.

2003-01-01

The Space Shuttle Reusable Solid Rocket Motor (RSRM) baseline is subject to various changes. Changes are necessary due to safety and quality improvements, environmental considerations, vendor changes, obsolescence issues, etc. The RSRM program has a goal to test changes on full-scale static test motors prior to flight due to the unique RSRM operating environment. Each static test motor incorporates several significant changes and numerous minor changes. Flight motors often implement multiple changes simultaneously. While each change is individually verified and assessed, the potential for changes to interact constitutes additional hidden risk. Mitigating this risk depends upon identification of potential interactions. Therefore, the ATK Thiokol Propulsion System Safety organization initiated the use of a risk interaction matrix to identify potential interactions that compound risk. Identifying risk interactions supports flight and test motor decisions. Uncovering hidden risks of a full-scale static test motor gives a broader perspective of the changes being tested. This broader perspective compels the program to focus on solutions for implementing RSRM changes with minimal/mitigated risk. This paper discusses use of a change risk interaction matrix to identify test challenges and uncover hidden risks to the RSRM program.

Sorptive tape extraction in the analysis of the volatile fraction emitted from biological solid matrices.

PubMed

Bicchi, C; Cordero, C; Liberto, E; Rubiolo, P; Sgorbini, B; Sandra, P

2007-05-04

Sorptive tape extraction (STE) is a recent sorption-based sampling technique in which a flexible polydimethylsiloxane (PDMS) tape is used to recover analytes at the surface of a solid matrix by direct contact as well as from the headspace in equilibrium with it. Solutes thus enriched on the inert PDMS material can be recovered either by solvent desorption or by thermo-desorption. The concentration capability of both direct contact and headspace STE was evaluated by sampling (a) aromatic plants to study the reaction of a vegetable matrix submitted to stress, and (b) fruits at the surface of the pulp or inside the pulp; the composition of the volatile fraction released from the skin when a perfume is sprayed on the back of the hand was also studied. The concentration capability of direct contact and headspace STE was compared to that of HSSE with a 20 microL PDMS twister and HS-SPME with a PDMS 100 microm fibre, by determining the relative abundances (RA) of the characterizing components of the aromatic plants under investigation. Repeatability and influence of tape surface on STE recovery were also evaluated.

Engineered glass seals for solid-oxide fuel cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Surdoval, Wayne; Lara-Curzio, Edgar; Stevenson, Jeffry

2017-02-07

A seal for a solid oxide fuel cell includes a glass matrix having glass percolation therethrough and having a glass transition temperature below 650.degree. C. A deformable second phase material is dispersed in the glass matrix. The second phase material can be a compliant material. The second phase material can be a crushable material. A solid oxide fuel cell, a precursor for forming a seal for a solid oxide fuel cell, and a method of making a seal for a solid oxide fuel cell are also disclosed.

Notch Sensitivity of Woven Ceramic Matrix Composites Under Tensile Loading: An Experimental, Analytical, and Finite Element Study

NASA Technical Reports Server (NTRS)

Haque, A.; Ahmed, L.; Ware, T.; Jeelani, S.; Verrilli, Michael J. (Technical Monitor)

2001-01-01

The stress concentrations associated with circular notches and subjected to uniform tensile loading in woven ceramic matrix composites (CMCs) have been investigated for high-efficient turbine engine applications. The CMC's were composed of Nicalon silicon carbide woven fabric in SiNC matrix manufactured through polymer impregnation process (PIP). Several combinations of hole diameter/plate width ratios and ply orientations were considered in this study. In the first part, the stress concentrations were calculated measuring strain distributions surrounding the hole using strain gages at different locations of the specimens during the initial portion of the stress-strain curve before any microdamage developed. The stress concentration was also calculated analytically using Lekhnitskii's solution for orthotropic plates. A finite-width correction factor for anisotropic and orthotropic composite plate was considered. The stress distributions surrounding the circular hole of a CMC's plate were further studied using finite element analysis. Both solid and shell elements were considered. The experimental results were compared with both the analytical and finite element solutions. Extensive optical and scanning electron microscopic examinations were carried out for identifying the fracture behavior and failure mechanisms of both the notched and notched specimens. The stress concentration factors (SCF) determined by analytical method overpredicted the experimental results. But the numerical solution underpredicted the experimental SCF. Stress concentration factors are shown to increase with enlarged hole size and the effects of ply orientations on stress concentration factors are observed to be negligible. In all the cases, the crack initiated at the notch edge and propagated along the width towards the edge of the specimens.

Approximate method of variational Bayesian matrix factorization/completion with sparse prior

NASA Astrophysics Data System (ADS)

Kawasumi, Ryota; Takeda, Koujin

2018-05-01

We derive the analytical expression of a matrix factorization/completion solution by the variational Bayes method, under the assumption that the observed matrix is originally the product of low-rank, dense and sparse matrices with additive noise. We assume the prior of a sparse matrix is a Laplace distribution by taking matrix sparsity into consideration. Then we use several approximations for the derivation of a matrix factorization/completion solution. By our solution, we also numerically evaluate the performance of a sparse matrix reconstruction in matrix factorization, and completion of a missing matrix element in matrix completion.

Solid supports for extraction and preconcentration of proteins and peptides in microfluidic devices: A review.

PubMed

Dziomba, Szymon; Araya-Farias, Monica; Smadja, Claire; Taverna, Myriam; Carbonnier, Benjamin; Tran, N Thuy

2017-02-22

Determination of proteins and peptides is among the main challenges of today's bioanalytical chemistry. The application of microchip technology in this field is an exhaustively developed concept that aims to create integrated and fully automated analytical devices able to quantify or detect one or several proteins from a complex matrix. Selective extraction and preconcentration of targeted proteins and peptides especially from biological fluids is of the highest importance for a successful realization of these microsystems. Incorporation of solid structures or supports is a convenient solution employed to face these demands. This review presents a critical view on the latest achievements in sample processing techniques for protein determination using solid supports in microfluidics. The study covers the period from 2006 to 2015 and focuses mainly on the strategies based on microbeads, monolithic materials and membranes. Less common approaches are also briefly discussed. The reviewed literature suggests future trends which are discussed in the concluding remarks. Copyright © 2016 Elsevier B.V. All rights reserved.

A simple and rapid in situ preconcentration method for the determination of phosphate in environmental waters by use of solid-phase extraction, and its applications to brackish lake waters.

PubMed

Okumura, M; Tong, L; Fujinaga, K; Seike, Y

2001-05-01

A simple and rapid in situ preconcentration method for the determination of phosphate in environmental waters has been developed for field analysis. This method is based on solid-phase extraction on a zirconium-loaded Sep-Pack Accell CM cartridge (Zr-SP) and is applicable to studies in which sampling is performed by use of a graduated syringe to prevent contamination and to ensure easy operation at sampling sites. The Zr-SP cartridge was prepared by passing 0.1 mol L(-1) zirconium solution through a Sep-Pak Accell CM cartridge, packed with cation exchange sorbent based on a silica matrix. The adsorption of phosphate and its desorption depend only on the pH of the solution. A water sample containing phosphate was adjusted to pH 2 and passed through the Zr-SP cartridge to collect it. The retained phosphate was quantitatively eluted with 0.5 mol L(-1) sodium hydroxide solution. The phosphate retained in the Zr-SP cartridge was stable for at least one month. The established preconcentration method was successfully applied to brackish lake waters to investigate seasonal changes in the distribution and behavior of phosphate in a brackish lake.

Effects of polyurethane matrices on fungal tannase and gallic acid production under solid state culture*

PubMed Central

Treviňo, Lucia; Contreras-Esquivel, Juan C.; Rodríguez-Herrera, Raul; Aguilar, Cristóbal Noé

2007-01-01

The influence of the physical structure of polyurethane matrix as a support in a solid state culture in tannase production and gallic acid accumulation by Aspergillus niger Aa-20 was evaluated. Three different polyurethane matrices were used as the support: continuous, semi-discontinuous and discontinuous. The highest tannase production at 2479.59 U/L during the first 12 h of culture was obtained using the discontinuous matrix. The gallic acid was accumulated at 7.64 g/L at the discontinuous matrix. The results show that the discontinuous matrix of polyurethane is better for tannase production and gallic acid accumulation in a solid state culture bioprocess than the continuous and semi-discontinuous matrices. PMID:17910122

Solid-state NMR for bacterial biofilms

NASA Astrophysics Data System (ADS)

Reichhardt, Courtney; Cegelski, Lynette

2014-04-01

Bacteria associate with surfaces and one another by elaborating an extracellular matrix to encapsulate cells, creating communities termed biofilms. Biofilms are beneficial in some ecological niches, but also contribute to the pathogenesis of serious and chronic infectious diseases. New approaches and quantitative measurements are needed to define the composition and architecture of bacterial biofilms to help drive the development of strategies to interfere with biofilm assembly. Solid-state nuclear magnetic resonance (NMR) is uniquely suited to the examination of insoluble and complex macromolecular and whole-cell systems. This article highlights three examples that implement solid-state NMR to deliver insights into bacterial biofilm composition and changes in cell-wall composition as cells transition to the biofilm lifestyle. Most recently, solid-state NMR measurements provided a total accounting of the protein and polysaccharide components in the extracellular matrix of an Escherichia coli biofilm and transformed our qualitative descriptions of matrix composition into chemical parameters that permit quantitative comparisons among samples. We present additional data for whole biofilm samples (cells plus the extracellular matrix) that complement matrix-only analyses. The study of bacterial biofilms by solid-state NMR is an exciting avenue ripe with many opportunities and we close the article by articulating some outstanding questions and future directions in this area.

Quantum-dot-in-perovskite solids.

PubMed

Ning, Zhijun; Gong, Xiwen; Comin, Riccardo; Walters, Grant; Fan, Fengjia; Voznyy, Oleksandr; Yassitepe, Emre; Buin, Andrei; Hoogland, Sjoerd; Sargent, Edward H

2015-07-16

Heteroepitaxy-atomically aligned growth of a crystalline film atop a different crystalline substrate-is the basis of electrically driven lasers, multijunction solar cells, and blue-light-emitting diodes. Crystalline coherence is preserved even when atomic identity is modulated, a fact that is the critical enabler of quantum wells, wires, and dots. The interfacial quality achieved as a result of heteroepitaxial growth allows new combinations of materials with complementary properties, which enables the design and realization of functionalities that are not available in the single-phase constituents. Here we show that organohalide perovskites and preformed colloidal quantum dots, combined in the solution phase, produce epitaxially aligned 'dots-in-a-matrix' crystals. Using transmission electron microscopy and electron diffraction, we reveal heterocrystals as large as about 60 nanometres and containing at least 20 mutually aligned dots that inherit the crystalline orientation of the perovskite matrix. The heterocrystals exhibit remarkable optoelectronic properties that are traceable to their atom-scale crystalline coherence: photoelectrons and holes generated in the larger-bandgap perovskites are transferred with 80% efficiency to become excitons in the quantum dot nanocrystals, which exploit the excellent photocarrier diffusion of perovskites to produce bright-light emission from infrared-bandgap quantum-tuned materials. By combining the electrical transport properties of the perovskite matrix with the high radiative efficiency of the quantum dots, we engineer a new platform to advance solution-processed infrared optoelectronics.

Elastic strain field due to an inclusion of a polyhedral shape with a non-uniform lattice misfit

NASA Astrophysics Data System (ADS)

Nenashev, A. V.; Dvurechenskii, A. V.

2017-03-01

An analytical solution in a closed form is obtained for the three-dimensional elastic strain distribution in an unlimited medium containing an inclusion with a coordinate-dependent lattice mismatch (an eigenstrain). Quantum dots consisting of a solid solution with a spatially varying composition are examples of such inclusions. It is assumed that both the inclusion and the surrounding medium (the matrix) are elastically isotropic and have the same Young's modulus and Poisson ratio. The inclusion shape is supposed to be an arbitrary polyhedron, and the coordinate dependence of the lattice misfit, with respect to the matrix, is assumed to be a polynomial of any degree. It is shown that, both inside and outside the inclusion, the strain tensor is expressed as a sum of contributions of all faces, edges, and vertices of the inclusion. Each of these contributions, as a function of the observation point's coordinates, is a product of some polynomial and a simple analytical function, which is the solid angle subtended by the face from the observation point (for a contribution of a face), or the potential of the uniformly charged edge (for a contribution of an edge), or the distance from the vertex to the observation point (for a contribution of a vertex). The method of constructing the relevant polynomial functions is suggested. We also found out that similar expressions describe an electrostatic or gravitational potential, as well as its first and second derivatives, of a polyhedral body with a charge/mass density that depends on coordinates polynomially.

End-Member Formulation of Solid Solutions and Reactive Transport

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lichtner, Peter C.

2015-09-01

A model for incorporating solid solutions into reactive transport equations is presented based on an end-member representation. Reactive transport equations are solved directly for the composition and bulk concentration of the solid solution. Reactions of a solid solution with an aqueous solution are formulated in terms of an overall stoichiometric reaction corresponding to a time-varying composition and exchange reactions, equivalent to reaction end-members. Reaction rates are treated kinetically using a transition state rate law for the overall reaction and a pseudo-kinetic rate law for exchange reactions. The composition of the solid solution at the onset of precipitation is assumed tomore » correspond to the least soluble composition, equivalent to the composition at equilibrium. The stoichiometric saturation determines if the solid solution is super-saturated with respect to the aqueous solution. The method is implemented for a simple prototype batch reactor using Mathematica for a binary solid solution. Finally, the sensitivity of the results on the kinetic rate constant for a binary solid solution is investigated for reaction of an initially stoichiometric solid phase with an undersaturated aqueous solution.« less

Application of symbolic/numeric matrix solution techniques to the NASTRAN program

NASA Technical Reports Server (NTRS)

Buturla, E. M.; Burroughs, S. H.

1977-01-01

The matrix solving algorithm of any finite element algorithm is extremely important since solution of the matrix equations requires a large amount of elapse time due to null calculations and excessive input/output operations. An alternate method of solving the matrix equations is presented. A symbolic processing step followed by numeric solution yields the solution very rapidly and is especially useful for nonlinear problems.

Effect of solute immobilization on the stability problem within the fractional model in the solute analog of the Horton-Rogers-Lapwood problem.

PubMed

Klimenko, Lyudmila S; Maryshev, Boris S

2017-11-24

The paper is devoted to the linear stability analysis within the solute analogue of the Horton-Rogers-Lapwood (HRL) problem. The solid nanoparticles are treated as solute within the continuous approach. Therefore, we consider the infinite horizontal porous layer saturated with a mixture (carrier fluid and solute). Solute transport in porous media is very often complicated by solute immobilization on a solid matrix of porous media. Solute immobilization (solute sorption) is taken into account within the fractal model of the MIM approach. According to this model a solute in porous media immobilizes within random time intervals and the distribution of such random variable does not have a finite mean value, which has a good agreement with some experiments. The solute concentration difference between the layer boundaries is assumed as constant. We consider two cases of horizontal external filtration flux: constant and time-modulated. For the constant flux the system of equations that determines the frequency of neutral oscillations and the critical value of the Rayleigh-Darcy number is derived. Neutral curves of the critical parameters on the governing parameters are plotted. Stability maps are obtained numerically in a wide range of parameters of the system. We have found that taking immobilization into account leads to an increase in the critical value of the Rayleigh-Darcy number with an increase in the intensity of the external filtration flux. The case of weak time-dependent external flux is investigated analytically. We have shown that the modulated external flux leads to an increase in the critical value of the Rayleigh-Darcy number and a decrease in the critical wave number. For moderate time-dependent filtration flux the differential equation with Caputo fractional derivatives has been obtained for the description of the behavior near the convection instability threshold. This equation is analyzed numerically by the Floquet method; the parametric excitation of convection is observed.

Infrared spectroscopy of water clusters isolated in methane matrices: Effects of isotope substitution and annealing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yamakawa, Koichiro, E-mail: koichiro.yamakawa@gakushuin.ac.jp; Ehara, Namika; Ozawa, Nozomi

2016-07-15

Using infrared-active solvents of CH{sub 4} and CD{sub 4} for matrix isolation, we measured infrared spectra of H{sub 2}O and D{sub 2}O clusters at 7 K. The solute-concentration dependence of the spectrum of H{sub 2}O clusters in a CH{sub 4} matrix was investigated and was used for the peak assignment. Annealing procedures were found to promote the size growth of water clusters in methane matrices for all the combinations of (H{sub 2}O, CH{sub 4}), (H{sub 2}O, CD{sub 4}), (D{sub 2}O, CH{sub 4}), and (D{sub 2}O, CD{sub 4}). We also monitored the ν{sub 3} absorption due to methane to find themore » annealing-induced structural change only of solid CH{sub 4}. The matrix effects on the vibrations of the clusters are discussed on the basis of “T{sub c} plots”, where their frequencies are plotted as a function of the square root of the matrix critical temperature, T{sub c}. The obtained plots assure the validity of the assignment of the cluster peaks.« less

Zwitterionic Hydrogel-Biopolymer Assembly towards Biomimetic Superlubricants

NASA Astrophysics Data System (ADS)

Seekell, Raymond; Zhu, Elaine

2014-03-01

One superlubricant in nature is the synovial fluid (SF), comprising of a high molecular weight polysaccharide, hyaluronic acid (HA), and a globule protein, lubricin. In this bio-inspired materials research, we have explored hydrogel particles to mimic lubricin as a ``ball-bearing'' and control their interaction with the viscoelastic HA matrix. Biocompatible poly(N-[2-(Methacyloyloxy)ethyl]dimethyl-(3-sulfopropyl) ammonium hydroxide) (PMSA) hydrogel particles are synthesized to examine the electrostatic induced assembly of PMSA-HA supramolecular complexes in aqueous solutions. Fluorescence microscopy and rheology experiments have characterized the tunable network structure and viscoelastic properties of PMSA-HA aggregates by HA concentration and ionic conditions in aqueous solution. When being grafted to a solid surface, the PMSA-HA composite thin film exhibits superior low biofouling and friction performance, suggesting great promises as artificial superlubricants.

Solid-phase extraction of some heavy metal ions on a double-walled carbon nanotube disk and determination by flame atomic absorption spectrometry.

PubMed

Karatepe, Aslihan; Soylak, Mustafa; Elçi, Latif

2011-01-01

A new preconcentration method was developed for the determination of trace amounts of Cu(II), Fe(III), Pb(II), Ni(II), and Cd(II) on a double-walled carbon nanotube disk. 4-(2-Thiazolylazo) resorcinol was used as a complexing reagent. The effects of parameters, including pH of the solutions, amounts of complexing reagent, eluent type, sample volume, flow rates of solutions, and matrix ions were examined for quantitative recoveries of the studied analyte ions. The retained metal ions were eluted by 2 M HNO3. The LOD values for the analytes were in the range of 0.7-4.4 microg/mL. Natural water samples and standard reference materials were analyzed by the presented method.

Synergistic Strategy to Enhance the Thermoelectric Properties of CoSbS1-xSex Compounds via Solid Solution.

PubMed

Yao, Wei; Yang, Dingfeng; Yan, Yanci; Peng, Kunling; Zhan, Heng; Liu, Anping; Lu, Xu; Wang, Guoyu; Zhou, Xiaoyuan

2017-03-29

High thermal conductivity of CoSbS-based limited its own prospect application in thermoelectric energy conversion. Solid solution is an effective approach to optimize the performance of thermoelectric materials with high lattice thermal conductivity because of the enhanced phonons scattering from disorder atoms. In this paper, we have synthesized and measured the thermoelectric properties of solid solution CoSbS 1-x Se x (x = 0, 0.05, 0.10, 0.15, 0.20, 0.30) series samples. The collaborative optimization (enhancing the power factors and reducing the thermal conductivities) to add zT values were realized via substitution of S atoms with the isoelectronic Se atoms in the matrix. Meanwhile, the lowest room temperature lattice thermal conductivity in CoSbS-based materials is obtained (4.72 W m -1 K -1 ) at present. Benefiting from the results of synergistic strategy, a zT of 0.35 was achieved at 923 K for sample CoSbS 0.85 Se 0.15 , a 59% improvement as compared with that of the pristine CoSbS. Band calculation demonstrated that CoSbS 0.85 Se 0.15 present a similar band dispersion with CoSbS. The mechanism of point defect scattering for reducing the lattice thermal conductivity at room temperature, was also analyzed by the Callaway model. The contributions to decrease the room temperature lattice thermal conductivity from the mass and the strain fluctuation in the crystal are comparable. These results can also be extended to other high-efficiency thermoelectric materials with stiff bond and smaller Gruneisen parameters.

Developing dissolution testing methodologies for extended-release oral dosage forms with supersaturating properties. Case example: Solid dispersion matrix of indomethacin.

PubMed

Tajiri, Tomokazu; Morita, Shigeaki; Sakamoto, Ryosaku; Mimura, Hisahi; Ozaki, Yukihiro; Reppas, Christos; Kitamura, Satoshi

2015-07-25

The objective of this study was to develop an in vitro dissolution test method with discrimination ability for an extended-release solid dispersion matrix of a lipophilic drug using the United States Pharmacopeia (USP) Apparatus 4, flow-through cell apparatus. In the open-loop configuration, the sink condition was maintained by manipulating the flow rate of the dissolution medium. To evaluate the testing conditions, the drug release mechanism from an extended-release solid dispersion matrix containing hydrophobic and hydrophilic polymers was investigated. As the hydroxypropyl methylcellulose (HPMC) maintained concentrations of indomethacin higher than the solubility in a dissolution medium, the release of HPMC into the dissolution medium was also quantified using size-exclusion chromatography. We concluded that the USP Apparatus 4 is suitable for application to an in vitro dissolution method for orally administered extended-release solid dispersion matrix formulations containing poorly water-soluble drugs. Copyright © 2015 Elsevier B.V. All rights reserved.

Matrix Isolation Spectroscopy Applied to Positron Moderatioin in Cryogenic Solids

DTIC Science & Technology

2011-07-01

Current Positron Applications • 2-γ decay exploited in Positron Emission Tomography (PET) scanners. • Positrons localize & annihilate preferentially at...Air Force  Eglin Air Force Base AFRL-RW-EG-TP-2011-024 Matrix Isolation Spectroscopy Applied to Positron Moderation in Cryogenic Solids Distribution... Spectroscopy Applied to Positron Moderation in Cryogenic Solids 5a. CONTRACT NUMBER 5b. GRANT NUMBER 62602F 5c. PROGRAM ELEMENT NUMBER 6

Biobased, Internally pH-Sensitive Materials: Immobilized Yellow Fluorescent Protein as an Optical Sensor for Spatiotemporal Mapping of pH Inside Porous Matrices.

PubMed

Consolati, Tanja; Bolivar, Juan M; Petrasek, Zdenek; Berenguer, Jose; Hidalgo, Aurelio; Guisán, Jose M; Nidetzky, Bernd

2018-02-28

The pH is fundamental to biological function and its measurement therefore crucial across all biosciences. Unlike homogenous bulk solution, solids often feature internal pH gradients due to partition effects and confined biochemical reactions. Thus, a full spatiotemporal mapping for pH characterization in solid materials with biological systems embedded in them is essential. In here, therefore, a fully biocompatible methodology for real-time optical sensing of pH within porous materials is presented. A genetically encoded ratiometric pH sensor, the enhanced superfolder yellow fluorescent protein (sYFP), is used to functionalize the internal surface of different materials, including natural and synthetic organic polymers as well as silica frameworks. By using controlled, tailor-made immobilization, sYFP is homogenously distributed within these materials and so enables, via self-referenced imaging analysis, pH measurements in high accuracy and with useful spatiotemporal resolution. Evolution of internal pH is monitored in consequence of a proton-releasing enzymatic reaction, the hydrolysis of penicillin by a penicillin acylase, taking place in solution or confined to the solid surface of the porous matrix. Unlike optochemical pH sensors, which often interfere with biological function, labeling with sYFP enables pH sensing without altering the immobilized enzyme's properties in any of the materials used. Fast response of sYFP to pH change permits evaluation of biochemical kinetics within the solid materials. Thus, pH sensing based on immobilized sYFP represents a broadly applicable technique to the study of biology confined to the internally heterogeneous environment of solid matrices.

The generalised Sylvester matrix equations over the generalised bisymmetric and skew-symmetric matrices

NASA Astrophysics Data System (ADS)

Dehghan, Mehdi; Hajarian, Masoud

2012-08-01

A matrix P is called a symmetric orthogonal if P = P T = P -1. A matrix X is said to be a generalised bisymmetric with respect to P if X = X T = PXP. It is obvious that any symmetric matrix is also a generalised bisymmetric matrix with respect to I (identity matrix). By extending the idea of the Jacobi and the Gauss-Seidel iterations, this article proposes two new iterative methods, respectively, for computing the generalised bisymmetric (containing symmetric solution as a special case) and skew-symmetric solutions of the generalised Sylvester matrix equation ? (including Sylvester and Lyapunov matrix equations as special cases) which is encountered in many systems and control applications. When the generalised Sylvester matrix equation has a unique generalised bisymmetric (skew-symmetric) solution, the first (second) iterative method converges to the generalised bisymmetric (skew-symmetric) solution of this matrix equation for any initial generalised bisymmetric (skew-symmetric) matrix. Finally, some numerical results are given to illustrate the effect of the theoretical results.

Equations for normal-mode statistics of sound scattering by a rough elastic boundary in an underwater waveguide, including backscattering.

PubMed

Morozov, Andrey K; Colosi, John A

2017-09-01

Underwater sound scattering by a rough sea surface, ice, or a rough elastic bottom is studied. The study includes both the scattering from the rough boundary and the elastic effects in the solid layer. A coupled mode matrix is approximated by a linear function of one random perturbation parameter such as the ice-thickness or a perturbation of the surface position. A full two-way coupled mode solution is used to derive the stochastic differential equation for the second order statistics in a Markov approximation.

Electrochemical membrane incinerator

DOEpatents

Johnson, Dennis C.; Houk, Linda L.; Feng, Jianren

2001-03-20

Electrochemical incineration of p-benzoquinone was evaluated as a model for the mineralization of carbon in toxic aromatic compounds. A Ti or Pt anode was coated with a film of the oxides of Ti, Ru, Sn and Sb. This quaternary metal oxide film was stable; elemental analysis of the electrolyzed solution indicated the concentration of these metal ions to be 3 .mu.g/L or less. The anode showed good reactivity for the electrochemical incineration of benzoquinone. The use of a dissolved salt matrix as the so-called "supporting electrolyte" was eliminated in favor of a solid-state electrolyte sandwiched between the anode and cathode.

Experimental simulations of sulfide formation in the solar nebula.

PubMed

Lauretta, D S; Lodders, K; Fegley, B

1997-07-18

Sulfurization of meteoritic metal in H2S-H2 gas produced three different sulfides: monosulfide solid solution [(Fe,Ni)1-xS], pentlandite [(Fe,Ni)9-xS8], and a phosphorus-rich sulfide. The composition of the remnant metal was unchanged. These results are contrary to theoretical predictions that sulfide formation in the solar nebula produced troilite (FeS) and enriched the remaining metal in nickel. The experimental sulfides are chemically and morphologically similar to sulfide grains in the matrix of the Alais (class CI) carbonaceous chondrite, suggesting that these meteoritic sulfides may be condensates from the solar nebula.

Condensation from Cluster-IDP Enriched Vapor Inside the Snow Line: Implications for Mercury, Asteroids, and Enstatite Chondrites

NASA Technical Reports Server (NTRS)

Ebel, D. S.; Alexander, C. M. OD.

2005-01-01

Enstatite chondrites (EC) contain highly reduced matrix minerals (e.g.- (Mg,Fe,Mn)S solid solution, CaS) that probably formed in thermodynamic equilibrium with a vapor phase. EC chondrules contain enstatite, Fs5 to Fs30, in which iron was reduced after formation, also by interaction with vapor [1, 2]. The origin and location of this reducing vapor bears upon the formation of the terrestrial planets (Mercury to Mars), the remnant chemical zoning of the asteroid belt (E, S, C, D-types), and the cosmochemistry of metals in the early solar system.

Headspace versus direct immersion solid phase microextraction in complex matrixes: investigation of analyte behavior in multicomponent mixtures.

PubMed

Gionfriddo, Emanuela; Souza-Silva, Érica A; Pawliszyn, Janusz

2015-08-18

This work aims to investigate the behavior of analytes in complex mixtures and matrixes with the use of solid-phase microextraction (SPME). Various factors that influence analyte uptake such as coating chemistry, extraction mode, the physicochemical properties of analytes, and matrix complexity were considered. At first, an aqueous system containing analytes bearing different hydrophobicities, molecular weights, and chemical functionalities was investigated by using commercially available liquid and solid porous coatings. The differences in the mass transfer mechanisms resulted in a more pronounced occurrence of coating saturation in headspace mode. Contrariwise, direct immersion extraction minimizes the occurrence of artifacts related to coating saturation and provides enhanced extraction of polar compounds. In addition, matrix-compatible PDMS-modified solid coatings, characterized by a new morphology that avoids coating fouling, were compared to their nonmodified analogues. The obtained results indicate that PDMS-modified coatings reduce artifacts associated with coating saturation, even in headspace mode. This factor, coupled to their matrix compatibility, make the use of direct SPME very practical as a quantification approach and the best choice for metabolomics studies where wide coverage is intended. To further understand the influence on analyte uptake on a system where additional interactions occur due to matrix components, ex vivo and in vivo sampling conditions were simulated using a starch matrix model, with the aim of mimicking plant-derived materials. Our results corroborate the fact that matrix handling can affect analyte/matrix equilibria, with consequent release of high concentrations of previously bound hydrophobic compounds, potentially leading to coating saturation. Direct immersion SPME limited the occurrence of the artifacts, which confirms the suitability of SPME for in vivo applications. These findings shed light into the implementation of in vivo SPME strategies in quantitative metabolomics studies of complex plant-based systems.

Solidification Microstructure, Segregation, and Shrinkage of Fe-Mn-C Twinning-Induced Plasticity Steel by Simulation and Experiment

NASA Astrophysics Data System (ADS)

Lan, Peng; Tang, Haiyan; Zhang, Jiaquan

2016-06-01

A 3D cellular automaton finite element model with full coupling of heat, flow, and solute transfer incorporating solidification grain nucleation and growth was developed for a multicomponent system. The predicted solidification process, shrinkage porosity, macrosegregation, grain orientation, and microstructure evolution of Fe-22Mn-0.7C twinning-induced plasticity (TWIP) steel match well with the experimental observation and measurement. Based on a new solute microsegregation model using the finite difference method, the thermophysical parameters including solid fraction, thermal conductivity, density, and enthalpy were predicted and compared with the results from thermodynamics and experiment. The effects of flow and solute transfer in the liquid phase on the solidification microstructure of Fe-22Mn-0.7C TWIP steel were compared numerically. Thermal convection decreases the temperature gradient in the liquid steel, leading to the enlargement of the equiaxed zone. Solute enrichment in front of the solid/liquid interface weakens the thermal convection, resulting in a little postponement of columnar-to-equiaxed transition (CET). The CET behavior of Fe-Mn-C TWIP steel during solidification was fully described and mathematically quantized by grain morphology statistics for the first time. A new methodology to figure out the CET location by linear regression of grain mean size with least-squares arithmetic was established, by which a composition design strategy for Fe-Mn-C TWIP steel according to solidification microstructure, matrix compactness, and homogeneity was developed.

Liquid-Solid Self-Lubricated Coatings

NASA Astrophysics Data System (ADS)

Armada, S.; Schmid, R.; Equey, S.; Fagoaga, I.; Espallargas, N.

2013-02-01

Self-lubricated coatings have been a major topic of interest in thermal spray in the last decades. Self-lubricated coatings obtained by thermal spray are exclusively based on solid lubricants (PTFE, h-BN, graphite, MoS2, etc.) embedded in the matrix. Production of thermal spray coatings containing liquid lubricants has not yet been achieved because of the complexity of keeping a liquid in a solid matrix during the spraying process. In the present article, the first liquid-solid self-lubricating thermal spray coatings are presented. The coatings are produced by inserting lubricant-filled capsules inside a polymeric matrix. The goal of the coating is to release lubricant to the system when needed. The first produced coatings consisted solely of capsules for confirming the feasibility of the process. For obtaining such a coating, the liquid-filled capsules were injected in the thermal spray flame without any other feedstock material. Once the concept and the idea were proven, a polymer was co-sprayed together with the capsules to obtain a coating containing the lubricant-filled capsules distributed in the solid polymeric matrix. The coatings and the self-lubricated properties have been investigated by means of optical microscopy, Scanning Electron Microscopy, and tribological tests.

The study of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites

NASA Astrophysics Data System (ADS)

Yu, Peng

Aluminum-based metal matrix composites (MMCs) have been widely used as structural materials in the automobile and aerospace industry due to their specific properties. In this thesis, we report the fabrication of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites by the displacement reactions between Al and selected metal oxides (NiO, CuO and ZnO). These MMCs were produced when the Al-20wt% NiO, Al-20wt% CuO and Al-10wt% ZnO green compacts were reaction sintered in the tube furnaces. In this work, differential thermal analysis (DTA) was performed on the green samples. The green samples were then sintered separately in different tube furnaces for 30 minutes. In order to study the reaction mechanisms, the x-ray diffractometry (XRD) was used to obtain diffraction patterns of these sintered samples, the scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to study the microstructures of these samples. The elemental quantitative compositions of samples were determined by the energy dispersive x-ray spectrometry (EDX). In order to study the effect of cooling rate on the samples, the green samples were further sintered to 1000°C and cooled down to room temperature in different conditions: by furnace-cooling, air-quenching, oil-quenching or NaCl-solution-quenching. The SEM, TEM and atomic force microscopy (AFM) were conducted to investigate their microstructures. A microhardness tester was used to measure the hardness values of these samples. It was found that during sintering of the Al-20wt% NiO green sample, displacement reaction between Al and NiO initially occurred in solid-solid form and was soon halted by its products that separated the NiO particles from the Al matrix. The reaction then resumed in solid-liquid form as the temperature increased to the eutectic temperature of Al3Ni-Al when liquid (Al, Ni) phase appeared in the sample. After cooling, Al2O 3 particles, Al3Ni proeutectic phase and fiber-like Al 3Ni-Al eutectic were found in the sintered Al-MMC sample. (Abstract shortened by UMI.)

Acoustic and elastic multiple scattering and radiation from cylindrical structures

NASA Astrophysics Data System (ADS)

Amirkulova, Feruza Abdukadirovna

Multiple scattering (MS) and radiation of waves by a system of scatterers is of great theoretical and practical importance and is required in a wide variety of physical contexts such as the implementation of "invisibility" cloaks, the effective parameter characterization, and the fabrication of dynamically tunable structures, etc. The dissertation develops fast, rapidly convergent iterative techniques to expedite the solution of MS problems. The formulation of MS problems reduces to a system of linear algebraic equations using Graf's theorem and separation of variables. The iterative techniques are developed using Neumann expansion and Block Toeplitz structure of the linear system; they are very general, and suitable for parallel computations and a large number of MS problems, i.e. acoustic, elastic, electromagnetic, etc., and used for the first time to solve MS problems. The theory is implemented in Matlab and FORTRAN, and the theoretical predictions are compared to computations obtained by COMSOL. To formulate the MS problem, the transition matrix is obtained by analyzing an acoustic and an elastic single scattering of incident waves by elastic isotropic and anisotropic solids. The mathematical model of wave scattering from multilayered cylindrical and spherical structures is developed by means of an exact solution of dynamic 3D elasticity theory. The recursive impedance matrix algorithm is derived for radially heterogeneous anisotropic solids. An explicit method for finding the impedance in piecewise uniform, transverse-isotropic material is proposed; the solution is compared to elasticity theory solutions involving Buchwald potentials. Furthermore, active exterior cloaking devices are modeled for acoustic and elastic media using multipole sources. A cloaking device can render an object invisible to some incident waves as seen by some external observer. The active cloak is generated by a discrete set of multipole sources that destructively interfere with an incident wave to produce zero total field over a finite spatial region. The approach precisely determines the necessary source amplitudes and enables a cloaked region to be determined using Graf's theorem. To apply the approach, the infinite series of multipole expansions are truncated, and the accuracy of cloaking is studied by modifying the truncation parameter.

Superalloy for high-temperature hydrogen environmental applications

NASA Technical Reports Server (NTRS)

McKannan, Eugene C. (Inventor); McPherson, William B. (Inventor); Ahmed, Shaffiq (Inventor); Chandler, Shirley S. (Inventor)

1991-01-01

A nickel-based superalloy is provided which is resistant to deterioration in hydrogen at high operating temperatures and pressures, and which thus can be used in hydrogen-fueled spacecraft such as the Space Shuttle. The superalloy is characterized by a two-phase microstructure and consists of a gamma-prime precipitated phase in a gamma matrix. The gamma matrix phase is a primary solid solution and the gamma precipitated phase will be an intermetallic compound of the type A.sub.3 B, such as nickel aluminide or titanide. Both phases are coherent, ordered, and compatible, and thus will retain most of their strength at elevated temperatures. The alloy consists essentially of (by weight): Ni 50-60%, Cr 10-20%, Al 2-6%, Co 2-5%, Ti 3-8%, W 5-12%, Mo 5-10%, Nb 1-3%, wherein the ratio W/MO is approximately equal to 1, and Ti/Al ranges from about 1 to about 2.

Experimental Analysis and Mathematical Modeling on Mg-Li Alloy Sheets with Three Crystal Structures during Cold Rolling and Heat Treatment.

PubMed

Tang, Yan; Le, Qichi; Wang, Tong; Chen, Xingrui

2017-10-12

The microstructural evolution, mechanical properties, and mathematical relationship of an α, α + β, and β phase Mg-Li alloy during the cold rolling and annealing process were investigated. The results showed that the increased Li element gradually transformed the Mg matrix structure from hcp to bcc. Simultaneously, the alloy plasticity was improved remarkably during cold rolling. In the annealing process, a sort of abnormal grain growth was found in Mg-11Li-3Al-2Zn-0.2Y, but was not detected in Mg-5Li-3Al-2Zn-0.2Y and Mg-8Li-3Al-2Zn-0.2Y. Moreover, the mechanical properties of alloy were evidently improved through a kind of solid solution in the β matrix. To accurately quantify this strengthening effect, the method of mathematical modeling was used to determine the relationship between strength and multiple factors.

Nano-sized precipitate stability and its controlling factors in a NiAl-strengthened ferritic alloy

PubMed Central

Sun, Zhiqian; Song, Gian; Ilavsky, Jan; Ghosh, Gautam; Liaw, Peter K.

2015-01-01

Coherent B2-ordered NiAl-type precipitates have been used to reinforce solid-solution body-centered-cubic iron for high-temperature application in fossil-energy power plants. In this study, we investigate the stability of nano-sized precipitates in a NiAl-strengthened ferritic alloy at 700–950 °C using ultra-small angle X-ray scattering and electron microscopies. Here we show that the coarsening kinetics of NiAl-type precipitates is in excellent agreement with the ripening model in multicomponent alloys. We further demonstrate that the interfacial energy between the matrix and NiAl-type precipitates is strongly dependent on differences in the matrix/precipitate compositions. Our results profile the ripening process in multicomponent alloys by illustrating controlling factors of interfacial energy, diffusivities, and element partitioning. The study provides guidelines to design and develop high-temperature alloys with stable microstructures for long-term service. PMID:26537060

Processing and characterization of Al-Al3Nb prepared by mechanical alloying and equal channel angular pressing

NASA Astrophysics Data System (ADS)

Chandran, P.; Zafari, A.; Lui, E. W.; Xia, K.

2017-05-01

Mechanically alloyed Al with immiscible elements such as Nb can lead to a uniform distribution of nanoscaled precipitates which are highly stable compared to conventional alloying and with excellent interface, resulting in significant increase in strength without problems associated with nano ceramic particles in metal matrix composites. Although immiscible, Nb can be alloyed with Al through mechanical milling, forming trialuminide (Al3Nb), either directly or upon subsequent precipitation, which possesses high strength, stiffness and stability at elevated temperatures. In the present study, Al-5 at.% Nb supersaturated solid solution was achieved after prolonged ball milling and nano Al3Nb precipitates were formed during subsequent ageing at 530°C. The Al-Al3Nb powder was consolidated by equal channel angular pressing (ECAP) at 400°C, resulting in a fully dense material with a uniform distribution of nanoscaled Al3Nb precipitates in the Al matrix.

Biomimetic Mineralization on a Macroporous Cellulose-Based Matrix for Bone Regeneration

PubMed Central

Petrauskaite, Odeta; Gomes, Pedro de Sousa; Fernandes, Maria Helena; Juodzbalys, Gintaras; Maminskas, Julius

2013-01-01

The aim of this study is to investigate the biomimetic mineralization on a cellulose-based porous matrix with an improved biological profile. The cellulose matrix was precalcified using three methods: (i) cellulose samples were treated with a solution of calcium chloride and diammonium hydrogen phosphate; (ii) the carboxymethylated cellulose matrix was stored in a saturated calcium hydroxide solution; (iii) the cellulose matrix was mixed with a calcium silicate solution in order to introduce silanol groups and to combine them with calcium ions. All the methods resulted in a mineralization of the cellulose surfaces after immersion in a simulated body fluid solution. Over a period of 14 days, the matrix was completely covered with hydroxyapatite crystals. Hydroxyapatite formation depended on functional groups on the matrix surface as well as on the precalcification method. The largest hydroxyapatite crystals were obtained on the carboxymethylated cellulose matrix treated with calcium hydroxide solution. The porous cellulose matrix was not cytotoxic, allowing the adhesion and proliferation of human osteoblastic cells. Comparatively, improved cell adhesion and growth rate were achieved on the mineralized cellulose matrices. PMID:24163816

Development of a poly(dimethylacrylamide) based matrix material for solid phase high density peptide array synthesis employing a laser based material transfer

NASA Astrophysics Data System (ADS)

Ridder, Barbara; Foertsch, Tobias C.; Welle, Alexander; Mattes, Daniela S.; von Bojnicic-Kninski, Clemens M.; Loeffler, Felix F.; Nesterov-Mueller, Alexander; Meier, Michael A. R.; Breitling, Frank

2016-12-01

Poly(dimethylacrylamide) (PDMA) based matrix materials were developed for laser-based in situ solid phase peptide synthesis to produce high density arrays. In this specific array synthesis approach, amino acid derivatives are embedded into a matrix material, serving as a ;solid; solvent material at room temperature. Then, a laser pulse transfers this mixture to the target position on a synthesis slide, where the peptide array is synthesized. Upon heating above the glass transition temperature of the matrix material, it softens, allowing diffusion of the amino acid derivatives to the synthesis surface and serving as a solvent for peptide bond formation. Here, we synthesized PDMA six-arm star polymers, offering the desired matrix material properties, using atom transfer radical polymerization. With the synthesized polymers as matrix material, we structured and synthesized arrays with combinatorial laser transfer. With densities of up to 20,000 peptide spots per cm2, the resolution could be increased compared to the commercially available standard matrix material. Time-of-Flight Secondary Ion Mass Spectrometry experiments revealed the penetration behavior of an amino acid derivative into the prepared acceptor synthesis surface and the effectiveness of the washing protocols.

Low-temperature matrix effects on orientational motion of Methyl radical trapped in gas solids: Angular tunneling vs. libration

NASA Astrophysics Data System (ADS)

Dmitriev, Yurij A.; Zelenetckii, Ilia A.; Benetis, Nikolas P.

2018-05-01

EPR investigation of the lineshape of matrix -isolated methyl radical, CH3, spectra recorded in solid N2O and CO2 was carried out. Reversible temperature-dependent line width anisotropy was observed in both matrices. This effect is a fingerprint of the extra-slow radical rotation about the in-plane C2 axes. The rotation was found to be anisotropic and closely correlated to the orientational dynamics of the matrix molecules. It was suggested that a recently discovered "hoping precession" effect of matrix molecules in solid CO2 is a common feature of matrices of the linear molecules CO, N2O, and CO2. A new low-temperature matrix effect, referred to as "libration trap", was proposed which accounts for the changing CH3 reorientational motion about the radical C3-axis from rotation to libration. Temperature dependence of the intensity of the EPR satellites produced by these nonrotating-but librating methyls was presented. This allowed for a rough estimation of the rotation hindering potential due to correlation mismatch between the radical and the nearest matrix molecules' librations.

Modeling of heat flow and effective thermal conductivity of fractured media: Analytical and numerical methods

NASA Astrophysics Data System (ADS)

Nguyen, S. T.; Vu, M.-H.; Vu, M. N.; Tang, A. M.

2017-05-01

The present work aims to modeling the thermal conductivity of fractured materials using homogenization-based analytical and pattern-based numerical methods. These materials are considered as a network of cracks distributed inside a solid matrix. Heat flow through such media is perturbed by the crack system. The problem of heat flow across a single crack is firstly investigated. The classical Eshelby's solution, extended to the thermal conduction problem of an ellipsoidal inclusion embedding in an infinite homogeneous matrix, gives an analytical solution of temperature discontinuity across a non-conducting penny-shaped crack. This solution is then validated by the numerical simulation based on the finite elements method. The numerical simulation allows analyzing the effect of crack conductivity. The problem of a single crack is then extended to a medium containing multiple cracks. Analytical estimations for effective thermal conductivity, that take into account the interaction between cracks and their spatial distribution, are developed for the case of non-conducting cracks. Pattern-based numerical method is then employed for both cases non-conducting and conducting cracks. In the case of non-conducting cracks, numerical and analytical methods, both account for the spatial distribution of the cracks, fit perfectly. In the case of conducting cracks, the numerical analyzing of crack conductivity effect shows that highly conducting cracks weakly affect heat flow and the effective thermal conductivity of fractured media.

Headspace analysis of polar organic compounds in biological matrixes using solid phase microextraction (SPME)

USDA-ARS?s Scientific Manuscript database

Analysis of biological fluids and waste material is difficult and tedious given the sample matrix. A rapid automated method for the determination of volatile fatty acids and phenolic and indole compounds was developed using a multipurpose sampler (MPS) with solid phase microextraction (SPME) and GC-...

Solid-state radioluminescent compositions

DOEpatents

Clough, Roger L.; Gill, John T.; Hawkins, Daniel B.; Renschler, Clifford L.; Shepodd, Timothy J.; Smith, Henry M.

1991-01-01

A solid state radioluminescent composition for light source comprises an optically clear polymer organic matrix containing tritiated organic materials and dyes capable of "red" shifting primary scintillation emissions from the polymer matrix. The tritiated organic materials are made by reducing, with tritium, an unsaturated organic compound that prior to reduction contains olefinic or alkynylic bonds.

[Analytical figures of merit of Hildebrand grid and ultrasonic nebulizations in inductively coupled plasma atomic emission].

PubMed

Tian, Mei; Han, Xiao-yuan; Zhuo, Shang-jun; Zhang, Rui-rong

2012-05-01

Hildebrand grid nebulizer is a kind of improved Babington nebulizer, which can nebulize solutions with high total dissolved solids. And the ultrasonic nebulizer (USN) possesses advantage of high nebulization efficiency and fine droplets. In the present paper, the detection limits, matrix effects, ICP robustness and memory effects of Hildebrand grid and ultrasonic nebulizers for ICP-AES were studied. The results show that the detection limits using USN are improved by a factor of 6-23 in comparison to Hildebrand grid nebulizer for Cu, Pb, Zn, Cr, Cd and Ni. With the USN the matrix effects were heavier, and the degree of intensity enhancement and lowering depends on the element line, the composition and concentrations of matrices. Moreover, matrix effects induced by Ca and Mg are more significant than those caused by Na and Mg, and intensities of ionic lines are affected more easily than those of atomic lines. At the same time, with the USN ICP has less robustness. In addition, memory effect of the USN is also heavier than that of Hildebrand grid nebulizer.

A General-applications Direct Global Matrix Algorithm for Rapid Seismo-acoustic Wavefield Computations

NASA Technical Reports Server (NTRS)

Schmidt, H.; Tango, G. J.; Werby, M. F.

1985-01-01

A new matrix method for rapid wave propagation modeling in generalized stratified media, which has recently been applied to numerical simulations in diverse areas of underwater acoustics, solid earth seismology, and nondestructive ultrasonic scattering is explained and illustrated. A portion of recent efforts jointly undertaken at NATOSACLANT and NORDA Numerical Modeling groups in developing, implementing, and testing a new fast general-applications wave propagation algorithm, SAFARI, formulated at SACLANT is summarized. The present general-applications SAFARI program uses a Direct Global Matrix Approach to multilayer Green's function calculation. A rapid and unconditionally stable solution is readily obtained via simple Gaussian ellimination on the resulting sparsely banded block system, precisely analogous to that arising in the Finite Element Method. The resulting gains in accuracy and computational speed allow consideration of much larger multilayered air/ocean/Earth/engineering material media models, for many more source-receiver configurations than previously possible. The validity and versatility of the SAFARI-DGM method is demonstrated by reviewing three practical examples of engineering interest, drawn from ocean acoustics, engineering seismology and ultrasonic scattering.

Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

NASA Astrophysics Data System (ADS)

Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

2017-06-01

A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

Solute Migration from the Aquifer Matrix into a Solution Conduit and the Reverse.

PubMed

Li, Guangquan; Field, Malcolm S

2016-09-01

A solution conduit has a permeable wall allowing for water exchange and solute transfer between the conduit and its surrounding aquifer matrix. In this paper, we use Laplace Transform to solve a one-dimensional equation constructed using the Euler approach to describe advective transport of solute in a conduit, a production-value problem. Both nonuniform cross-section of the conduit and nonuniform seepage at the conduit wall are considered in the solution. Physical analysis using the Lagrangian approach and a lumping method is performed to verify the solution. Two-way transfer between conduit water and matrix water is also investigated by using the solution for the production-value problem as a first-order approximation. The approximate solution agrees well with the exact solution if dimensionless travel time in the conduit is an order of magnitude smaller than unity. Our analytical solution is based on the assumption that the spatial and/or temporal heterogeneity in the wall solute flux is the dominant factor in the spreading of spring-breakthrough curves, and conduit dispersion is only a secondary mechanism. Such an approach can lead to the better understanding of water exchange and solute transfer between conduits and aquifer matrix. Euler and Lagrangian approaches are used to solve transport in conduit. Two-way transfer between conduit and matrix is investigated. The solution is applicable to transport in conduit of persisting solute from matrix. © 2016, National Ground Water Association.

Tribological properties and lubrication mechanism of in situ graphene-nickel matrix composite impregnated with lubricating oil

NASA Astrophysics Data System (ADS)

Lei, Yu; Du, Jinfang; Pang, Xianjuan; Wang, Haizhong; Yang, Hua; Jiang, Jinlong

2018-05-01

A solid-liquid synergetic lubricating system has been designed to develop a novel self-lubricating nickel matrix composite. The graphene-nickel (G-Ni) matrix composite with porous structure was fabricated by in situ growing graphene in bulk nickel using a powder metallurgy method. The porous structures of the composite were used to store polyalphaolefin (PAO) oil for self-lubricating. It is found that the G-Ni matrix composite under oil lubrication condition exhibited superior tribological properties as compared to pure nickel and the composite under dry sliding condition. The prestored oil was released from pores to the sliding surface forming a lubricating oil film during friction process. This lubricating oil film can protect the worn surface from severe oxidation, and help the formation and transfer of a carbon-based solid tribofilm derived from graphene and lubricating oil. This solid (graphene)-liquid (oil) synergistic lubricating mechanism is responsible for the reduction of friction coefficient and improvement of wear resistance of the in situ fabricated G-Ni matrix composite.

The matrix exponential in transient structural analysis

NASA Technical Reports Server (NTRS)

Minnetyan, Levon

1987-01-01

The primary usefulness of the presented theory is in the ability to represent the effects of high frequency linear response with accuracy, without requiring very small time steps in the analysis of dynamic response. The matrix exponential contains a series approximation to the dynamic model. However, unlike the usual analysis procedure which truncates the high frequency response, the approximation in the exponential matrix solution is in the time domain. By truncating the series solution to the matrix exponential short, the solution is made inaccurate after a certain time. Yet, up to that time the solution is extremely accurate, including all high frequency effects. By taking finite time increments, the exponential matrix solution can compute the response very accurately. Use of the exponential matrix in structural dynamics is demonstrated by simulating the free vibration response of multi degree of freedom models of cantilever beams.

Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy as an Analytical Method to Investigate the Secondary Structure of a Model Protein Embedded in Solid Lipid Matrices.

PubMed

Zeeshan, Farrukh; Tabbassum, Misbah; Jorgensen, Lene; Medlicott, Natalie J

2018-02-01

Protein drugs may encounter conformational perturbations during the formulation processing of lipid-based solid dosage forms. In aqueous protein solutions, attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy can investigate these conformational changes following the subtraction of spectral interference of solvent with protein amide I bands. However, in solid dosage forms, the possible spectral contribution of lipid carriers to protein amide I band may be an obstacle to determine conformational alterations. The objective of this study was to develop an ATR FT-IR spectroscopic method for the analysis of protein secondary structure embedded in solid lipid matrices. Bovine serum albumin (BSA) was chosen as a model protein, while Precirol AT05 (glycerol palmitostearate, melting point 58 ℃) was employed as the model lipid matrix. Bovine serum albumin was incorporated into lipid using physical mixing, melting and mixing, or wet granulation mixing methods. Attenuated total reflection FT-IR spectroscopy and size exclusion chromatography (SEC) were performed for the analysis of BSA secondary structure and its dissolution in aqueous media, respectively. The results showed significant interference of Precirol ATO5 with BSA amide I band which was subtracted up to 90% w/w lipid content to analyze BSA secondary structure. In addition, ATR FT-IR spectroscopy also detected thermally denatured BSA solid alone and in the presence of lipid matrix indicating its suitability for the detection of denatured protein solids in lipid matrices. Despite being in the solid state, conformational changes occurred to BSA upon incorporation into solid lipid matrices. However, the extent of these conformational alterations was found to be dependent on the mixing method employed as indicated by area overlap calculations. For instance, the melting and mixing method imparted negligible effect on BSA secondary structure, whereas the wet granulation mixing method promoted more changes. Size exclusion chromatography analysis depicted the complete dissolution of BSA in the aqueous media employed in the wet granulation method. In conclusion, an ATR FT-IR spectroscopic method was successfully developed to investigate BSA secondary structure in solid lipid matrices following the subtraction of lipid spectral interference. The ATR FT-IR spectroscopy could further be applied to investigate the secondary structure perturbations of therapeutic proteins during their formulation development.

Study on the Preparation Process and Influential Factors of Large Area Environment-friendly Molten Carbonate Fuel Cell Matrix

NASA Astrophysics Data System (ADS)

Zhang, Ruiyun; Xu, Shisen; Cheng, Jian; Wang, Hongjian; Ren, Yongqiang

2017-07-01

Low-cost and high-performance matrix materials used in mass production of molten carbonate fuel cell (MCFC) were prepared by automatic casting machine with α-LiAlO2 powder material synthesized by gel-solid method, and distilled water as solvent. The single cell was assembled for generating test, and the good performance of the matrix was verified. The paper analyzed the factors affecting aqueous tape casting matrix preparation, such as solvent content, dispersant content, milling time, blade height and casting machine running speed, providing a solid basis for the mass production of large area environment-friendly matrix used in molten carbonate fuel cell.

Chemical disorder and 207Pb hyperfine fields in the magnetoelectric multiferroic Pb (F e1 /2S b1 /2 ) O3 and its solid solution with Pb (F e1 /2N b1 /2) O3

NASA Astrophysics Data System (ADS)

Zagorodniy, Yu. O.; Kuzian, R. O.; Kondakova, I. V.; Maryško, M.; Chlan, V.; Štěpánková, H.; Olekhnovich, N. M.; Pushkarev, A. V.; Radyush, Yu. V.; Raevski, I. P.; Zalar, B.; Laguta, V. V.; Stephanovich, V. A.

2018-01-01

We report on the results of magnetic susceptibility, electron paramagnetic resonance, and 207Pb nuclear magnetic resonance (NMR) studies of the magnetoelectric multiferroic Pb (F e1 /2S b1 /2 ) O3 (PFS) ceramic, as well as its solid solution with Pb (F e1 /2N b1 /2) O3 (PFN) of different degrees of the 1:1 ordering of magnetic F e3 + and nonmagnetic S b5 + ions. The ordering has been studied by x-ray diffraction (XRD) and NMR methods. In particular, two spectral lines, originating from the ordered and disordered regions, respectively, are resolved in the 207Pb NMR spectra. This demonstrates the presence of spatially heterogeneous ordering where ordered regions are embedded into a disordered matrix. Combining XRD and NMR data, we have determined both the long-range order parameter s and the volume fraction of ordered regions s' for all investigated samples. The values vary in the range s =0 -0.93 and s'=0 -1 . We have found that the 207Pb Fermi contact interaction strongly depends on the disorder in the Fe/Sb positions: whereas it reaches 7.08 MHz in the ordered lattice, it is almost zero in the disordered environment. These results are further supported by the studies of PFS-PFN solid solutions. The analysis of experimental data in terms of density functional theory reveals a noticeably higher hybridization between Pb 6s and Fe 3d orbitals in the ordered case. The ordering of magnetic and nonmagnetic ions has a strong impact on the magnetic properties of PFS, leading to a transformation of the long-range ordered antiferromagnetic phase in chemically ordered samples to the spin glass state already in partially (s =0.35 ) disordered specimens. In our opinion, the difference in the magnetic properties of PFN and PFS is related to the fact that PFN is completely disordered, in contrast to PFS, which is only partially disordered, with small ordered regions existing in the disordered matrix that prevent the percolation of the nearest-neighbor Fe-Fe exchange interaction across the lattice.

Solid-state, ambient-operation thermally activated delayed fluorescence from flexible, non-toxic gold-nanocluster thin films: towards the development of biocompatible light-emitting devices

NASA Astrophysics Data System (ADS)

Talite, M. J. A.; Lin, H. T.; Jiang, Z. C.; Lin, T. N.; Huang, H. Y.; Heredia, E.; Flores, A.; Chao, Y. C.; Shen, J. L.; Lin, C. A. J.; Yuan, C. T.

2016-08-01

Luminescent gold nanoclusters (AuNCs) with good biocompatibility have gained much attention in bio-photonics. In addition, they also exhibit a unique photo-physical property, namely thermally activated delayed fluorescence (TADF), by which both singlet and triplet excitons can be harvested. The combination of their non-toxic material property and unique TADF behavior makes AuNCs biocompatible nano-emitters for bio-related light-emitting devices. Unfortunately, the TADF emission is quenched when colloidal AuNCs are transferred to solid states under ambient environment. Here, a facile, low-cost and effective method was used to generate efficient and stable TADF emissions from solid AuNCs under ambient environment using polyvinyl alcohol as a solid matrix. To unravel the underlying mechanism, temperature-dependent static and transient photoluminescence measurements were performed and we found that two factors are crucial for solid TADF emission: small energy splitting between singlet and triplet states and the stabilization of the triplet states. Solid TADF films were also deposited on the flexible plastic substrate with patterned structures, thus mitigating the waveguide-mode losses. In addition, we also demonstrated that warm white light can be generated based on a co-doped single emissive layer, consisting of non-toxic, solution-processed TADF AuNCs and fluorescent carbon dots under UV excitation.

Elastic moduli and thermal expansion coefficients of medium-entropy subsystems of the CrMnFeCoNi high-entropy alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Laplanche, Guillaume; Gadaud, P.; Barsch, C.

Elastic moduli of a set of equiatomic alloys (CrFeCoNi, CrCoNi, CrFeNi, FeCoNi, MnCoNi, MnFeNi, and CoNi), which are medium-entropy subsystems of the CrMnFeCoNi high-entropy alloy were determined as a function of temperature over the range 293 K–1000 K. Thermal expansion coefficients were determined for these alloys over the temperature range 100 K–673 K. All alloys were single-phase and had the face-centered cubic (FCC) crystal structure, except CrFeNi which is a two-phase alloy containing a small amount of body-centered cubic (BCC) precipitates in a FCC matrix. The temperature dependences of thermal expansion coefficients and elastic moduli obtained here are useful for quantifying fundamental aspects suchmore » as solid solution strengthening, and for structural analysis/design. Furthermore, using the above results, the yield strengths reported in literature for these alloys were normalized by their shear moduli to reveal the influence of shear modulus on solid solution strengthening.« less

Development and characterization of laser surface cladding (Ti,W)C reinforced Ni-30Cu alloy composite coating on copper

NASA Astrophysics Data System (ADS)

Yan, Hua; Zhang, Peilei; Yu, Zhishui; Li, Chonggui; Li, Ruidi

2012-07-01

To improve the wear resistance of copper components, laser surface cladding (LSC) was applied to deposit (Ti,W)C reinforced Ni-30Cu alloy composite coating on copper using a cladding interlayer of Ni-30Cu alloy by Nd:YAG laser. The microstructure and phases of the composite coating were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray energy dispersive microanalysis (EDX). Microhardness tester and pin-on-disc wear tester were employed to evaluate the hardness and dry-sliding wear resistance. The results show that crack-free composite coating with metallurgical bonding to the copper substrate is obtained. Phases identified in the (Ti,W)C-reinforced Ni-30Cu alloy composite layer are composed of TiWC2 reinforcements and (Ni,Cu) solid solution. TiWC2 reinforcements are distributed uniformly in the (Ni,Cu) solid solution matrix with dendritic morphology in the upper region and with particles in the mid-lower region. The microhardness and wear properties of the composite coating are improved significantly in comparison to the as-received copper substrate due to the addition of 50 wt% (Ti,W)C multicarbides.

Synthesis and characterisation of the hollandite solid solution Ba1.2-xCsxFe2.4-xTi5.6+xO16 for partitioning and conditioning of radiocaesium

NASA Astrophysics Data System (ADS)

Bailey, Daniel J.; Stennett, Martin C.; Mason, Amber R.; Hyatt, Neil C.

2018-05-01

The geological disposal of high level radioactive waste requires careful budgeting of the heat load produced by radiogenic decay. Removal of high-heat generating radionuclides, such as 137Cs, reduces the heat load in the repository allowing the remaining high level waste to be packed closer together therefore reducing demand for repository space and the cost of the disposal of the remaining wastes. Hollandites have been proposed as a possible host matrix for the long-term disposal of Cs separated from HLW raffinate. The incorporation of Cs into the hollandite phase is aided by substitution of cations on the B-site of the hollandite structure, including iron. A range of Cs containing iron hollandites were synthesised via an alkoxide-nitrate route and the structural environment of Fe in the resultant material characterised by Mössbauer and X-ray Absorption Near Edge Spectroscopy. The results of spectroscopic analysis found that Fe was present as octahedrally co-ordinated Fe (III) in all cases and acts as an effective charge compensator over a wide solid solution range.

Electrosprayed core–shell solid dispersions of acyclovir fabricated using an epoxy-coated concentric spray head

PubMed Central

Liu, Zhe-Peng; Cui, Lei; Yu, Deng-Guang; Zhao, Zhuan-Xia; Chen, Lan

2014-01-01

A novel structural solid dispersion (SD) taking the form of core–shell microparticles for poorly water-soluble drugs is reported for the first time. Using polyvinylpyrrolidone (PVP) as a hydrophilic polymer matrix, the SDs were fabricated using coaxial electrospraying (characterized by an epoxy-coated concentric spray head), although the core fluids were unprocessable using one-fluid electrospraying. Through manipulating the flow rates of the core drug-loaded solutions, two types of core–shell microparticles with tunable drug contents were prepared. They had average diameters of 1.36±0.67 and 1.74±0.58 μm, and were essentially a combination of nanocomposites with the active ingredient acyclovir (ACY) distributed in the inner core, and the sweeter sucralose and transmembrane enhancer sodium dodecyl sulfate localized in the outer shell. Differential scanning calorimetry and X-ray diffraction results demonstrated that ACY, sodium dodecyl sulfate, and sucralose were well distributed in the PVP matrix in an amorphous state because of favorable second-order interactions. In vitro dissolution and permeation studies showed that the core–shell microparticle SDs rapidly freed ACY within 1 minute and promoted nearly eightfold increases in permeation rate across the sublingual mucosa compared with raw ACY powders. PMID:24790437

Formation and Stability of Pb-Sn Embedded Multiphase Alloy Nanoparticles via Mechanical Alloying

NASA Astrophysics Data System (ADS)

Khan, Patan Yousaf; Devi, M. Manolata; Biswas, Krishanu

2015-08-01

The present paper describes the preparation, characterization, and stability of Pb-Sn multiphase alloy nanoparticles embedded in Al matrix via mechanical alloying (MA). MA is a solid-state processing route, which can produce nanocrystalline phases by severely deforming the materials at high strain rate. Therefore, in order to understand the effect of the increasing interface as well as defects on the phase transformation behavior of Pb-Sn nanoparticles, Pb-Sn multiphase nanoparticles have been embedded in Al by MA. The nanoparticles have extensively been characterized using X-ray diffraction and transmission electron microscope. The characterization reveals the formation of biphasic as well as single-phase solid solution nanoparticles embedded in the matrix. The detailed microstructural and differential scanning calorimetry studies indicate that the formation of biphasic nanoparticles is due to size effect, mechanical attrition, and ballistic diffusion of Pb and Sn nanoparticles embedded in Al grains. Thermal characterization data reveal that the heating event consists of the melting peaks due to the multiphase nanoparticles and the peak positions shift to lower temperature with the increase in milling time. The role of interface structure is believed to play a prominent role in determining the phase stability of the nanoparticle. The results are discussed in the light of the existing literature.

Enhanced electrical conductivity of poly(methyl methacrylate) filled with graphene and in situ synthesized gold nanoparticles

NASA Astrophysics Data System (ADS)

Feng, Jie; Athanassiou, Athanassia; Bonaccorso, Francesco; Fragouli, Despina

2018-06-01

The improvement of the electrical conductivity of polymers by incorporating graphene has been intensively studied in recent years. To further boost the electrical conductivity, blending third-party additives into the polymer/graphene systems has been demonstrated as a viable strategy. Herein, we propose a simple route to increase the electrical conductivity of poly(methyl methacrylate) (PMMA)/graphene nanoplatelet (GnP) composites, by the in situ synthesis of gold nanoparticles directly into the solid film. In particular, PMMA, GnPs and a gold precursor are solution blended to form the composite films. The subsequent heat-induced formation of gold nanoparticles directly in the solid state film, cause the significant decrease of the percolation threshold of GnPs loading, from 3% to 1% by weight in the composite. This is attributed to the preferential formation of the gold nanoparticles onto the GnPs, with synergistic effects beneficial for the improvement of the electrical conductivity. The formation procedure of the gold nanoparticles, and their arrangement into the composite matrix are studied. We demonstrate that following this straightforward process it is possible to form nanocomposites able to conduct efficiently electric current even at low graphene loadings preserving at the same time the mechanical properties of the polymer matrix.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Arya, Anil; Sharma, Sweety; Sharma, A. L., E-mail: alsharmaiitkgp@gmail.com

Blend polymer electrolytes are prepared for salt concentration (Ö/Li = 4) with the constant ratio (0.5 gm) of PEO and PAN using solution casting technique. The prepared free standing solid polymeric film is characterized by Field Emission Scanning Electron Microscopy (FESEM) which confirms the homogeneous distribution of dissociated salt in blend polymer matrix. After addition of salt the ionic conductivity value is found to be of the order of 7.13 × 10{sup −5} Scm{sup −1} which is three orders higher when compared with pure blend polymer films. The microscopic interaction among the polymer-ion, ion-ion has been confirmed by the Fouriermore » Transform Infrared (FTIR) Spectroscopy. A very fine correlation has been built in the electrical conductivity and FTIR result. On the basis of above finding, a prepared free standing solid polymeric film appears to be appropriate for the energy storage/conversion device applications.« less

Unsupervised Calculation of Free Energy Barriers in Large Crystalline Systems

NASA Astrophysics Data System (ADS)

Swinburne, Thomas D.; Marinica, Mihai-Cosmin

2018-03-01

The calculation of free energy differences for thermally activated mechanisms in the solid state are routinely hindered by the inability to define a set of collective variable functions that accurately describe the mechanism under study. Even when possible, the requirement of descriptors for each mechanism under study prevents implementation of free energy calculations in the growing range of automated material simulation schemes. We provide a solution, deriving a path-based, exact expression for free energy differences in the solid state which does not require a converged reaction pathway, collective variable functions, Gram matrix evaluations, or probability flux-based estimators. The generality and efficiency of our method is demonstrated on a complex transformation of C 15 interstitial defects in iron and double kink nucleation on a screw dislocation in tungsten, the latter system consisting of more than 120 000 atoms. Both cases exhibit significant anharmonicity under experimentally relevant temperatures.

Using a fast Fourier method to model sound propagation in a stratified atmosphere over a stratified porous-elastic ground

NASA Technical Reports Server (NTRS)

Tooms, S.; Attenborough, K.

1990-01-01

Using a Fast Fourier integration method and a global matrix method for solution of the boundary condition equations at all interfaces simultaneously, a useful tool for predicting acoustic propagation in a stratified fluid over a stratified porous-elastic solid was developed. The model for the solid is a modified Biot-Stoll model incorporating four parameters describing the pore structure corresponding to the Rayleigh-Attenborough rigid-porous structure model. The method is also compared to another Fast Fourier code (CERL-FFP) which models the ground as an impedance surface under a horizontally stratified air. Agreement with the CERL FFP is good. The effects on sound propagation of a combination of ground elasticity, complex ground structure, and atmospheric conditions are demonstrated by theoretical results over a snow layer, and experimental results over a model ground surface.

Ultrasound-assisted analyte extraction for the determination of sulfate and elemental sulfur in zinc sulfide by different liquid chromatography techniques.

PubMed

Dash, K; Thangavel, S; Krishnamurthy, N V; Rao, S V; Karunasagar, D; Arunachalam, J

2005-04-01

The speciation and determination of sulfate (SO4(2-)) and elemental sulfur (S degree) in zinc sulfide (ZnS) using ion-chromatography (IC) and reversed-phase liquid chromatography (RPLC) respectively is described. Three sample pretreatment approaches were employed with the aim of determining sulfate: (i) conventional water extraction of the analyte; (ii) solid-liquid aqueous extraction with an ultrasonic probe; and (iii) elimination of the zinc sulfide matrix via ion-exchange dissolution (IED). The separation of sulfate was carried out by an anion-exchange column (IonPac AS17), followed by suppressed conductivity detection. Elemental sulfur was extracted ultrasonically from the acid treated sample solution into chloroform and separated on a reversed phase HPLC column equipped with a diode array detector (DAD) at 264 nm. The achievable solid detection limits for sulfate and sulfur were 35 and 10 microg g(-1) respectively.

Extraction of domoic acid from seawater and urine using a resin based on 2-(trifluoromethyl)acrylic acid.

PubMed

Piletska, Elena V; Villoslada, Fernando Navarro; Chianella, Iva; Bossi, Alessandra; Karim, Kal; Whitcombe, Michael J; Piletsky, Sergey A; Doucette, Gregory J; Ramsdell, John S

2008-03-03

A new solid-phase extraction (SPE) matrix with high affinity for the neurotoxin domoic acid (DA) was designed and tested. A computational modelling study led to the selection of 2-(trifluoromethyl)acrylic acid (TFMAA) as a functional monomer capable of imparting affinity towards domoic acid. Polymeric adsorbents containing TFMAA were synthesised and tested in high ionic strength solutions such as urine and seawater. The TFMAA-based polymers demonstrated excellent performance in solid-phase extraction of domoic acid, retaining the toxin while salts and other interfering compounds such as aspartic and glutamic acids were removed by washing and selective elution. It was shown that the TFMAA-based polymer provided the level of purification of domoic acid from urine and seawater acceptable for its quantification by high performance liquid chromatography-mass spectrometry (HPLC-MS) and enzyme-linked immunosorbent assay (ELISA) without any additional pre-concentration and purification steps.

Solid-state surface luminescence of polycyclic aromatic hydrocarbons adsorbed on cellulose diacetate matrices

NASA Astrophysics Data System (ADS)

Rogacheva, Svetlana M.; Shipovskaya, Anna B.; Volkova, Elena V.; Khurshudyan, Grachia N.; Suska-Malawska, Malgorzata; Gubina, Tamara I.

2018-04-01

The spectral-kinetic characteristics of luminescence of 17 polycyclic aromatic hydrocarbons (PAH) sorbed from a "water-organic solvent" medium on cellulose diacetate (CDA) matrices were studied. A significant increase in the fluorescence signal on the CDA matrix was observed for 13 PAHs in comparison with aqueous solutions. The highest detection sensitivity was found for pyrene, benzo(a)pyrene, and benzo(k)fluoranthene. The fluorescence spectra of two PAH indicator pairs (anthracene-phenanthrene and pyrene-fluoranthene) used to control toxicant emission sources were studied with the simultaneous presence of isomers in the analyte, depending on the excitation wavelength. For both isomer pairs, it has been found that the spectra of their solid-state luminescence overlap insignificantly, the characteristic peaks do not coincide and do not overlap, the sensitivities of detection are close to each other, which makes it possible to consider this technique as promising to control PAH contamination sources.

Reciprocated suppression of polymer crystallization toward improved solid polymer electrolytes: Higher ion conductivity and tunable mechanical properties

DOE PAGES

Bi, Sheng; Sun, Che-Nan; Zawodzinski, Thomas A.; ...

2015-08-06

Solid polymer electrolytes based on lithium bis(trifluoromethanesulfonyl) imide and polymer matrix were extensively studied in the past due to their excellent potential in a broad range of energy related applications. Poly(vinylidene fluoride) (PVDF) and polyethylene oxide (PEO) are among the most examined polymer candidates as solid polymer electrolyte matrix. In this paper, we study the effect of reciprocated suppression of polymer crystallization in PVDF/PEO binary matrix on ion transport and mechanical properties of the resultant solid polymer electrolytes. With electron and X-ray diffractions as well as energy filtered transmission electron microscopy, we identify and examine the appropriate blending composition thatmore » is responsible for the diminishment of both PVDF and PEO crystallites. Laslty, a three-fold conductivity enhancement is achieved along with a highly tunable elastic modulus ranging from 20 to 200 MPa, which is expected to contribute toward future designs of solid polymer electrolytes with high room-temperature ion conductivities and mechanical flexibility.« less

Designing Metallic and Insulating Nanocrystal Heterostructures to Fabricate Highly Sensitive and Solution Processed Strain Gauges for Wearable Sensors.

PubMed

Lee, Woo Seok; Lee, Seung-Wook; Joh, Hyungmok; Seong, Mingi; Kim, Haneun; Kang, Min Su; Cho, Ki-Hyun; Sung, Yun-Mo; Oh, Soong Ju

2017-12-01

All-solution processed, high-performance wearable strain sensors are demonstrated using heterostructure nanocrystal (NC) solids. By incorporating insulating artificial atoms of CdSe quantum dot NCs into metallic artificial atoms of Au NC thin film matrix, metal-insulator heterostructures are designed. This hybrid structure results in a shift close to the percolation threshold, modifying the charge transport mechanism and enhancing sensitivity in accordance with the site percolation theory. The number of electrical pathways is also manipulated by creating nanocracks to further increase its sensitivity, inspired from the bond percolation theory. The combination of the two strategies achieves gauge factor up to 5045, the highest sensitivity recorded among NC-based strain gauges. These strain sensors show high reliability, durability, frequency stability, and negligible hysteresis. The fundamental charge transport behavior of these NC solids is investigated and the combined site and bond percolation theory is developed to illuminate the origin of their enhanced sensitivity. Finally, all NC-based and solution-processed strain gauge sensor arrays are fabricated, which effectively measure the motion of each finger joint, the pulse of heart rate, and the movement of vocal cords of human. This work provides a pathway for designing low-cost and high-performance electronic skin or wearable devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improving the dissolution rate of poorly water soluble drug by solid dispersion and solid solution: pros and cons.

PubMed

Chokshi, Rina J; Zia, Hossein; Sandhu, Harpreet K; Shah, Navnit H; Malick, Waseem A

2007-01-01

The solid dispersions with poloxamer 188 (P188) and solid solutions with polyvinylpyrrolidone K30 (PVPK30) were evaluated and compared in an effort to improve aqueous solubility and bioavailability of a model hydrophobic drug. All preparations were characterized by differential scanning calorimetry, powder X-ray diffraction, intrinsic dissolution rates, and contact angle measurements. Accelerated stability studies also were conducted to determine the effects of aging on the stability of various formulations. The selected solid dispersion and solid solution formulations were further evaluated in beagle dogs for in vivo testing. Solid dispersions were characterized to show that the drug retains its crystallinity and forms a two-phase system. Solid solutions were characterized to be an amorphous monophasic system with transition of crystalline drug to amorphous state. The evaluation of the intrinsic dissolution rates of various preparations indicated that the solid solutions have higher initial dissolution rates compared with solid dispersions. However, after storage at accelerated conditions, the dissolution rates of solid solutions were lower due to partial reversion to crystalline form. The drug in solid dispersion showed better bioavailability in comparison to solid solution. Therefore, considering physical stability and in vivo study results, the solid dispersion was the most suitable choice to improve dissolution rates and hence the bioavailability of the poorly water soluble drug.

The Effect of Milling Time on the Microstructural Characteristics and Strengthening Mechanisms of NiMo-SiC Alloys Prepared via Powder Metallurgy.

PubMed

Yang, Chao; Muránsky, Ondrej; Zhu, Hanliang; Thorogood, Gordon J; Avdeev, Maxim; Huang, Hefei; Zhou, Xingtai

2017-04-06

A new generation of alloys, which rely on a combination of various strengthening mechanisms, has been developed for application in molten salt nuclear reactors. In the current study, a battery of dispersion and precipitation-strengthened (DPS) NiMo-based alloys containing varying amounts of SiC (0.5-2.5 wt %) were prepared from Ni-Mo-SiC powder mixture via a mechanical alloying (MA) route followed by spark plasma sintering (SPS) and rapid cooling. Neutron Powder Diffraction (NPD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the characterization of the microstructural properties of these in-house prepared NiMo-SiC DPS alloys. The study showed that uniformly-dispersed SiC particles provide dispersion strengthening, the precipitation of nano-scale Ni₃Si particles provides precipitation strengthening, and the solid-solution of Mo in the Ni matrix provides solid-solution strengthening. It was further shown that the milling time has significant effects on the microstructural characteristics of these alloys. Increased milling time seems to limit the grain growth of the NiMo matrix by producing well-dispersed Mo₂C particles during sintering. The amount of grain boundaries greatly increases the Hall-Petch strengthening, resulting in significantly higher strength in the case of 48-h-milled NiMo-SiC DPS alloys compared with the 8-h-milled alloys. However, it was also shown that the total elongation is considerably reduced in the 48-h-milled NiMo-SiC DPS alloy due to high porosity. The porosity is a result of cold welding of the powder mixture during the extended milling process.

The Effect of Milling Time on the Microstructural Characteristics and Strengthening Mechanisms of NiMo-SiC Alloys Prepared via Powder Metallurgy

PubMed Central

Yang, Chao; Muránsky, Ondrej; Zhu, Hanliang; Thorogood, Gordon J.; Avdeev, Maxim; Huang, Hefei; Zhou, Xingtai

2017-01-01

A new generation of alloys, which rely on a combination of various strengthening mechanisms, has been developed for application in molten salt nuclear reactors. In the current study, a battery of dispersion and precipitation-strengthened (DPS) NiMo-based alloys containing varying amounts of SiC (0.5–2.5 wt %) were prepared from Ni-Mo-SiC powder mixture via a mechanical alloying (MA) route followed by spark plasma sintering (SPS) and rapid cooling. Neutron Powder Diffraction (NPD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the characterization of the microstructural properties of these in-house prepared NiMo-SiC DPS alloys. The study showed that uniformly-dispersed SiC particles provide dispersion strengthening, the precipitation of nano-scale Ni3Si particles provides precipitation strengthening, and the solid-solution of Mo in the Ni matrix provides solid-solution strengthening. It was further shown that the milling time has significant effects on the microstructural characteristics of these alloys. Increased milling time seems to limit the grain growth of the NiMo matrix by producing well-dispersed Mo2C particles during sintering. The amount of grain boundaries greatly increases the Hall–Petch strengthening, resulting in significantly higher strength in the case of 48-h-milled NiMo-SiC DPS alloys compared with the 8-h-milled alloys. However, it was also shown that the total elongation is considerably reduced in the 48-h-milled NiMo-SiC DPS alloy due to high porosity. The porosity is a result of cold welding of the powder mixture during the extended milling process. PMID:28772747

Optimisation of dynamic nuclear polarisation of [1-13C] pyruvate by addition of gadolinium-based contrast agents

NASA Astrophysics Data System (ADS)

Friesen-Waldner, Lanette; Chen, Albert; Mander, Will; Scholl, Timothy J.; McKenzie, Charles A.

2012-10-01

Dynamic nuclear polarisation (DNP) of carbon-13 (13C) enriched endogenous compounds provides a novel means for magnetic resonance imaging and spectroscopy of biological processes. Adding small amounts of gadolinium-based contrast agents (GBCAs) to the 13C-enriched substrate matrix increases the amount of hyperpolarisation that can be achieved, but also may decrease the longitudinal relaxation time (T1) of the 13C nucleus in solution. This study examined the effects of five different GBCA at concentrations of 0.5, 1, 2, and 3 mM on [1-13C]-enriched pyruvic acid. It was found that contrast agents with an open chain structure (Gadobenate dimeglumine, Gadopentetate dimeglumine, Gadodiamide) caused the largest enhancement (up to 82%) in solid state polarisation relative to solutions without GBCA. In the liquid state, T1 of pyruvate decreased by as much as 62% and polarisation was much lower (70%) relative to solutions without GBCA added. Conversely, for GBCA with macrocyclic structures (Gadoterate meglumine, Gadoteridol), the solid state polarisation enhancement was only slightly less than the open chain GBCA, but enhanced polarisation was retained much better in the liquid state with minimal decrease in T1 (25% at the highest GBCA concentrations). Near maximum polarisation in the solid state was obtained at a GBCA concentration of 2 mM, with a higher concentration of 3 mM producing minimal improvement. These results indicate that the macrocyclic contrast agents provide the best combination of high solid state and liquid state polarisations with minimal loss of T1 in experiments with hyperpolarised 13C-enriched pyruvate. This suggests that macrocyclic contrast agents should be the GBCA of choice for maximising signal in experiments with hyperpolarised 13C-enriched pyruvate, particularly for in vivo measurements where shortened substrate T1 is especially problematic.

SEPARATION AND CHARACTERIZATION OF TETROL METABOLITES OF BENZO[A]PYRENE-DNA ADDUCTS USING HPLC AND SOLID-MATRIX ROOM TEMPERATURE LUMINESCENCE. (R824100)

EPA Science Inventory

Abstract

Four tetrols of benzo[a]pyrene-DNA adducts were separated using reversed-phase high performance liquid chromatography. Chromatographic fractions containing a given tetrol were readily characterized with solid-matrix room temperature luminescence techniques. So...

Rheological Behavior and Microstructure of Ceramic Particulate/Aluminum Alloy Composites. Ph.D. Thesis Final Technical Report

NASA Technical Reports Server (NTRS)

Moon, Hee-Kyung

1990-01-01

The rheological behavior and microstructure were investigated using a concentric cylinder viscometer for three different slurries: semi-solid alloy slurries of a matrix alloy, Al-6.5wt percent Si: composite slurries, SiC (sub p) (8.5 microns)/Al-6.5wt percent Si, with the same matrix alloy in the molten state, and composite slurries of the same composition with the matrix alloy in the semi-solid state. The pseudoplasticity of these slurries was obtained by step changes of the shear rate from a given initial shear rate. To study the thixotropic behavior of the system, a slurry was allowed to rest for different periods of time, prior to shearing at a given initial shear rate. In the continuous cooling experiments, the viscosities of these slurries were dependent on the shear rate, cooling rate, volume fraction of the primary solid of the matrix alloy, and volume fraction of silicon carbide. In the isothermal experiments, all three kinds of slurries exhibited non-Newtonian behavior, depending on the volume fraction of solid particles.

Top-down synthesized TiO2 nanowires as a solid matrix for surface-assisted laser desorption/ionization time-of-flight (SALDI-TOF) mass spectrometry.

PubMed

Kim, Jo-Il; Park, Jong-Min; Hwang, Seung-Ju; Kang, Min-Jung; Pyun, Jae-Chul

2014-07-11

Top-down synthesized TiO2 nanowires are presented as an ideal solid matrix to analyze small biomolecules at a m/z of less than 500. The TiO2 nanowires were synthesized as arrays using a modified hydrothermal process directly on the surface of a Ti plate. Finally, the feasibility of the TiO2 nanowires in the anatase phase as a solid matrix. The crystal and electronic structures of the top-down TiO2 nanowires were analyzed at each step of the hydrothermal process, and the optimal TiO2 nanowires were identified by checking their performance toward the ionization of analytes in surface-assisted laser desorption/ionization time-of-flight (SALDI-TOF) mass spectrometry. Finally, the feasibility of the TiO2 nanowires in the anatase phase as a solid matrix for SALDI-TOF mass spectrometry was demonstrated using eight types of amino acids and peptides as model analytes. Copyright © 2014 Elsevier B.V. All rights reserved.

Solid electrolytes

DOEpatents

Abraham, Kuzhikalail M.; Alamgir, Mohamed

1993-06-15

This invention pertains to Li ion (Li.sup.+) conductive solid polymer electrolytes composed of solvates of Li salts immobilized (encapsulated) in a solid organic polymer matrix. In particular, this invention relates to solid polymer electrolytes derived by immobilizing complexes (solvates) formed between a Li salt such as LiAsF.sub.6, LiCF.sub.3 SO.sub.3 or LiClO.sub.4 and a mixture of aprotic organic solvents having high dielectric constants such as ethylene carbonate (EC) (dielectric constant=89.6) and propylene carbonate (PC) (dielectric constant=64.4) in a polymer matrix such as polyacrylonitrile, poly(tetraethylene glycol diacrylate), or poly(vinyl pyrrolidinone).

Determination of phenolic acids and flavonoids in raw propolis by silica-supported ionic liquid-based matrix solid phase dispersion extraction high performance liquid chromatography-diode array detection.

PubMed

Wang, Zhibing; Sun, Rui; Wang, Yuanpeng; Li, Na; Lei, Lei; Yang, Xiao; Yu, Aimin; Qiu, Fangping; Zhang, Hanqi

2014-10-15

The silica-supported ionic liquid (S-SIL) was prepared by impregnation and used as the dispersion adsorbent of matrix solid phase dispersion (MSPD) for the simultaneous extraction of eight phenolic acids and flavonoids, including caffeic acid, ferulic acid, morin, luteolin, quercetin, apigenin, chrysin, and kaempferide in raw propolis. High performance liquid chromatography with a Zorbax SB-C18 column (150mm×4.6mm, 3.5μm) was used for separation of the analytes. The mobile phase consisted of 0.2% phosphoric acid aqueous solution and acetonitrile and the flow rate of the mobile phase was 0.5mL/min. The experimental conditions for silica-supported ionic liquid-based matrix solid phase dispersion (S-SIL-based MSPD) were optimized. S-SIL containing 10% [C6MIM]Cl was used as dispersant, 20mL of n-hexane as washing solvent and 15mL of methanol as elution solvent. The ratio of S-SIL to sample was selected to be 4:1. The standard curves showed good linear relationship (r>0.9995). The limits of detection and quantification were in the range of 5.8-22.2ngmL(-1) and 19.2-74.0ngmL(-1), respectively. The relative standard deviations (RSDs) of intra-day and inter-day determination were lower than 8.80% and 11.19%, respectively. The recoveries were between 65.51% and 92.32% with RSDs lower than 8.95%. Compared with ultrasound-assisted extraction (UAE) and soxhlet extraction, the present method consumed less sample, organic solvent, and extraction time, although the extraction yields obtained by S-SIL-based MSPD are slightly lower than those obtained by UAE. Copyright © 2014 Elsevier B.V. All rights reserved.

Spectroscopy of lithium atoms sublimated from isolation matrix of solid Ne.

PubMed

Sacramento, R L; Scudeller, L A; Lambo, R; Crivelli, P; Cesar, C L

2011-10-07

We have studied, via laser absorption spectroscopy, the velocity distribution of (7)Li atoms released from a solid neon matrix at cryogenic temperatures. The Li atoms are implanted into the Ne matrix by laser ablation of a solid Li precursor. A heat pulse is then applied to the sapphire substrate sublimating the matrix together with the isolated atoms at around 12 K. We find interesting differences in the velocity distribution of the released Li atoms from the model developed for our previous experiment with Cr [R. Lambo, C. C. Rodegheri, D. M. Silveira, and C. L. Cesar, Phys. Rev. A 76, 061401(R) (2007)]. This may be due to the sublimation regime, which is at much lower flux for the Li experiment than for the Cr experiment, as well as to the different collisional cross sections between those species to the Ne gas. We find a drift velocity compatible with Li being thermally sublimated at 11-13 K, while the velocity dispersion around this drift velocity is low, around 5-7 K. With a slow sublimation of the matrix we can determine the penetration depth of the laser ablated Li atoms into the Ne matrix, an important information that is not usually available in most matrix isolation spectroscopy setups. The present results with Li, together with the previous results with Cr suggest this to be a general technique for obtaining cryogenic atoms, for spectroscopic studies, as well as for trap loading. The release of the isolated atoms is also a useful tool to study and confirm details of the matrix isolated atoms which are masked or poorly understood in the solid. © 2011 American Institute of Physics

Processing and properties of SiC whisker reinforced Si sub 3 N sub 4 ceramic matrix composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nunn, S.D.

1991-01-01

Silicon carbide whiskers reinforced silicon nitride ceramic matrix composites were pressureless sintered to high density by liquid phase sintering. Important processing parameters included: whisker dispersion by ultrasonic shear homogenization, particle refinement by attrition milling, pressure slip casting to obtain high greed densities, and sintering in a protective powder bed to limit decomposition. Composites with a {beta}20-Si{sub 3}N{sub 4} solid solution matrix containing 20 vol.% SiC whiskers were sintered to 98-100% theoretical density; composites having a Si{sub 3}N{sub 4} matrix containing YAG sintering aid were sintered to 98% of the theoretical density with 20 vol.% SiC whiskers, and 94% density withmore » 30 vol.% SiC whiskers. Analysis of the pressureless sintered composites revealed orientation of the SiC whiskers and the Si{sub 3}N{sub 4} matrix grains. The mechanical properties of hot pressed Si{sub 3}N{sub 4} composites reinforced with 20 vol.% SiC whiskers were shown to depend on the characteristics of the intergranular phase. Variations in the properties of the composites were analyzed in terms of the amount and morphology of the secondary phase, and the development of internal residual stresses due to the thermal expansion mismatch between the sintering aid phase at the grain boundaries.« less

Simultaneous determination of phenolic compounds in Equisetum palustre L. by ultra high performance liquid chromatography with tandem mass spectrometry combined with matrix solid-phase dispersion extraction.

PubMed

Wei, Zuofu; Pan, Youzhi; Li, Lu; Huang, Yuyang; Qi, Xiaolin; Luo, Meng; Zu, Yuangang; Fu, Yujie

2014-11-01

A method based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with tandem mass spectrometry is presented for the extraction and determination of phenolic compounds in Equisetum palustre. This method combines the high efficiency of matrix solid-phase dispersion extraction and the rapidity, sensitivity, and accuracy of ultra high performance liquid chromatography with tandem mass spectrometry. The influential parameters of the matrix solid-phase dispersion extraction were investigated and optimized. The optimized conditions were as follows: silica gel was selected as dispersing sorbent, the ratio of silica gel to sample was selected to be 2:1 (400/200 mg), and 8 mL of 80% methanol was used as elution solvent. Furthermore, a fast and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the determination of nine phenolic compounds in E. palustre. This method was carried out within <6 min, and exhibited satisfactory linearity, precision, and recovery. Compared with ultrasound-assisted extraction, the proposed matrix solid-phase dispersion procedure possessed higher extraction efficiency, and was more convenient and time saving with reduced requirements on sample and solvent amounts. All these results suggest that the developed method represents an excellent alternative for the extraction and determination of active components in plant matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

CO2 in solid para-hydrogen: spectral splitting and the CO2···(o-H2)n clusters.

PubMed

Du, Jun-He; Wan, Lei; Wu, Lei; Xu, Gang; Deng, Wen-Ping; Liu, An-Wen; Chen, Yang; Hu, Shui-Ming

2011-02-17

Complicated high-resolution spectral structures are often observed for molecules doped in solid molecular hydrogen. The structures can result from miscellaneous effects and are often interpreted differently in references. The spectrum of the ν(3) band of CO(2) in solid para-H(2) presents a model system which exhibits rich spectral structures. With the help of the potential energy simulation of the CO(2) molecule doped in para-hydrogen matrix, and extensive experiments with different CO(2) isotopologues and different ortho-hydrogen concentrations in the matrix, the spectral features observed in p-H(2) matrix are assigned to the CO(2)···(o-H(2))(n) clusters and also to energy level splitting that is due to different alignments of the doped CO(2) molecules in the matrix. The assignments are further supported by the dynamics analysis and also by the spectrum recorded with sample codoped with O(2) which serves as catalyst transferring o-H(2) to p-H(2) in the matrix at 4 K temperature. The observed spectral features of CO(2)/pH(2) can potentially be used as an alternative readout of the temperature and orthohydrogen concentration in the solid para-hydrogen.

Thermodynamic modeling of solid solutions between monosulfate and monochromate 3CaO Bullet Al{sub 2}O{sub 3} Bullet Ca[(CrO{sub 4}){sub x}(SO{sub 4}){sub 1-x}] Bullet nH{sub 2}O

DOE Office of Scientific and Technical Information (OSTI.GOV)

Leisinger, Sabine M., E-mail: sabine.leisinger@eawag.ch; Institute of Biogeochemistry and Pollutant Dynamics, ETH, CH-8092 Zurich; Lothenbach, Barbara

2012-01-15

In hydrated cement paste AFm-phases are regarded to play an important role in the binding of the toxic contaminant chromate through isomorphic substitution with sulfate. Solid solutions formation can lower the solubility of the solids, thus reducing chromate leaching concentrations. Solid solutions between monosulfate and monochromate were synthesized and characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX) and inductive coupled plasma optical emission spectroscopy (ICP-OES). Based on the measured ion concentrations in solution total solubility products of the solid solution series were determined. For pure monochromate a logK = - 28.4more » {+-} 0.7 was determined. Results from solid and solution analysis showed that limited solid solutions exist. Based on XRD diffractograms a solid solution with a miscibility gap 0.15 < Crx < 0.85 with a dimensionless Guggenheim parameter of 2.43 was proposed.« less

Three-wave resonant interactions: Multi-dark-dark-dark solitons, breathers, rogue waves, and their interactions and dynamics

NASA Astrophysics Data System (ADS)

Zhang, Guoqiang; Yan, Zhenya; Wen, Xiao-Yong

2018-03-01

We investigate three-wave resonant interactions through both the generalized Darboux transformation method and numerical simulations. Firstly, we derive a simple multi-dark-dark-dark-soliton formula through the generalized Darboux transformation. Secondly, we use the matrix analysis method to avoid the singularity of transformed potential functions and to find the general nonsingular breather solutions. Moreover, through a limit process, we deduce the general rogue wave solutions and give a classification by their dynamics including bright, dark, four-petals, and two-peaks rogue waves. Ever since the coexistence of dark soliton and rogue wave in non-zero background, their interactions naturally become a quite appealing topic. Based on the N-fold Darboux transformation, we can derive the explicit solutions to depict their interactions. Finally, by performing extensive numerical simulations we can predict whether these dark solitons and rogue waves are stable enough to propagate. These results can be available for several physical subjects such as fluid dynamics, nonlinear optics, solid state physics, and plasma physics.

Alcohol dose dumping: The influence of ethanol on hot-melt extruded pellets comprising solid lipids.

PubMed

Jedinger, N; Schrank, S; Mohr, S; Feichtinger, A; Khinast, J; Roblegg, E

2015-05-01

The objective of the present study was to investigate interactions between alcohol and hot-melt extruded pellets and the resulting drug release behavior. The pellets were composed of vegetable calcium stearate as matrix carrier and paracetamol or codeine phosphate as model drugs. Two solid lipids (Compritol® and Precirol®) were incorporated into the matrix to form robust/compact pellets. The drug release characteristics were a strong function of the API solubility, the addition of solid lipids, the dissolution media composition (i.e., alcohol concentration) and correspondingly, the pellet wettability. Pellets comprising paracetamol, which is highly soluble in ethanol, showed alcohol dose dumping regardless of the matrix composition. The wettability increased with increasing ethanol concentrations due to higher paracetamol solubilities yielding increased dissolution rates. For pellets containing codeine phosphate, which has a lower solubility in ethanol than in acidic media, the wettability was a function of the matrix composition. Dose dumping occurred for formulations comprising solid lipids as they showed increased wettabilities with increasing ethanol concentrations. In contrast, pellets comprising calcium stearate as single matrix component showed robustness in alcoholic media due to wettabilities that were not affected by the addition of ethanol. The results clearly indicate that the physico-chemical properties of the drug and the matrix systems are crucial for the design of ethanol-resistant dosage forms. Moreover, hydrophobic calcium stearate can be considered a suitable matrix system that minimizes the risk of ethanol-induced dose dumping for certain API's. Copyright © 2015 Elsevier B.V. All rights reserved.

A review on management of chrome-tanned leather shavings: a holistic paradigm to combat the environmental issues.

PubMed

Pati, Anupama; Chaudhary, Rubina; Subramani, Saravanabhavan

2014-10-01

Raw hide/skins come to the tanners as a by-product of meat industry which is converted into value-added leather as product for fashion market. Leather manufacturing is a chemical process of natural biological matrix. It employs a huge quantity of water and inorganic and organic chemicals for processing and thereby discharges solid and liquid wastes into the environment. One of the potential solid wastes generated from leather industry is chrome-tanned leather shavings (CTLSs), and its disposal is increasingly becoming a huge challenge on disposal to tanners due to presence of heavy metal chromium. Hence, finding a sustainable solution to the CTLS disposal problem is a prime challenge for global tanners and researchers. This paper aims to the deeper review of various disposal methods on CTLS such as protein, chromium, and energy recovery processes and its utilization methodologies. Sustainable technologies have been developed to overcome CTLS solid wastes emanating from leather processing operations. Further, this review paper brings a broader classification of developed methodologies for treatment of CTLSs.

Structural, Electronic, and Optical Properties of BiOX1-xYx (X, Y = F, Cl, Br, and I) Solid Solutions from DFT Calculations.

PubMed

Zhao, Zong-Yan; Liu, Qing-Lu; Dai, Wen-Wu

2016-08-23

Six BiOX1-xYx (X, Y = F, Cl, Br, and I) solid solutions have been systematically investigated by density functional theory calculations. BiOCl1-xBrx, BiOBr1-xIx, and BiOCl1-xIx solid solutions have very small bowing parameters; as such, some of their properties increase almost linearly with increasing x. For BiOF1-xYx solid solutions, the bowing parameters are very large and it is extremely difficult to fit the related calculated data by a single equation. Consequently, BiOX1-xYx (X, Y = Cl, Br, and I) solid solutions are highly miscible, while BiOF1-xYx (Y = Cl, Br, and I) solid solutions are partially miscible. In other words, BiOF1-xYx solid solutions have miscibility gaps or high miscibility temperature, resulting in phase separation and F/Y inhomogeneity. Comparison and analysis of the calculated results and the related physical-chemical properties with different halogen compositions indicates that the parameters of BiOX1-xYx solid solutions are determined by the differences of the physical-chemical properties of the two halogen compositions. In this way, the large deviation of some BiOX1-xYx solid solutions from Vegard's law observed in experiments can be explained. Moreover, the composition ratio of BiOX1-xYx solid solutions can be measured or monitored using optical measurements.

Solid state and aqueous behavior of uranyl peroxide cage clusters

NASA Astrophysics Data System (ADS)

Pellegrini, Kristi Lynn

Uranyl peroxide cage clusters include a large family of more than 50 published clusters of a variety of sizes, which can incorporate various ligands including pyrophosphate and oxalate. Previous studies have reported that uranyl clusters can be used as a method to separate uranium from a solid matrix, with potential applications in reprocessing of irradiated nuclear fuel. Because of the potential applications of these novel structures in an advanced nuclear fuel cycle and their likely presence in areas of contamination, it is important to understand their behavior in both solid state and aqueous systems, including complex environments where other ions are present. In this thesis, I examine the aqueous behavior of U24Pp 12, as well as aqueous cluster systems with added mono-, di-, and trivalent cations. The resulting solutions were analyzed using dynamic light scattering and ultra-small angle X-ray scattering to evaluate the species in solution. Precipitates of these systems were analyzed using powder X-ray diffraction, X-ray fluorescence spectrometry, and Raman spectroscopy. The results of these analyses demonstrate the importance of cation size, charge, and concentration of added cations on the aqueous behavior of uranium macroions. Specifically, aggregates of various sizes and shapes form rapidly upon addition of cations, and in some cases these aggregates appear to precipitate into an X-ray amorphous material that still contains U24Pp12 clusters. In addition, I probe aggregation of U24Pp12 and U60, another uranyl peroxide cage cluster, in mixed solvent water-alcohol systems. The aggregation of uranyl clusters in water-alcohol systems is a result of hydrogen bonding with polar organic molecules and the reduction of the dielectric constant of the system. Studies of aggregation of uranyl clusters also allow for comparison between the newer uranyl polyoxometalate family and century-old transition metal polyoxometalates. To complement the solution studies of uranyl cage clusters, solid state analyses of U24Pp12 are presented, including single crystal X-ray diffraction and preliminary single crystal neutron diffraction. Solid state analyses are used to probe the complicated bonding environments between U24Pp12 and crystallized counterions, giving further insight into the importance of cluster protonation and counterions in uranyl cluster systems. The combination of solid state and solution techniques provides information about the complicated nature of uranyl peroxide nanoclusters, and insight towards future applications of clusters in the advanced nuclear fuel cycle and the environment.

Graphene nanocomposites for electrochemical cell electrodes

DOEpatents

Zhamu, Aruna; Jang, Bor Z.; Shi, Jinjun

2015-11-19

A composite composition for electrochemical cell electrode applications, the composition comprising multiple solid particles, wherein (a) a solid particle is composed of graphene platelets dispersed in or bonded by a first matrix or binder material, wherein the graphene platelets are not obtained from graphitization of the first binder or matrix material; (b) the graphene platelets have a length or width in the range of 10 nm to 10 .mu.m; (c) the multiple solid particles are bonded by a second binder material; and (d) the first or second binder material is selected from a polymer, polymeric carbon, amorphous carbon, metal, glass, ceramic, oxide, organic material, or a combination thereof. For a lithium ion battery anode application, the first binder or matrix material is preferably amorphous carbon or polymeric carbon. Such a composite composition provides a high anode capacity and good cycling response. For a supercapacitor electrode application, the solid particles preferably have meso-scale pores therein to accommodate electrolyte.

The Raman spectrum of Ca-Mg-Fe carbonates; Applications in geobiology

NASA Astrophysics Data System (ADS)

van Zuilen, M. A.; Rividi, N.; Ménez, B.; Philippot, P.

2012-04-01

Carbonates form a very important mineral group in geobiological studies. They are a common mineral matrix for putative carbonaceous microfossils in Archean greenstone belts, form an important chemical deposit in seafloor hydrothermal systems, and are a common product in biomineralization processes. In many geobiological studies there is a specific need for simple characterization of carbonate composition while avoiding complex sample preparation or sample destruction. Raman spectroscopy is a highly versatile non-destructive technique enabling in-situ characterization of minerals and carbonaceous materials. It can be combined with confocal microscopy enabling high-resolution Raman mapping of entire rock thin sections, or can be integrated in submersibles and potentially Mars-rovers for direct field-based mineral identification. It is thus important that well-established spectral databases exist which enable unambiguous identification of a wide variety of carbonate minerals. The most common carbonates in the Ca-Mg-Fe system include the CaCO3 polymorphs calcite, aragonite, and vaterite, as well as the solid solutions CaMg(CO3)2-CaFe(CO3)2 (dolomite-ankerite) and MgCO3-FeCO3 (magnesite-siderite). Although various carbonate end-members have been studied exhaustively by Raman spectroscopy, a simple protocol for rapid distinction of various carbonate solid solutions is still lacking. Here we present a detailed study of Raman shifts in various carbonate standards of known composition in the Ca-Mg-Fe system. Carbonates with rhombohedral symmetry display a Raman spectrum with six characteristic vibrational modes - four of these represent vibrations within the (CO3)2- unit and two represent external vibrations of the crystal lattice. We show that Raman band shifts of internal mode 2ν2 (range 1725-1765 cm-1), and external modes T (range 170-215 cm-1) and L (range 285-330 cm-1) for siderite-magnesite and ankerite-dolomite solid solutions display distinct and well defined positive correlations with Mg number (Mg/Mg+Fe+Mn+Ca). Raman shifts calibrated as a function of Mg number were used in turn to evaluate the chemical composition of natural carbonate samples. In particular it is shown that detailed micron-resolution Raman maps can be generated of carbonate crystal-zonation in hydrothermally altered sedimentary deposits from Archean greenstone belts. Large spectral-range analysis (140-2000 cm-1) in static-mode (centered at 1150 cm-1) allows for combined Raman mapping of both carbonate-composition (2ν2, T, L modes) as well as kerogen structural ordering (D1-D4 and G modes in the range 1100-1700 cm-1), and therefore allows for simultaneous characterization of putative organic microfossils and associated carbonate matrix in metamorphosed Archean rock samples. Finally, it will be shown that these carbonate solid solutions can be distinguished from other end-member carbonates such as calcite, vaterite and the orthorhombic polymorph aragonite.

Solution of matrix equations using sparse techniques

NASA Technical Reports Server (NTRS)

Baddourah, Majdi

1994-01-01

The solution of large systems of matrix equations is key to the solution of a large number of scientific and engineering problems. This talk describes the sparse matrix solver developed at Langley which can routinely solve in excess of 263,000 equations in 40 seconds on one Cray C-90 processor. It appears that for large scale structural analysis applications, sparse matrix methods have a significant performance advantage over other methods.

Solid phase immobilization of optically responsive liposomes insol-gel materials for chemical and biological sensing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yamanaka, Stacey A.; Charych, Deborah H.; Loy, Douglas A.

1997-04-01

Liposomes enhanced with surface recognition groups have previously been found to have high affinity for heavy metal ions and virus particles with unique fluorescent and colorimetric responses, respectively. These lipid aggregate systems have now been successfully immobilized in a silica matrix via the sol-gel method, affording sensor materials that are robust, are easily handled, and offer optical clarity. The mild processing conditions allow quantitative entrapment of preformed liposomes without modification of the aggregate structure. Lipid extraction studies of immobilized nonpolymerized liposomes showed no lipid leakage in aqueous solution over a period of 3 months. Heavy metal fluorescent sensor materials preparedmore » with 5 percent N-[8-[1-octadecyl-2-(9-(1-pyrenyl)nonyl)-rac-glyceroyl]-3,6-dioxaoctyl]imino acid/distearylphosphatidylcholineliposomes exhibited a 4-50-fold enhancement in sensitivity to various metal ions compared to that of the liposomes in free solution. Through ionic attraction the anionic silicate surface, at the experimental pH of 7.4, may act as a preconcentrator of divalent metal ions, boosting the gel's internal metal concentration. Entrapped sialic acid-coated polydiacetylene liposomes responded with colorimetric signaling to influenza virus X31, although slower than the free liposomes in solution. The successful transport of the virus (50-100 nm diameter) reveals a large pore diameter of the gel connecting the liposome to the bulk solution. The porous and durable silica matrix additionally provides a protective barrier to biological attack (bacterial, fungal) and allows facile recycling of the liposome heavy metal sensor.« less

Formation of Al3Ti/Mg composite by powder metallurgy of Mg-Al-Ti system.

PubMed

Yang, Zi R; Qi Wang, Shu; Cui, Xiang H; Zhao, Yu T; Gao, Ming J; Wei, Min X

2008-07-01

An in situ titanium trialuminide (Al 3 Ti)-particle-reinforced magnesium matrix composite has been successfully fabricated by the powder metallurgy of a Mg-Al-Ti system. The reaction processes and formation mechanism for synthesizing the composite were studied by differential scanning calorimetry (DSC), x-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDS). Al 3 Ti particles are found to be synthesized in situ in the Mg alloy matrix. During the reaction sintering of the Mg-Al-Ti system, Al 3 Ti particles are formed through the reaction of liquid Al with as-dissolved Ti around the Ti particles. The formed intermetallic particles accumulate at the original sites of the Ti particles. As sintering time increases, the accumulated intermetallic particles disperse and reach a relatively homogeneous distribution in the matrix. It is found that the reaction process of the Mg-Al-Ti system is almost the same as that of the Al-Ti system. Mg also acts as a catalytic agent and a diluent in the reactions and shifts the reactions of Al and Ti to lower temperatures. An additional amount of Al is required for eliminating residual Ti and solid-solution strengthening of the Mg matrix.

A Green's function method for two-dimensional reactive solute transport in a parallel fracture-matrix system

NASA Astrophysics Data System (ADS)

Chen, Kewei; Zhan, Hongbin

2018-06-01

The reactive solute transport in a single fracture bounded by upper and lower matrixes is a classical problem that captures the dominant factors affecting transport behavior beyond pore scale. A parallel fracture-matrix system which considers the interaction among multiple paralleled fractures is an extension to a single fracture-matrix system. The existing analytical or semi-analytical solution for solute transport in a parallel fracture-matrix simplifies the problem to various degrees, such as neglecting the transverse dispersion in the fracture and/or the longitudinal diffusion in the matrix. The difficulty of solving the full two-dimensional (2-D) problem lies in the calculation of the mass exchange between the fracture and matrix. In this study, we propose an innovative Green's function approach to address the 2-D reactive solute transport in a parallel fracture-matrix system. The flux at the interface is calculated numerically. It is found that the transverse dispersion in the fracture can be safely neglected due to the small scale of fracture aperture. However, neglecting the longitudinal matrix diffusion would overestimate the concentration profile near the solute entrance face and underestimate the concentration profile at the far side. The error caused by neglecting the longitudinal matrix diffusion decreases with increasing Peclet number. The longitudinal matrix diffusion does not have obvious influence on the concentration profile in long-term. The developed model is applied to a non-aqueous-phase-liquid (DNAPL) contamination field case in New Haven Arkose of Connecticut in USA to estimate the Trichloroethylene (TCE) behavior over 40 years. The ratio of TCE mass stored in the matrix and the injected TCE mass increases above 90% in less than 10 years.

Wood composites

Treesearch

Lars Berglund; Roger M. Rowell

2005-01-01

A composite can be defined as two or more elements held together by a matrix. By this definition, what we call “solid wood” is a composite. Solid wood is a three-dimensional composite composed of cellulose, hemicelluloses and lignin (with smaller amounts of inorganics and extractives), held together by a lignin matrix. The advantages of developing wood composites are (...

Towards an acoustic model-based poroelastic imaging method: I. Theoretical foundation.

PubMed

Berry, Gearóid P; Bamber, Jeffrey C; Armstrong, Cecil G; Miller, Naomi R; Barbone, Paul E

2006-04-01

The ultrasonic measurement and imaging of tissue elasticity is currently under wide investigation and development as a clinical tool for the assessment of a broad range of diseases, but little account in this field has yet been taken of the fact that soft tissue is porous and contains mobile fluid. The ability to squeeze fluid out of tissue may have implications for conventional elasticity imaging, and may present opportunities for new investigative tools. When a homogeneous, isotropic, fluid-saturated poroelastic material with a linearly elastic solid phase and incompressible solid and fluid constituents is subjected to stress, the behaviour of the induced internal strain field is influenced by three material constants: the Young's modulus (E(s)) and Poisson's ratio (nu(s)) of the solid matrix and the permeability (k) of the solid matrix to the pore fluid. New analytical expressions were derived and used to model the time-dependent behaviour of the strain field inside simulated homogeneous cylindrical samples of such a poroelastic material undergoing sustained unconfined compression. A model-based reconstruction technique was developed to produce images of parameters related to the poroelastic material constants (E(s), nu(s), k) from a comparison of the measured and predicted time-dependent spatially varying radial strain. Tests of the method using simulated noisy strain data showed that it is capable of producing three unique parametric images: an image of the Poisson's ratio of the solid matrix, an image of the axial strain (which was not time-dependent subsequent to the application of the compression) and an image representing the product of the aggregate modulus E(s)(1-nu(s))/(1+nu(s))(1-2nu(s)) of the solid matrix and the permeability of the solid matrix to the pore fluid. The analytical expressions were further used to numerically validate a finite element model and to clarify previous work on poroelastography.

Method of making carbon fiber-carbon matrix reinforced ceramic composites

NASA Technical Reports Server (NTRS)

Williams, Brian (Inventor); Benander, Robert (Inventor)

2007-01-01

A method of making a carbon fiber-carbon matrix reinforced ceramic composite wherein the result is a carbon fiber-carbon matrix reinforcement is embedded within a ceramic matrix. The ceramic matrix does not penetrate into the carbon fiber-carbon matrix reinforcement to any significant degree. The carbide matrix is a formed in situ solid carbide of at least one metal having a melting point above about 1850 degrees centigrade. At least when the composite is intended to operate between approximately 1500 and 2000 degrees centigrade for extended periods of time the solid carbide with the embedded reinforcement is formed first by reaction infiltration. Molten silicon is then diffused into the carbide. The molten silicon diffuses preferentially into the carbide matrix but not to any significant degree into the carbon-carbon reinforcement. Where the composite is intended to operate between approximately 2000 and 2700 degrees centigrade for extended periods of time such diffusion of molten silicon into the carbide is optional and generally preferred, but not essential.

Iterative methods for mixed finite element equations

NASA Technical Reports Server (NTRS)

Nakazawa, S.; Nagtegaal, J. C.; Zienkiewicz, O. C.

1985-01-01

Iterative strategies for the solution of indefinite system of equations arising from the mixed finite element method are investigated in this paper with application to linear and nonlinear problems in solid and structural mechanics. The augmented Hu-Washizu form is derived, which is then utilized to construct a family of iterative algorithms using the displacement method as the preconditioner. Two types of iterative algorithms are implemented. Those are: constant metric iterations which does not involve the update of preconditioner; variable metric iterations, in which the inverse of the preconditioning matrix is updated. A series of numerical experiments is conducted to evaluate the numerical performance with application to linear and nonlinear model problems.

Single crystal structure analyses of scheelite-powellite CaW1-xMoxO4 solidsolutions and unique occurrence in Jisyakuyama skarn deposits

NASA Astrophysics Data System (ADS)

Yamashita, K.; Yoshiasa, A.; Miyazaki, H.; Tokuda, M.; Tobase, T.; Isobe, H.; Nishiyama, T.; Sugiyama, K.; Miyawaki, R.

2017-12-01

Jisyakuyama skarn deposit, Fukuchi, Fukuoka, Japan, shows a simple occurrenceformed by penetration of hot water into limestone cracks. A unique occurrence of scheelite-powellite CaW1-xMoxO4 minerals is observed in the skarn deposit. Many syntheticexperiments for scheelite-powellite solid solutions have been reported as research onfluorescent materials. In this system it is known that a complete continuous solid solution isformed even at room temperature. In this study, we have carried out the chemical analyses,crystal structural refinements and detail description of occurrence on scheelite-powelliteminerals. We have also attempted synthesis of single crystal of solid solution in a widecomposition range. The chemical compositions were determined by JEOL scanningelectron microscope and EDS, INCA system. We have performed the crystal structurerefinements of the scheelite-powellite CaW1-xMoxO4 solid solutions (x=0.0-1.0) byRIGAKU single-crystal structure analysis system RAPID. The R and S values are around0.0s and 1.03. As the result of structural refinements of natural products and many solidsolutions, we confirm that most large natural single crystals have compositions at bothendmembers, and large solid solution crystals are rare. The lattice constants, interatomicdistances and other crystallographic parameters for the solid solution change uniquely withcomposition and it was confirmed as a continuous solid solution. Single crystals of scheeliteendmember + powellite endmember + solid solution with various compositions form anaggregate in the deposit (Figure 1). Crystal shapes of powellite and scheelite arehypidiomorphic and allotriomorphic, respectively. Many solid solution crystals areaccompanied by scheelite endmember and a compositional gap is observed betweenpowellite and solid-solution crystals. The presence of several penetration solutions withsignificantly different W and Mo contents may be assumed. This research can be expectedto lead to giving restrictive conditions to elucidate the mineralization process. Figure1. Scheelite + Powellite + solid solution aggregate

Analytical Solution for Transport with Bimolecular Reactions in Fracture-Matrix Systems with Application to In-Situ Chemical Oxidation

NASA Astrophysics Data System (ADS)

Rajaram, H.; Arshadi, M.

2016-12-01

In-situ chemical oxidation (ISCO) is an effective strategy for remediation of DNAPL contamination in fractured rock. During ISCO, an oxidant (e.g. permanganate) is typically injected through fractures and is consumed by bimolecular reactions with DNAPLs such as TCE and natural organic matter in the fracture and the adjacent rock matrix. Under these conditions, moving reaction fronts form and propagate along the fracture and into the rock matrix. The propagation of these reaction fronts is strongly influenced by the heterogeneity/discontinuity across the fracture-matrix interface (advective transport dominates in the fractures, while diffusive transport dominates in the rock matrix). We present analytical solutions for the concentrations of the oxidant, TCE and natural organic matter; and the propagation of the reaction fronts in a fracture-matrix system. Our approximate analytical solutions assume advection and reaction dominate over diffusion/dispersion in the fracture and neglect the latter. Diffusion and reaction with both TCE and immobile natural organic matter in the rock matrix are considered. The behavior of the reaction-diffusion equations in the rock matrix is posed as a Stefan problem where the diffusing oxidant reacts with both diffusing (TCE) and immobile (natural organic matter) reductants. Our analytical solutions establish that the reaction fronts propagate diffusively (i.e. as the square root of time) in both the matrix and the fracture. Our analytical solutions agree very well with numerical simulations for the case of uniform advection in the fracture. We also present extensions of our analytical solutions to non-uniform flows in the fracture by invoking a travel-time transformation. The non-uniform flow solutions are relevant to field applications of ISCO. The approximate analytical solutions are relevant to a broad class of reactive transport problems in fracture-matrix systems where moving reaction fronts occur.

Interference-free determination of trace copper in freshly ripened honeys by flame atomic absorption spectrometry following a preconcentration by solid-phase extraction and a two-step elution process.

PubMed

Pohl, Pawel; Stecka, Helena; Jamroz, Piotr

2014-02-01

A fast and straightforward procedure aimed at separating copper (Cu) ions from monosacharides and preconcentrating their traces before flame atomic absorption spectrometry (FAAS) measurements was developed, and its suitability was evaluated by the analysis of freshly ripened honeys on the content of this environmentally and physiologically relevant element. This procedure included the passage (at 20 mL/min) of 10 % (m/v) solutions of honeys (100 mL) through resin beds of Dowex 50 W × 8-400 to retain Cu by solid-phase extraction (SPE) and separate it from the glucose and fructose matrix. In turn, SPE columns were rinsed at 20 mL/min with 20 mL of water and subsequently washed with 20 mL of a 0.5 mol/L HNO3 solution (at 2.0 mL/min) to elute potassium and sodium. Preconcentrated Cu was stripped (at 2.0 mL/min) with 5.0 mL of a 2.0 mol/L HCl solution and determined by FAAS. The proposed procedure was used for the analysis of six ripened monoflower and multiflower honeys, enabling the measurement of Cu within the range of 0.17-0.42 μg/g and with a precision of 3-10%. Recoveries of Cu added to respective honey solutions were within 94-102%, proving the good accuracy of this procedure. The detection limit of Cu achieved with this SPE preconcentration/separation procedure and FAAS detection was 3.6 ng/g.

Fabrication of all-inorganic nanocrystal solids through matrix encapsulation of nanocrystal arrays.

PubMed

Kinder, Erich; Moroz, Pavel; Diederich, Geoffrey; Johnson, Alexa; Kirsanova, Maria; Nemchinov, Alexander; O'Connor, Timothy; Roth, Dan; Zamkov, Mikhail

2011-12-21

A general strategy for low-temperature processing of colloidal nanocrystals into all-inorganic films is reported. The present methodology goes beyond the traditional ligand-interlinking scheme and relies on encapsulation of morphologically defined nanocrystal arrays into a matrix of a wide-band gap semiconductor, which preserves optoelectronic properties of individual nanoparticles while rendering the nanocrystal film photoconductive. Fabricated solids exhibit excellent thermal stability, which is attributed to the heteroepitaxial structure of nanocrystal-matrix interfaces, and show compelling light-harvesting performance in prototype solar cells. © 2011 American Chemical Society

Mixed oxide solid solutions

DOEpatents

Magno, Scott; Wang, Ruiping; Derouane, Eric

2003-01-01

The present invention is a mixed oxide solid solution containing a tetravalent and a pentavalent cation that can be used as a support for a metal combustion catalyst. The invention is furthermore a combustion catalyst containing the mixed oxide solid solution and a method of making the mixed oxide solid solution. The tetravalent cation is zirconium(+4), hafnium(+4) or thorium(+4). In one embodiment, the pentavalent cation is tantalum(+5), niobium(+5) or bismuth(+5). Mixed oxide solid solutions of the present invention exhibit enhanced thermal stability, maintaining relatively high surface areas at high temperatures in the presence of water vapor.

NanoRelease: Pilot interlaboratory comparison of a weathering protocol applied to resilient and labile polymers with and without embedded carbon nanotubes

EPA Science Inventory

A major use of multi-walled carbon nanotubes (MWCNTs) is as functional fillers embedded in a solid matrix, such as plastics or coatings. Weathering and abrasion of the solid matrix during use can lead to environmental releases of the MWCNTs. Here we focus on a protocol to identif...

Influence wt.% of SiC and borax on the mechanical properties of AlSi-Mg-TiB-SiC composite by the method of semi solid stir casting

NASA Astrophysics Data System (ADS)

Bhiftime, E. I.; Guterres, Natalino F. D. S.; Haryono, M. B.; Sulardjaka, Nugroho, Sri

2017-04-01

SiC particle reinforced metal matrix composites (MMCs) with solid semi stir casting method is becoming popular in recent application (automotive, aerospace). Stirring the semi solid condition is proven to enhance the bond between matrix and reinforcement. The purpose of this study is to investigate the effect of the SiC wt.% and the addition of borax on mechanical properties of composite AlSi-Mg-TiB-SiC and AlSi-Mg-TiB-SiC/Borax. Specimens was tested focusing on the density, porosity, tensile test, impact test microstructure and SEM. AlSi is used as a matrix reinforced by SiC with percentage variations (10, 15, 20 wt.%). Giving wt.% Borax which is the ratio of 1: 4 between wt.% SiC. The addition of 1.5% of TiB gives grain refinement. The use of semi-solid stir casting method is able to increase the absorption of SiC particles into a matrix AlSi evenly. The improved composite presented here can be used as a guideline to make a new composite.

Reactive solute transport in an asymmetrical fracture-rock matrix system

NASA Astrophysics Data System (ADS)

Zhou, Renjie; Zhan, Hongbin

2018-02-01

The understanding of reactive solute transport in a single fracture-rock matrix system is the foundation of studying transport behavior in the complex fractured porous media. When transport properties are asymmetrically distributed in the adjacent rock matrixes, reactive solute transport has to be considered as a coupled three-domain problem, which is more complex than the symmetric case with identical transport properties in the adjacent rock matrixes. This study deals with the transport problem in a single fracture-rock matrix system with asymmetrical distribution of transport properties in the rock matrixes. Mathematical models are developed for such a problem under the first-type and the third-type boundary conditions to analyze the spatio-temporal concentration and mass distribution in the fracture and rock matrix with the help of Laplace transform technique and de Hoog numerical inverse Laplace algorithm. The newly acquired solutions are then tested extensively against previous analytical and numerical solutions and are proven to be robust and accurate. Furthermore, a water flushing phase is imposed on the left boundary of system after a certain time. The diffusive mass exchange along the fracture/rock matrixes interfaces and the relative masses stored in each of three domains (fracture, upper rock matrix, and lower rock matrix) after the water flushing provide great insights of transport with asymmetric distribution of transport properties. This study has the following findings: 1) Asymmetric distribution of transport properties imposes greater controls on solute transport in the rock matrixes. However, transport in the fracture is mildly influenced. 2) The mass stored in the fracture responses quickly to water flushing, while the mass stored in the rock matrix is much less sensitive to the water flushing. 3) The diffusive mass exchange during the water flushing phase has similar patterns under symmetric and asymmetric cases. 4) The characteristic distance which refers to the zero diffusion between the fracture and the rock matrix during the water flushing phase is closely associated with dispersive process in the fracture.

Directional solidification of Bi-Mn alloys using an applied magnetic field

NASA Technical Reports Server (NTRS)

Decarlo, J. L.; Pirich, R. G.

1987-01-01

Off-eutectic compositions of Bi-Mn were directionally solidified in applied transverse magnetic fields up to 3 kG, to determine the effects on thermal and solutal convection. Plane front directional solidification of eutectic and near-eutectic Bi-Mn results in a two-phase rodlike morphology consisting of ferromagnetic MnBi rods in a Bi solid solution matrix. Compositions of either side of the eutectic were studied in growth orientations vertically up and down. Temperature gradient was monitored during growth by means of an in-situ thermocouple. For Bi-rich compositions, the magnetic field appeared to increase mixing as determined from thermal, morphological, chemical, and magnetic analyses. For Mn-rich compositions, morphological and chemical analyses suggest some reduction in mixing due to application of the magnetic force. The capability for carrying out directional solidification of Bi-Mn in high longitudinal magnetic fields was established.

Composite Ni-Co-fly ash coatings on 5083 aluminium alloy

NASA Astrophysics Data System (ADS)

Panagopoulos, C. N.; Georgiou, E. P.; Tsopani, A.; Piperi, L.

2011-03-01

Ni-Co-fly ash coatings were deposited on zincate treated 5083 wrought aluminium alloy substrates with the aid of the electrodeposition technique. Structural and chemical characterization of the produced composite coatings was performed with the aid of X-ray diffraction (XRD), scanning electron microscopy (SEM) and electron dispersive X-ray analysis (EDS) techniques. The Ni-Co-fly ash coatings were found to consist of a crystalline Ni-Co solid solution with dispersed fly ash particles. In addition, chemical analysis of the Ni-Co matrix showed that it consisted of 80 wt.% Ni and 20 wt.% Co. The co-deposition of fly ash particles leads to a significant increase of the microhardness of the coating. The corrosion behaviour of the Ni-Co-fly ash/zincate coated aluminium alloy, in a 0.3 M NaCl solution (pH = 3.5), was studied by means of potentiodynamic corrosion experiments.

Acoustic coupled fluid-structure interactions using a unified fast multipole boundary element method.

PubMed

Wilkes, Daniel R; Duncan, Alec J

2015-04-01

This paper presents a numerical model for the acoustic coupled fluid-structure interaction (FSI) of a submerged finite elastic body using the fast multipole boundary element method (FMBEM). The Helmholtz and elastodynamic boundary integral equations (BIEs) are, respectively, employed to model the exterior fluid and interior solid domains, and the pressure and displacement unknowns are coupled between conforming meshes at the shared boundary interface to achieve the acoustic FSI. The low frequency FMBEM is applied to both BIEs to reduce the algorithmic complexity of the iterative solution from O(N(2)) to O(N(1.5)) operations per matrix-vector product for N boundary unknowns. Numerical examples are presented to demonstrate the algorithmic and memory complexity of the method, which are shown to be in good agreement with the theoretical estimates, while the solution accuracy is comparable to that achieved by a conventional finite element-boundary element FSI model.

Direct Solve of Electrically Large Integral Equations for Problem Sizes to 1M Unknowns

NASA Technical Reports Server (NTRS)

Shaeffer, John

2008-01-01

Matrix methods for solving integral equations via direct solve LU factorization are presently limited to weeks to months of very expensive supercomputer time for problems sizes of several hundred thousand unknowns. This report presents matrix LU factor solutions for electromagnetic scattering problems for problem sizes to one million unknowns with thousands of right hand sides that run in mere days on PC level hardware. This EM solution is accomplished by utilizing the numerical low rank nature of spatially blocked unknowns using the Adaptive Cross Approximation for compressing the rank deficient blocks of the system Z matrix, the L and U factors, the right hand side forcing function and the final current solution. This compressed matrix solution is applied to a frequency domain EM solution of Maxwell's equations using standard Method of Moments approach. Compressed matrix storage and operations count leads to orders of magnitude reduction in memory and run time.

Ultrasonic transient bounded-beam propagation in a solid cylinder waveguide embedded in a solid medium.

PubMed

Laguerre, Laurent; Grimault, Anne; Deschamps, Marc

2007-04-01

A semianalytical solution alternative and complementary to modal technique is presented to predict and interpret the ultrasonic pulsed-bounded-beam propagation in a solid cylinder embedded in a solid matrix. The spectral response to an inside axisymmetric velocity source of longitudinal and transversal cylindrical waves is derived from Debye series expansion of the embedded cylinder generalized cylindrical reflection/transmission coefficients. So, the transient guided wave response, synthesized by inverse double Fourier-Bessel transform, is expressed as a combination of the infinite medium contribution, longitudinal, transversal, and coupled longitudinal and transversal waveguide sidewall interactions. Simulated (f, 1/lambdaz) diagrams show the influence of the number of waveguide sidewall interactions to progressively recover dispersion curves. Besides, they show the embedding material filters specific signal portions by concentrating the propagating signal in regions where phase velocity is closer to phase velocity in steel. Then, simulated time waveforms using broadband high-frequency excitation show that signal leading portions exhibit a similar periodical pattern, for both free and embedded waveguides. Debye series-based interpretation shows that double longitudinal/transversal and transversal/longitudinal conversions govern the time waveform leading portion as well as the radiation attenuation in the surrounding cement grout. Finally, a methodology is deduced to minimize the radiation attenuation for the long-range inspection of embedded cylinders.

Temporal and spatial variability of chemical and isotopic composition of soil solutions from cambisols - field study and experiments.

PubMed

Schön, Walter; Mittermayr, Florian; Leis, Albrecht; Mischak, Irene; Dietzel, Martin

2016-12-01

The chemical and isotopic composition of soil solutions is highly relevant for environmental and forensic tasks. We investigated interstitial solutions from soil horizons of three cambisols in Styria (Austria). The soils consisted mainly of quartz, feldspar and clay minerals with a vertical variability. Two soil solution fractions from meso-, macro- and micropores (m) and micropores only (μ) were extracted at two subsequent hydraulic pressure steps corresponding to matrix potentials of up to pF 5.43 and from 5.43 to 5.73, respectively. While solute concentrations indicated diverse distribution in soil solution fractions m and μ, heavy stable hydrogen and oxygen isotopes of H 2 O (-92.5‰<δ 2 H<-34.4‰; -11.9‰<δ 18 O<-4.0‰, VSMOW) are clearly enriched in the μ versus m fractions. Principal component analysis on the hydrochemical data set indicates that the intensity of the overall silicate weathering is higher in autumn versus spring, whereas the anthropogenic impact on weathering behaves inversely. The anthropogenic impact is related to seasonal variability of nitrification of N-fertilizers. In consequence of evaluated signals for overall silicate weathering about three-fourths of the soil solutions sampled in autumn indicated elevated total dissolved solid concentration vs. those in spring accompanied with washing out solutes from the soil cover following precipitation events in autumn before sampling. Isotopic shift of soil solutions from the local meteoric water line in spring obviously followed an evaporation trend because of less precipitation and high evaporation before sampling. Experimentally simulated evaporation of soil samples confirmed the observed isotopic evaporation trend. Wetting experiments indicated the infiltration of water within minutes into the micropores of the soils. Exchange of water molecules between micro-, meso- and macropores is an almost instantaneous process and soil solutions in micropores are not as isolated from the soil water system as it was formerly suggested, e.g. for plant uptake. Highly dynamic and complex mechanisms in the gas-water-solid system of soils have to be considered for the application of elemental and isotope proxies related to environmental, forensic and agricultural tasks. Copyright © 2016 Elsevier B.V. All rights reserved.

Hybrid self-healing matrix using core-shell nanofibers and capsuleless microdroplets.

PubMed

Lee, Min Wook; An, Seongpil; Lee, Changmin; Liou, Minho; Yarin, Alexander L; Yoon, Sam S

2014-07-09

In this work, we developed novel self-healing anticorrosive hierarchical coatings that consist of several components. Namely, as a skeleton we prepared a core-shell nanofiber mat electrospun from emulsions of cure material (dimethyl methylhydrogen siloxane) in a poly(acrylonitrile) (PAN) solution in dimethylformamide. In these nanofibers, cure is in the core, while PAN is in the shell. The skeleton deposited on a protected surface is encased in an epoxy-based matrix, which contains emulsified liquid droplets of dimethylvinyl-terminated dimethylsiloxane resin monomer. When such hierarchical coatings are damaged, cure is released from the nanofiber cores and the resin monomer, released from the damaged matrix, is polymerized in the presence of cure. This polymerization and solidification process takes about 1-2 days and eventually heals the damaged material when solid poly(dimethylsiloxane) resin is formed. The self-healing effect was demonstrated using an electrochemical analogue of the scanning vibrating electrode technique. Damaged samples were left for 2 days. After that, the electric current through a damaged coating was found to be negligibly small for the samples with self-healing properties. On the other hand, for the samples without self-healing properties, the electric current was significant.

Reflection K-matrices for a nineteen vertex model with Uq [ osp (2 | 2) (2) ] symmetry

NASA Astrophysics Data System (ADS)

Vieira, R. S.; Lima Santos, A.

2017-09-01

We derive the solutions of the boundary Yang-Baxter equation associated with a supersymmetric nineteen vertex model constructed from the three-dimensional representation of the twisted quantum affine Lie superalgebra Uq [ osp (2 | 2) (2) ]. We found three classes of solutions. The type I solution is characterized by three boundary free-parameters and all elements of the corresponding reflection K-matrix are different from zero. In the type II solution, the reflection K-matrix is even (every element of the K-matrix with an odd parity is null) and it has only one boundary free-parameter. Finally, the type III solution corresponds to a diagonal reflection K-matrix with two boundary free-parameters.

Synthesis of phthalocyanine doped sol-gel materials

NASA Technical Reports Server (NTRS)

Dunn, Bruce

1993-01-01

The synthesis of sol-gel silica materials doped with three different types of metallophthalocyanines has been studied. Homogeneous materials of good optical quality were prepared and the first optical limiting measurements of dyes in sol-gel hosts were carried out. The properties of these solid state limiters are similar to limiters based on phthalocyanine (Pc) in solution. Sol-gel silica materials containing copper, tin and germanium phthalocyanines were investigated. The initial step in all cases was to prepare silica sols by the sonogel method using tetramethoxy silane (TMOS), HCl and distilled water. Thereafter, the synthesis depended upon the specific Pc and its solubility characteristics. Copper phthalocyanine tetrasulfonic acid tetra sodium salt (CuPc4S) is soluble in water and various doping levels (1 x 10 (exp -4) M to 1 x 10 (exp -5) M) were added to the sol. The group IV Pc's, SnPc(OSi(n-hexyl)3)2 and GePc(OSi(n-hexyl)3)2, are insoluble in water and the process was changed accordingly. In these cases, the compounds were dissolved in THF and then added to the sol. The Pc concentration in the sol was 2 x 10(exp -5)M. The samples were then aged and dried in the standard method of making xerogel monoliths. Comparative nanosecond optical limiting experiments were performed on silica xerogels that were doped with the different metallophthalocyanines. The ratio of the net excited state absorption cross section (sigma(sub e)) to the ground state cross section (sigma(sub g)) is an important figure of merit that is used to characterize these materials. By this standard the SnPc sample exhibits the best limiting for the Pc doped sol-gel materials. Its cross section ratio of 19 compares favorably with the value of 22 that was measured in toluene. The GePc materials appear to not be as useful as those containing SnPc. The GePc doped solids exhibit a higher onset energy (2.5 mj and lower cross section ratio, 7. The CuPc4S sol-gel material has a still lower cross section ratio, 4, however, the tetrasulfonate groups make the dye soluble in water which greatly facilitates its incorporation into the sol-gel matrix. The nonlinear transmission of CuPc4S in a pH 2 buffer solution and in a silica xerogel were compared. It is evident that the CuPc4S preserves its optical limiting behavior in the sol-gel matrix, indicating that the fundamental excited state absorption process is essentially the same for a molecule in solution or in the solid state. Although the spectroscopic details of energy level lifetimes are unknown, the significance is that passive optical limiting has been achieved in the solid state via incorporation of a dye into an inorganic host. The only compromise occurs at the extremely high energy regime where photobleaching is observed. This is a result of the limited mobility of the dye molecules in the solid silica host relative to a liquid host. The effects of photodegradation in the xerogel are additive, whereas the solution provides a supply of fresh molecules that are free to enter the active volume between pulses.

Solution behavior of PVP-VA and HPMC-AS-based amorphous solid dispersions and their bioavailability implications.

PubMed

Qian, Feng; Wang, Jennifer; Hartley, Ruiling; Tao, Jing; Haddadin, Raja; Mathias, Neil; Hussain, Munir

2012-10-01

To identify the mechanism behind the unexpected bio-performance of two amorphous solid dispersions: BMS-A/PVP-VA and BMS-A/HPMC-AS. Solubility of crystalline BMS-A in PVP-VA and HPMC-AS was measured by DSC. Drug-polymer interaction parameters were obtained by Flory-Huggins model fitting. Drug dissolution kinetics of spray-dried dispersions were studied under sink and non-sink conditions. BMS-A supersaturation was studied in the presence of pre-dissolved PVP-VA and HPMC-AS. Potency and crystallinity of undissolved solid dispersions were determined by HPLC and DSC. Polymer dissolution kinetics were obtained by mass balance calculation. Bioavailability of solid dispersions was assessed in dogs. In solid state, both polymers are miscible with BMS-A, while PVP-VA solublizes the drug better. BMS-A dissolves similarly from both solid dispersions in vitro regardless of dissolution method, while the HPMC-AS dispersion performed much better in vivo. At the same concentration, HPMC-AS is more effective in prolonging BMS-A supersaturation; this effect was negated by the slow dissolution rate of HPMC-AS. Further study revealed that fast PVP-VA dissolution resulted in elevated drug loading in undissolved dispersions and facilitated drug recrystallization before complete release. In contrast, the hydrophobicity and slower HPMC-AS dissolution prevented BMS-A recrystallization within the HPMC-AS matrix for >24 h. The lower bioavailability of PVP-VA dispersion was attributed to BMS-A recrystallization within the undissolved dispersion, due to hydrophilicity and fast PVP-VA dissolution rate. Polymer selection for solid dispersion development has significant impact on in vivo performance besides physical stability.

Field method for the determination of hexavalent chromium by ultrasonication and strong anion-exchange solid-phase extraction.

PubMed

Wang, J; Ashley, K; Marlow, D; England, E C; Carlton, G

1999-03-01

A simple, fast, sensitive, and economical field method was developed and evaluated for the determination of hexavalent chromium (CrVI) in environmental and workplace air samples. By means of ultrasonic extraction in combination with a strong anion-exchange solid-phase extraction (SAE-SPE) technique, the filtration, isolation, and determination of CrVI in the presence of trivalent chromium (CrIII) and potential interferents was achieved. The method entails (1) ultrasonication in basic ammonium buffer solution to extract CrVI from environmental matrixes; (2) SAE-SPE to separate CrVI from CrIII and interferences; (3) elution/acidification of the eluate; (4) complexation of chromium with 1,5-diphenylcarbazide; and (5) spectrophotometric determination of the colored chromium-diphenylcarbazone complex. Several critical parameters were optimized in order to effect the extraction of both soluble (K2CrO4) and insoluble (PbCrO4) forms of CrVI without inducing CrIII oxidation or CrVI reduction. The method allowed for the dissolution and purification of CrVI from environmental and workplace air sample matrixes for up to 24 samples simultaneously in less than 90 min (including ultrasonication). The results demonstrated that the method was simple, fast, quantitative, and sufficiently sensitive for the determination of occupational exposures of CrVI. The method is applicable for on-site monitoring of CrVI in environmental and industrial hygiene samples.

Accurate Exchange-Correlation Energies for the Warm Dense Electron Gas.

PubMed

Malone, Fionn D; Blunt, N S; Brown, Ethan W; Lee, D K K; Spencer, J S; Foulkes, W M C; Shepherd, James J

2016-09-09

The density matrix quantum Monte Carlo (DMQMC) method is used to sample exact-on-average N-body density matrices for uniform electron gas systems of up to 10^{124} matrix elements via a stochastic solution of the Bloch equation. The results of these calculations resolve a current debate over the accuracy of the data used to parametrize finite-temperature density functionals. Exchange-correlation energies calculated using the real-space restricted path-integral formalism and the k-space configuration path-integral formalism disagree by up to ∼10% at certain reduced temperatures T/T_{F}≤0.5 and densities r_{s}≤1. Our calculations confirm the accuracy of the configuration path-integral Monte Carlo results available at high density and bridge the gap to lower densities, providing trustworthy data in the regime typical of planetary interiors and solids subject to laser irradiation. We demonstrate that the DMQMC method can calculate free energies directly and present exact free energies for T/T_{F}≥1 and r_{s}≤2.

Nano-sized precipitate stability and its controlling factors in a NiAl-strengthened ferritic alloy

DOE PAGES

Sun, Zhiqian; Song, Gian; Ilavsky, Jan; ...

2015-11-05

Coherent B2-ordered NiAl-type precipitates have been used to reinforce solid-solution bodycentered- cubic iron for high-temperature application in fossil-energy power plants. In this study, the stability of nano-sized precipitates in a NiAl-strengthened ferritic alloy was investigated at 700 - 950°C using ultra-small angle X-ray scattering and electron microscopies. Here we show that the coarsening kinetics of NiAl-type precipitates is in excellent agreement with the ripening model in multicomponent alloys. We further demonstrate that the interfacial energy between the matrix and NiAl-type precipitates is strongly dependent to differences in the matrix/precipitate compositions. The results profile the ripening process in multicomponent alloys bymore » illustrating controlling factors (i.e., interfacial energy, diffusivities, and element partitioning). As a result, the study provides guidelines to design and develop high-temperature alloys with stable microstructures for long-term service.« less

Structural, thermodynamic, and mechanical properties of WCu solid solutions

NASA Astrophysics Data System (ADS)

Liang, C. P.; Wu, C. Y.; Fan, J. L.; Gong, H. R.

2017-11-01

Various properties of Wsbnd Cu solid solutions are systematically investigated through a combined use of first-principles calculation, cluster expansion, special quasirandom structures (SQS), and lattice dynamics. It is shown that SQS are effective to unravel the intrinsic nature of solid solutions, and that BCC and FCC W100-xCux solid solutions are energetically more stable when 0 ≤ x ≤ 70 and 70 < x ≤ 100, respectively. Calculations also reveal that the Debye model should be appropriate to derive thermodynamic properties of Wsbnd Cu, and that the coefficients of thermal expansion of W100-xCux solid solutions are much lower than those of corresponding mechanical mixtures. In addition, the G/B values of W100-xCux solid solutions reach a minimum at x = 50, which is fundamentally due to the softening of phonons as well as strong chemical bonding between W and Cu with a mainly metallic feature.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cai, Zhaobing

Ni-Cr-Co-Ti-V-Al high-entropy alloy coating on Ti-6Al-4V was synthesized by laser surface alloying. The coating is composed of a B2 matrix and (Co, Ni)Ti{sub 2} compounds with few β-Ti phases. Focused ion beam technique was utilized to prepare TEM sample and TEM observations agree well with XRD and SEM results. The formation of HEA phases is due to high temperature and rapid cooling rate during laser surface alloying. The thermodynamic parameters, ΔH{sub mix}, ΔS{sub mix}and δ as well as Δχ, should be used to predict the formation of the BCC solid solution, but they are not the strict criteria. Especially whenmore » Δχ reaches a high value (≥ 10%), BCC HEA will be partially decomposed, leading to the formation of (Co, Ni)Ti{sub 2} compound phases. - Highlights: •Preparing HEA coating on Ti-6Al-4V by laser surface alloying is successful. •The synthesized HEA coating mainly consists of BCC HEA and (Co, Ni)Ti{sub 2} compounds. •FIB technology was used to prepare the sample for TEM analysis. • ΔH{sub mix}, ΔS{sub mix}and δ as well as Δχ, should be all used to predict the formation of solid solution.« less

Effect of Boron Doping on Cellular Discontinuous Precipitation for Age-Hardenable Cu–Ti Alloys

PubMed Central

Semboshi, Satoshi; Ikeda, Jun; Iwase, Akihiro; Takasugi, Takayuki; Suzuki, Shigeru

2015-01-01

The effects of boron doping on the microstructural evolution and mechanical and electrical properties of age-hardenable Cu–4Ti (at.%) alloys are investigated. In the quenched Cu–4Ti–0.03B (at.%) alloy, elemental B (boron) is preferentially segregated at the grain boundaries of the supersaturated solid-solution phase. The aging behavior of the B-doped alloy is mostly similar to that of conventional age-hardenable Cu–Ti alloys. In the early stage of aging at 450 °C, metastable β′-Cu4Ti with fine needle-shaped precipitates continuously form in the matrix phase. Cellular discontinuous precipitates composed of the stable β-Cu4Ti and solid-solution laminates are then formed and grown at the grain boundaries. However, the volume fraction of the discontinuous precipitates is lower in the Cu–4Ti–0.03B alloy than the Cu–4Ti alloy, particularly in the over-aging period of 72–120 h. The suppression of the formation of discontinuous precipitates eventually results in improvement of the hardness and tensile strength. It should be noted that minor B doping of Cu–Ti alloys also effectively enhances the elongation to fracture, which should be attributed to segregation of B at the grain boundaries.

Effect of Heat Treatment on Borides Precipitation and Mechanical Properties of CoCrFeNiAl1.8Cu0.7B0.3Si0.1 High-Entropy Alloy Prepared by Arc-Melting and Laser-Cladding

NASA Astrophysics Data System (ADS)

Zhang, H.; Tang, H.; He, Y. Z.; Zhang, J. L.; Li, W. H.; Guo, S.

2017-11-01

Effects of heat treatment on borides precipitation and mechanical properties of arc-melted and laser-cladded CoCrNiFeAl1.8Cu0.7B0.3Si0.1 high-entropy alloys were comparatively studied. The arc-melted alloy contains lots of long strip borides distributed in the body-centered cubic phase, with a hardness about 643 HV0.5. Laser-cladding can effectively inhibit the boride precipitation and the laser-cladded alloy is mainly composed of a simple bcc solid solution, with a high hardness about 769 HV0.5, indicating the strengthening effect by interstitial boron atoms is greater than the strengthening by borides precipitation. Heat treatments between 800°C and 1200°C can simultaneously improve the hardness and fracture toughness of arc-melted alloys, owing to the boride spheroidization, dissolution, re-precipitation, and hence the increased boron solubility and nano-precipitation in the bcc solid solution. By contrast, the hardness of laser-cladded alloys reduce after heat treatments in the same temperature range, due to the decreased boron solubility in the matrix.

Improvement of a headspace solid phase microextraction-gas chromatography/mass spectrometry method for the analysis of wheat bread volatile compounds.

PubMed

Raffo, Antonio; Carcea, Marina; Castagna, Claudia; Magrì, Andrea

2015-08-07

An improved method based on headspace solid phase microextraction combined with gas chromatography-mass spectrometry (HS-SPME/GC-MS) was proposed for the semi-quantitative determination of wheat bread volatile compounds isolated from both whole slice and crust samples. A DVB/CAR/PDMS fibre was used to extract volatiles from the headspace of a bread powdered sample dispersed in a sodium chloride (20%) aqueous solution and kept for 60min at 50°C under controlled stirring. Thirty-nine out of all the extracted volatiles were fully identified, whereas for 95 other volatiles a tentative identification was proposed, to give a complete as possible profile of wheat bread volatile compounds. The use of an array of ten structurally and physicochemically similar internal standards allowed to markedly improve method precision with respect to previous HS-SPME/GC-MS methods for bread volatiles. Good linearity of the method was verified for a selection of volatiles from several chemical groups by calibration with matrix-matched extraction solutions. This simple, rapid, precise and sensitive method could represent a valuable tool to obtain semi-quantitative information when investigating the influence of technological factors on volatiles formation in wheat bread and other bakery products. Copyright © 2015 Elsevier B.V. All rights reserved.

Mechanisms of radiation-induced segregation in CrFeCoNi-based single-phase concentrated solid solution alloys

DOE PAGES

He, Mo-Rigen; Wang, Shuai; Shi, Shi; ...

2016-12-31

Single-phase concentrated solid solution alloys have attracted wide interest due to their superior mechanical properties and enhanced radiation tolerance, which make them promising candidates for the structural applications in next-generation nuclear reactors. However, little has been understood about the intrinsic stability of their as-synthesized, high-entropy configurations against radiation damage. In this paper, we report the element segregation in CrFeCoNi, CrFeCoNiMn, and CrFeCoNiPd equiatomic alloys when subjected to 1250 kV electron irradiations at 400 °C up to a damage level of 1 displacement per atom. Cr/Fe/Mn/Pd can deplete and Co/Ni can accumulate at radiation-induced dislocation loops, while the actively segregating elementsmore » are alloy-specific. Moreover, electron-irradiated matrix of CrFeCoNiMn and CrFeCoNiPd shows L1 0 (NiMn)-type ordering decomposition and <001>-oriented spinodal decomposition between Co/Ni and Pd, respectively. Finally, these findings are rationalized based on the atomic size difference and enthalpy of mixing between the alloying elements, and identify a new important requirement to the design of radiation-tolerant alloys through modification of the composition.« less

Conversion of depleted uranium hexafluoride to a solid uranium compound

DOEpatents

Rothman, Alan B.; Graczyk, Donald G.; Essling, Alice M.; Horwitz, E. Philip

2001-01-01

A process for converting UF.sub.6 to a solid uranium compound such as UO.sub.2 and CaF. The UF.sub.6 vapor form is contacted with an aqueous solution of NH.sub.4 OH at a pH greater than 7 to precipitate at least some solid uranium values as a solid leaving an aqueous solution containing NH.sub.4 OH and NH.sub.4 F and remaining uranium values. The solid uranium values are separated from the aqueous solution of NH.sub.4 OH and NH.sub.4 F and remaining uranium values which is then diluted with additional water precipitating more uranium values as a solid leaving trace quantities of uranium in a dilute aqueous solution. The dilute aqueous solution is contacted with an ion-exchange resin to remove substantially all the uranium values from the dilute aqueous solution. The dilute solution being contacted with Ca(OH).sub.2 to precipitate CaF.sub.2 leaving dilute NH.sub.4 OH.

Matrix solid-phase dispersion followed by liquid chromatography tandem mass spectrometry for the determination of selective ciclooxygenase-2 inhibitors in sewage sludge samples.

PubMed

Triñanes, Sara; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

2016-09-02

A straightforward single-step extraction method based on matrix solid-phase dispersion (MSPD), followed by high-performance liquid chromatography with hybrid quadrupole time of flight mass spectrometry (LC-QTOF-MS), was developed and optimized to determine five non-steroidal anti-inflammatory drugs (Valdecoxib, Etoricoxib, Parecoxib, Celecoxib and 2,5-Dimethylcelecoxib) in sewage sludge samples. The influence of different operational parameters on the extraction efficiency a well as in the matrix effects of the produced extracts was evaluated in detail. Under final working conditions, freeze dried samples (0.2g) were first soaked with 100μL of aqueous potassium hydroxide solution (60%, w/v), mixed with 1g of anhydrous sodium sulfate and dispersed with 1g of Florisil. This blend was transferred to the top of a polypropylene column cartridge containing 3g of silica. Analytes were recovered using 15mL of hexane/acetone (1:2, v/v) mixture. The extracts were concentrated by evaporation and reconstituted with 1mL of methanol/water (1:1, v/v), filtered and injected in the LC system. Quantification limits from 0.005 and 0.05ngg(-1) and absolute recoveries between 86 and 105% were achieved. Results indicated the presence of two of the targeted COXIBs in real samples of sewage sludge, the highest average concentration (22ngg(-1)) corresponding to celecoxib. Moreover, the screening capabilities of the LC-QTOF-MS system demonstrated that the developed MSPD extraction procedure might be useful for the selective extraction of some other pharmaceuticals (e.g. amiodarone and their metabolite N-desethylamiodarone, miconazole, clotrimazole and ketoprofen) from sludge samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and application of Fe3O4@SiO2@TiO2 for photocatalytic decomposition of organic matrix simultaneously with magnetic solid phase extraction of heavy metals prior to ICP-MS analysis.

PubMed

Habila, Mohamed A; ALOthman, Zeid A; El-Toni, Ahmed Mohamed; Labis, Joselito Puzon; Soylak, Mustafa

2016-07-01

Interference of organic compounds in the matrix of heavy metal solution could suppress their pre-concentration and detection processes. Therefore, this work aimed to develop simple and facile methods for separation of heavy metals before ICP-MS analysis. Fe3O4@SiO2@TiO2 core-double shell magnetic adsorbent was prepared and characterized by TEM, SEM, FTIR, XRD and surface area, and tested for Magnetic Solid Phase Extraction (MSPE) of Cu(II), Zn(II), Cd(II) and Pb(II). TEM micrograph of Fe3O4@SiO2@TiO2 reveals the uniform coating of TiO2 layer of about 20nm onto the Fe3O4@SiO2 nanoparticles and indicates that all nanoparticles are monodispersed and uniform. The saturation magnetization from the room-temperature hysteresis loops of Fe3O4 and Fe3O4@SiO2@TiO2 was found to be 72 and 40emug(-1), respectively, suggesting good separability of the nanoparticles. The Fe3O4@SiO2@TiO2 showed maximum adsorption capacity of 125, 137, 148 and 160mgg(-1) for Cu(II), Zn(II), Cd(II) and Pb(II) respectively, and the process was found to fit with the second order kinetic model and Langmuir isotherm. Fe3O4@SiO2@TiO2 showed efficient photocatalytic decomposition for tartrazine and sunset yellow (consider as Interfering organic compounds) in aqueous solution under the irradiation of UV light. The maximum recovery% was achieved at pH 5, by elution with 10mL of 2M nitric acid solution. The LODs were found to be 0.066, 0.049, 0.041 and 0.082µgL(-1) for Cu(II), Zn(II), Cd(II) and Pb(II), respectively while the LOQs were found to be 0.20, 0.15, 0.12 and 0.25µgL(-1) for Cu(II), Zn(II), Cd(II) and Pb(II), respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Spin generalization of the Calogero–Moser hierarchy and the matrix KP hierarchy

NASA Astrophysics Data System (ADS)

Pashkov, V.; Zabrodin, A.

2018-05-01

We establish a correspondence between rational solutions to the matrix KP hierarchy and the spin generalization of the Calogero–Moser system on the level of hierarchies. Namely, it is shown that the rational solutions to the matrix KP hierarchy appear to be isomorphic to the spin Calogero–Moser system in a sense that the dynamics of poles of solutions to the matrix KP hierarchy in the higher times is governed by the higher Hamiltonians of the spin Calogero–Moser integrable hierarchy with rational potential.

Numerical simulation on semi-solid die-casting of magnesium matrix composite based on orthogonal experiment

NASA Astrophysics Data System (ADS)

Liu, Huihui; He, Xiongwei; Guo, Peng

2017-04-01

Three factors (pouring temperature, injection speed and mold temperature) were selected to do three levels L9 (33)orthogonal experiment, then simulate processing of semi-solid die-casting of magnesium matrix composite by Flow-3D software. The stress distribution, temperature field and defect distribution of filling process were analyzed to find the optimized processing parameter with the help of orthogonal experiment. The results showed that semi-solid has some advantages of well-proportioned stress and temperature field, less defect concentrated in the surface. The results of simulation were the same as the experimental results.

Thermal analysis studies of doping effects on the conformational motions of polymer chains in solid solutions with lasing molecules

NASA Astrophysics Data System (ADS)

Kalogeras, Ioannis M.; Pallikari, Fotini; Vassilikou-Dova, Aglaia; Neagu, Eugen R.

2007-05-01

The advancement of the solid-state dye laser performance largely depends on the systematic study of the dye-matrix interactions at the nanoscopic scale. The current work deals with blends of a comparatively inert dye host, poly(methyl methacrylate) (PMMA), with nonionic/apolar (substituted perylenes) and ionic/polar (rhodamine 6G, pyrromethene 567) dyes at ≈10-4 mol L-1 loading. Differential scanning calorimetry (DSC) and thermally stimulated currents (TSC) were used to explore the relative strength of inter- and intramolecular guest-host interactions by monitoring blending-induced modifications of the high-temperature signals: the segmental relaxation, the space-charge relaxation, and the liquid-liquid transition. Both techniques revealed the antiplasticizing role of the oligomeric organics on the relaxation dynamics of polymer segments, evidenced by clear glass-transition temperature upshifts. It becomes apparent that this effect is independent of the size, polarity, and ionicity of the dopant, signifying a common mechanism underway. It is suggested that, at least for the dyes under investigation, the chromophores simply fill the voids within the matrix, imposing strong steric hindrances on the rearrangement of the long-range structure. A comparison between the present results and earlier low-temperature dielectric data reveals that the large-scale relaxation dynamics show stronger perturbations due to blending, in comparison to the localized rotational motion of the pendant groups. DSC provided estimates for the unconverted monomer percentages in the solid blends. These were also determined more accurately by nuclear magnetic resonance (NMR), which additionally confirmed that the tacticity of the chains is not affected by the presence of the dye.

Generalization of Jacobi's Decomposition Theorem to the Rotation and Translation of a Solid in a Fluid.

NASA Astrophysics Data System (ADS)

Chiang, Rong-Chang

Jacobi found that the rotation of a symmetrical heavy top about a fixed point is composed of the two torque -free rotations of two triaxial bodies about their centers of mass. His discovery rests on the fact that the orthogonal matrix which represents the rotation of a symmetrical heavy top is decomposed into a product of two orthogonal matrices, each of which represents the torque-free rotations of two triaxial bodies. This theorem is generalized to the Kirchhoff's case of the rotation and translation of a symmetrical solid in a fluid. This theorem requires the explicit computation, by means of theta functions, of the nine direction cosines between the rotating body axes and the fixed space axes. The addition theorem of theta functions makes it possible to decompose the rotational matrix into a product of similar matrices. This basic idea of utilizing the addition theorem is simple but the carry-through of the computation is quite involved and the full proof turns out to be a lengthy process of computing rather long and complex expressions. For the translational motion we give a new treatment. The position of the center of mass as a function of the time is found by a direct evaluation of the elliptic integral by means of a new theta interpretation of Legendre's reduction formula of the elliptic integral. For the complete solution of the problem we have added further the study of the physical aspects of the motion. Based on a complete examination of the all possible manifolds of the steady helical cases it is possible to obtain a full qualitative description of the motion. Many numerical examples and graphs are given to illustrate the rotation and translation of the solid in a fluid.

Thermodynamics of magnesian calcite solid-solutions at 25°C and 1 atm total pressure

USGS Publications Warehouse

Busenberg, Eurybiades; Plummer, Niel

1989-01-01

The stability of magnesian calcites was reexamined, and new results are presented for 28 natural inorganic, 12 biogenic, and 32 synthetic magnesian calcites. The magnesian calcite solid-solutions were separated into two groups on the basis of differences in stoichiometric solubility and other physical and chemical properties. Group I consists of solids of mainly metamorphic and hydrothermal origin, synthetic calcites prepared at high temperatures and pressures, and synthetic solids prepared at low temperature and very low calcite supersaturations () from artificial sea water or NaClMgCl2CaCl2solutions. Group I solids are essentially binary s of CaCO2 and MgCO2, and are thought to be relatively free of structural defects. Group II solid-solutions are of either biogenic origin or are synthetic magnesian calcites and protodolomites (0–20 and ∼ 45 mole percent MgCO3) prepared at high calcite supersaturations () from NaClNa2SO4MgCl2CaCl2 or NaClMgCl2CaCl2 solutions. Group II solid-solutions are treated as massively defective solids. The defects include substitution foreign ions (Na+ and SO42−) in the magnesian calcite lattice (point defects) and dislocations (~2 · 109 cm−2). Within each group, the excess free energy of mixing, GE, is described by the mixing model , where x is the mole fraction of the end-member Ca0.5Mg0.5CO3 in the solid-solution. The values of A0and A1 for Group I and II solids were evaluated at 25°C. The equilibrium constants of all the solids are closely described by the equation ln , where KC and KD are the equilibrium constants of calcite and Ca0.5Mg0.5CO3. Group I magnesian calcites were modeled as sub-regular solid-solutions between calcite and dolomite, and between calcite and “disordered dolomite”. Both models yield almost identical equilibrium constants for these magnesian calcites. The Group II magnesian calcites were modeled as sub-regular solid-solutions between defective calcite and protodolomite. Group I and II solid-solutions differ significantly in stability. The rate of crystal growth and the chemical composition of the aqueous solutions from which the solids were formed are the main factors controlling stoichiometric solubility of the magnesian calcites and the density of crystal defects. The literature on the occurrence and behavior of magnesian calcites in sea water and other aqueous solutions is also examined.

Comparison of ultrasonic and thermospray systems for high performance sample introduction to inductively coupled plasma atomic emission spectrometry

NASA Astrophysics Data System (ADS)

Conver, Timothy S.; Koropchak, John A.

1995-06-01

This paper describes detailed work done in our lab to compare analytical figures of merit for pneumatic, ultrasonic and thermospray sample introduction (SI) systems with three different inductively coupled plasma-atomic emission spectrometry (ICP-AES) instruments. One instrument from Leeman Labs, Inc. has an air path echelle spectrometer and a 27 MHz ICP. For low dissolved solid samples with this instrument, we observed that the ultrasonic nebulizer (USN) and fused silica aperture thermospray (FSApT) both offered similar LOD improvements as compared to pneumatic nebulization (PN), 14 and 16 times, respectively. Average sensitivities compared to PN were better for the USN, by 58 times, compared to 39 times for the FSApT. For solutions containing high dissolved solids we observed that FSApT optimized at the same conditions as for low dissolved solids, whereas USN required changes in power and gas flows to maintain a stable discharge. These changes degraded the LODs for USN substantially as compared to those utilized for low dissolved solid solutions, limiting improvement compared to PN to an average factor of 4. In general, sensitivities for USN were degraded at these new conditions. When solutions with 3000 μg/g Ca were analyzed, LOD improvements were smaller for FSApT and USN, but FSApT showed an improvement over USN of 6.5 times. Sensitivities compared to solutions without high dissolved solids were degraded by 19% on average for FSApT, while those for USN were degraded by 26%. The SI systems were also tested with a Varian Instruments Liberty 220 having a vacuum path Czerny-Turner monochromator and a 40 MHz generator. The sensitivities with low dissolved solids solutions compared to PN were 20 times better for the USN and 39 times better for FSApT, and LODs for every element were better for FSApT. Better correlation between relative sensitivities and anticipated relative analyte mass fluxes for FSApT and USN was observed with the Varian instrument. LOD improvements averaged 18 times lower than PN with FSApT while with USN values averaged 8 times lower. When solutions with high dissolved solids were studied it was found that FSApT still offered 5.5 times better LODs than PN and USN offered 4.6 times better LODs than PN. Sensitivities for FSApT averaged 20 times better, while those for USN were 13 times better compared to PN. Finally, background RSDs on the Varian system were generally higher for FSApT than for the USN for similar sample types. A third instrument used for a small set of elements was a Perkin-Elmer model 5500 ICP-AES. This system has a 27 MHz generator with a N 2 purged Czerny-Turner monochromator. LOD trends, background RSDs, and sensitivities were similar to those with the Leeman instrument. However, matrix effects more closely resembled those seen with the Varian instrument for both SI systems. To compare performance and recoveries on a real sample, a National Institute of Standards and Technology, Standard Reference Material 1643c trace elements in water, was analyzed using the Varian system and it was found that both SI systems offered similar recoveries.

Simple preparation of fluorescent composite films based on cerium and europium doped LaF3 nanoparticles

NASA Astrophysics Data System (ADS)

Secco, Henrique de L.; Ferreira, Fabio F.; Péres, Laura O.

2018-03-01

The combination of materials to form hybrids with unique properties, different from those of the isolated components, is a strategy used to prepare functional materials with improved properties aiming to allow their application in specific fields. The doping of lanthanum fluoride with other rare earth elements is used to obtain luminescent particles, which may be useful to the manufacturing of electronic devices' displays and biological markers, for instance. The application of the powder of nanoparticles has limitations in some fields; to overcome this, the powder may be incorporated in a suitable polymeric matrix. In this work, lanthanum fluoride nanoparticles, undoped and doped with cerium and europium, were synthesized through the co-precipitation method in aqueous solution. Aiming the formation of solid state films, composites of nanoparticles in an elastomeric matrix, the nitrile rubber (NBR), were prepared. The flexibility and the transparency of the matrix in the regions of interest are advantages for the application of the luminescent composites. The composites were applied as films using the casting and the spin coating techniques and luminescent materials were obtained in the samples doped with europium and cerium. Scanning electron microscopy images showed an adequate dispersion of the particles in the matrix in both film formation techniques. Aggregates of the particles were detected in the samples which may affect the uniformity of the emission of the composites.

Insights into the mechanism of the formation of the most stable crystal polymorph of milk fat in model protein matrices.

PubMed

Ramel, P R; Marangoni, A G

2017-09-01

The effect of incorporation and presence of various ingredients in a model sodium caseinate-based imitation cheese matrix on the polymorphism of milk fat was comprehensively described using powder x-ray diffraction, differential scanning calorimetry, and microscopy. With anhydrous milk fat (AMF) in bulk used as control, the embedding of AMF as droplets in a protein matrix was found to result in a greater extent of formation of the β polymorph than AMF alone and AMF homogenized with water and salts solution. The use of other protein matrices such as soy and whey protein isolate gels revealed that the nature of the protein and other factors associated with it (i.e., hydrophobicity and molecular structure) do not seem to play a role in the formation of the β polymorph. These results indicated that the most important factor in the formation of the β polymorph is the physical constraints imposed by a solid protein matrix, which forces the triacylglycerols in milk fat to arrange themselves in the most stable crystal polymorph. Characterization of the crystal structure of milk fat or fats in general within a food matrix could provide insights into the complex thermal and rheological behavior of foods with added fats. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Trace element analysis of extraterrestrial metal samples by inductively coupled plasma mass spectrometry: the standard solutions and digesting acids.

PubMed

Wang, Guiqin; Wu, Yangsiqian; Lin, Yangting

2016-02-28

Nearly 99% of the total content of extraterrestrial metals is composed of Fe and Ni, but with greatly variable trace element contents. The accuracy obtained in the inductively coupled plasma mass spectrometry (ICP-MS) analysis of solutions of these samples can be significantly influenced by matrix contents, polyatomic ion interference, and the concentrations of external standard solutions. An ICP-MS instrument (X Series 2) was used to determine 30 standard solutions with different concentrations of trace elements, and different matrix contents. Based on these measurements, the matrix effects were determined. Three iron meteorites were dissolved separately in aqua regia and HNO3. Deviations due to variation of matrix contents in the external standard solutions were evaluated and the analysis results of the two digestion methods for iron meteorites were assessed. Our results show obvious deviations due to unmatched matrix contents in the external standard solutions. Furthermore, discrepancy in the measurement of some elements was found between the sample solutions prepared with aqua regia and HNO3, due to loss of chloride during sample preparation and/or incomplete digestion of highly siderophile elements in iron meteorites. An accurate ICP-MS analysis method for extraterrestrial metal samples has been established using external standard solutions with matched matrix contents and digesting the samples with HNO3 and aqua regia. Using the data from this work, the Mundrabilla iron meteorite previously classified as IAB-ung is reclassified as IAB-MG. Copyright © 2016 John Wiley & Sons, Ltd.

Evaluation of a molecularly imprinted polymer for determination of steroids in goat milk by matrix solid phase dispersion.

PubMed

Gañán, Judith; Morante-Zarcero, Sonia; Gallego-Picó, Alejandrina; Garcinuño, Rosa María; Fernández-Hernando, Pilar; Sierra, Isabel

2014-08-01

A molecularly imprinted polymer-matrix solid-phase dispersion methodology for simultaneous determination of five steroids in goat milk samples was proposed. Factors affecting the extraction recovery such as sample/dispersant ratio and washing and elution solvents were investigated. The molecularly imprinted polymer used as dispersant in the matrix solid-phase dispersion procedure showed high affinity to steroids, and the obtained extracts were sufficiently cleaned to be directly analyzed. Analytical separation was performed by micellar electrokinetic chromatography using a capillary electrophoresis system equipped with a diode array detector. A background electrolyte composed of borate buffer (25mM, pH 9.3), sodium dodecyl sulfate (10mM) and acetonitrile (20%) was used. The developed MIP-MSPD methodology was applied for direct determination of testosterone (T), estrone (E1), 17β-estradiol (17β-E2), 17α-ethinylestradiol (EE2) and progesterone (P) in different goat milk samples. Mean recoveries obtained ranged from 81% to 110%, with relative standard deviations (RSD)≤12%. The molecularly imprinted polymer-matrix solid-phase dispersion method is fast, selective, cost-effective and environment-friendly compared with other pretreatment methods used for extraction of steroids in milk. Copyright © 2014 Elsevier B.V. All rights reserved.

Influence of topical anesthesia on tear dynamics and ocular drug bioavailability in albino rabbits.

PubMed

Patton, T F; Robinson, J R

1975-02-01

The bioavailability of topically applied ocular drugs is very poor, due largely to drug loss through drainage and tear turnover. The use of high viscosity solutions or solid matrixes to delay or eliminate drainage is the usual approach for decreasing drug loss but the alternative approach of chemically reducing tear turnover and/or solution drainage has not been investigated. By means of a simple isotopic dilution technique, using radioactive technetium sulfur colloid, the quantitative influence of topical anesthetics on tear production and instilled solution drainage was determined. The reduction in the rate of tear turnover and solution drainage varies for different anesthetics and is dose dependent. The implication of these results for some long accepted clinical procedures is discussed, and questions are raised regarding the present understanding of the mechanisms of tear production. Quantitation of precorneal drug loss through instilled solution drainage and tear turnover permits the establishment of a baseline for ocular drug bioavailability. Aqueous humor drug concentration versus time profiles of radioactive pilocarpine nitrate were obtained, both in the presence and absence of topical anesthesia. The results verify the importance of tear turnover and instilled solution drainage as a major route of drug loss in the eye. Moreover, the success of the present study in improving ocular drug bioavailability by the chemical approach of repressing solution drainage and tear turnover suggests that this approach is viable for improving drug bioavailability.

Uptake of perfluorinated compounds by plants grown in nutrient solution.

PubMed

García-Valcárcel, A I; Molero, E; Escorial, M C; Chueca, M C; Tadeo, J L

2014-02-15

The uptake rates of three perfluorinated carboxylates and three perfluorinated sufonates by a grass (B diandrus) grown in nutrient solution at two different perfluorinated compounds (PFCs) concentrations were assessed. Grass can be ingested by grazing animals causing the PFCs to enter the food chain, which is a pathway of human exposure to these compounds. A rapid and miniaturized method was developed to determine PFCs in plants, based on a matrix solid-phase dispersion (MSPD) extraction procedure followed by quantitation by HPLC-MS/MS with an MQL in the range from 1 to 9 ng/g. An increase of PFCs levels in plant was observed along the exposure time. Differences in uptake for studied perfluorinated carboxylates were found, showing a decrease with carbon chain length (from 3027 to 1,167 ng/g at the end of assay), whereas no significant differences in absorption were obtained between perfluorinated sulfonates (about 1,700 ng/g). Initially, higher PFC transfer factors (ratio between concentration in plant and concentration in initial nutrient solution) were obtained for plants growing in the nutrient solution at the highest PFC concentration, but these factors became similar with time to plants exposed to the lowest concentration. © 2013 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, J.; Hurtubise, R.J.

A new kind of solid matrix, glasses from sugars, was developed for trace organic analysis. Clear glasses of glucose and trehalose were prepared by evaporating the sugar solutions onto solid supports. It was determined that the ratio of methanol to water was very important in forming a clear glass. Also, glasses made from pure trehalose often cracked. However, with the addition of 8{endash}10{percent} NaCl to the trehalose, no cracks were formed. Clear and rigid glasses of both glucose and trehalose/NaCl were obtained on quartz plates. Strong room-temperature fluorescence (RTF) and room-temperature phosphorescence (RTP) were obtained from benzo[{ital f}]quinoline ({ital B}[{italmore » f}]{ital Q}), 4-phenylphenol (4-PP), B[{ital a}]P-{ital r}-7,{ital t}-8,9,{ital c}-10-tetrahydrotetrol (tetrol I-1), triphenylene, and phenanthrene. The limits of detection (LODs) of both the RTF and RTP for 4-PP and B[{ital f}]Q in the glasses were in the subnanogram/milligram range. {copyright} {ital 1996 Society for Applied Spectroscopy.}« less

Temperature dependent dielectric properties and ion transportation in solid polymer electrolyte for lithium ion batteries

NASA Astrophysics Data System (ADS)

Sengwa, R. J.; Dhatarwal, Priyanka; Choudhary, Shobhna

2016-05-01

Solid polymer electrolyte (SPE) film consisted of poly(ethylene oxide) (PEO) and poly(methyl methacrylate) (PMMA) blend matrix with lithium tetrafluroborate (LiBF4) as dopant ionic salt and poly(ethylene glycol) (PEG) as plasticizer has been prepared by solution casting method followed by melt pressing. Dielectric properties and ionic conductivity of the SPE film at different temperatures have been determined by dielectric relaxation spectroscopy. It has been observed that the dc ionic conductivity of the SPE film increases with increase of temperature and also the decrease of relaxation time. The temperature dependent relaxation time and ionic conductivity values of the electrolyte are governed by the Arrhenius relation. Correlation observed between dc conductivity and relaxation time confirms that ion transportation occurs with polymer chain segmental dynamics through hopping mechanism. The room temperature ionic conductivity is found to be 4 × 10-6 S cm-1 which suggests the suitability of the SPE film for rechargeable lithium batteries.

Temperature dependent dielectric properties and ion transportation in solid polymer electrolyte for lithium ion batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sengwa, R. J., E-mail: rjsengwa@rediffmail.com; Dhatarwal, Priyanka, E-mail: dhatarwalpriyanka@gmail.com; Choudhary, Shobhna, E-mail: shobhnachoudhary@rediffmail.com

2016-05-06

Solid polymer electrolyte (SPE) film consisted of poly(ethylene oxide) (PEO) and poly(methyl methacrylate) (PMMA) blend matrix with lithium tetrafluroborate (LiBF{sub 4}) as dopant ionic salt and poly(ethylene glycol) (PEG) as plasticizer has been prepared by solution casting method followed by melt pressing. Dielectric properties and ionic conductivity of the SPE film at different temperatures have been determined by dielectric relaxation spectroscopy. It has been observed that the dc ionic conductivity of the SPE film increases with increase of temperature and also the decrease of relaxation time. The temperature dependent relaxation time and ionic conductivity values of the electrolyte are governedmore » by the Arrhenius relation. Correlation observed between dc conductivity and relaxation time confirms that ion transportation occurs with polymer chain segmental dynamics through hopping mechanism. The room temperature ionic conductivity is found to be 4 × 10{sup −6} S cm{sup −1} which suggests the suitability of the SPE film for rechargeable lithium batteries.« less

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

PubMed

Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Coarsening in Solid-liquid Mixtures: Overview of Experiments on Shuttle and ISS

NASA Technical Reports Server (NTRS)

Duval, Walter M. B.; Hawersaat, Robert W.; Lorik, T.; Thompson, J.; Gulsoy, B.; Voorhees, P. W.

2013-01-01

The microgravity environment on the Shuttle and the International Space Station (ISS) provides the ideal condition to perform experiments on Coarsening in Solid-Liquid Mixtures (CSLM) as deleterious effects such as particle sedimentation and buoyancy-induced convection are suppressed. For an ideal system such as Lead-Tin in which all the thermophysical properties are known, the initial condition in microgravity of randomly dispersed particles with local clustering of solid Tin in eutectic liquid Lead-Tin matrix, permitted kinetic studies of competitive particle growth for a range of volume fractions. Verification that the quenching phase of the experiment had negligible effect of the spatial distribution of particles is shown through the computational solution of the dynamical equations of motion, thus insuring quench-free effects from the coarsened microstructure measurements. The low volume fraction experiments conducted on the Shuttle showed agreement with transient Ostwald ripening theory, and the steady-state requirement of LSW theory was not achieved. More recent experiments conducted on ISS with higher volume fractions have achieved steady-state condition and show that the kinetics follows the classical diffusion limited particle coarsening prediction and the measured 3D particle size distribution becomes broader as predicted from theory.

Solid-state voltammetry-based electrochemical immunosensor for Escherichia coli using graphene oxide-Ag nanoparticle composites as labels.

PubMed

Jiang, Xiaochun; Chen, Kun; Wang, Jing; Shao, Kang; Fu, Tao; Shao, Feng; Lu, Donglian; Liang, Jiangong; Foda, M Frahat; Han, Heyou

2013-06-21

A new electrochemical immunosensor based on solid-state voltammetry was fabricated for the detection of Escherichia coli (E. coli) by using graphene oxide-Ag nanoparticle composites (P-GO-Ag) as labels. To construct the platform, Au nanoparticles (AuNPs) were first self-assembled on an Au electrode surface through cysteamine and served as an effective matrix for antibody (Ab) attachment. Under a sandwich-type immunoassay format, the analyte and the probe (P-GO-Ag-Ab) were successively captured onto the immunosensor. Finally, the bonded AgNPs were detected through a solid-state redox process in 0.2 M of KCl solution. Combining the advantages of the high-loading capability of graphene oxide with promoted electron-transfer rate of AuNPs, this immunosensor produced a 26.92-fold signal enhancement compared with the unamplified protocol. Under the optimal conditions, the immunosensor exhibited a wide linear dependence on the logarithm of the concentration of E. coli ranging from 50 to 1.0 × 10(6) cfu mL(-1) with a detection limit of 10 cfu mL(-1). Moreover, as a practical application, the proposed immunosensor was used to monitor E. coli in lake water with satisfactory results.

Bottom-Up and Top-Down Solid-State NMR Approaches for Bacterial Biofilm Matrix Composition

PubMed Central

Cegelski, Lynette

2015-01-01

The genomics and proteomics revolutions have been enormously successful in providing crucial “parts lists” for biological systems. Yet, formidable challenges exist in generating complete descriptions of how the parts function and assemble into macromolecular complexes and whole-cell assemblies. Bacterial biofilms are complex multicellular bacterial communities protected by a slime-like extracellular matrix that confers protection to environmental stress and enhances resistance to antibiotics and host defenses. As a non-crystalline, insoluble, heterogeneous assembly, the biofilm extracellular matrix poses a challenge to compositional analysis by conventional methods. In this Perspective, bottom-up and top-down solid-state NMR approaches are described for defining chemical composition in complex macrosystems. The “sum-of-theparts” bottom-up approach was introduced to examine the amyloid-integrated biofilms formed by E. coli and permitted the first determination of the composition of the intact extracellular matrix from a bacterial biofilm. An alternative top-down approach was developed to define composition in V. cholerae biofilms and relied on an extensive panel of NMR measurements to tease out specific carbon pools from a single sample of the intact extracellular matrix. These two approaches are widely applicable to other heterogeneous assemblies. For bacterial biofilms, quantitative parameters of matrix composition are needed to understand how biofilms are assembled, to improve the development of biofilm inhibitors, and to dissect inhibitor modes of action. Solid-state NMR approaches will also be invaluable in obtaining parameters of matrix architecture. PMID:25797008

Bottom-up and top-down solid-state NMR approaches for bacterial biofilm matrix composition.

PubMed

Cegelski, Lynette

2015-04-01

The genomics and proteomics revolutions have been enormously successful in providing crucial "parts lists" for biological systems. Yet, formidable challenges exist in generating complete descriptions of how the parts function and assemble into macromolecular complexes and whole-cell assemblies. Bacterial biofilms are complex multicellular bacterial communities protected by a slime-like extracellular matrix that confers protection to environmental stress and enhances resistance to antibiotics and host defenses. As a non-crystalline, insoluble, heterogeneous assembly, the biofilm extracellular matrix poses a challenge to compositional analysis by conventional methods. In this perspective, bottom-up and top-down solid-state NMR approaches are described for defining chemical composition in complex macrosystems. The "sum-of-the-parts" bottom-up approach was introduced to examine the amyloid-integrated biofilms formed by Escherichia coli and permitted the first determination of the composition of the intact extracellular matrix from a bacterial biofilm. An alternative top-down approach was developed to define composition in Vibrio cholerae biofilms and relied on an extensive panel of NMR measurements to tease out specific carbon pools from a single sample of the intact extracellular matrix. These two approaches are widely applicable to other heterogeneous assemblies. For bacterial biofilms, quantitative parameters of matrix composition are needed to understand how biofilms are assembled, to improve the development of biofilm inhibitors, and to dissect inhibitor modes of action. Solid-state NMR approaches will also be invaluable in obtaining parameters of matrix architecture. Copyright © 2015 Elsevier Inc. All rights reserved.

Bottom-up and top-down solid-state NMR approaches for bacterial biofilm matrix composition

NASA Astrophysics Data System (ADS)

Cegelski, Lynette

2015-04-01

The genomics and proteomics revolutions have been enormously successful in providing crucial "parts lists" for biological systems. Yet, formidable challenges exist in generating complete descriptions of how the parts function and assemble into macromolecular complexes and whole-cell assemblies. Bacterial biofilms are complex multicellular bacterial communities protected by a slime-like extracellular matrix that confers protection to environmental stress and enhances resistance to antibiotics and host defenses. As a non-crystalline, insoluble, heterogeneous assembly, the biofilm extracellular matrix poses a challenge to compositional analysis by conventional methods. In this perspective, bottom-up and top-down solid-state NMR approaches are described for defining chemical composition in complex macrosystems. The "sum-of-the-parts" bottom-up approach was introduced to examine the amyloid-integrated biofilms formed by Escherichia coli and permitted the first determination of the composition of the intact extracellular matrix from a bacterial biofilm. An alternative top-down approach was developed to define composition in Vibrio cholerae biofilms and relied on an extensive panel of NMR measurements to tease out specific carbon pools from a single sample of the intact extracellular matrix. These two approaches are widely applicable to other heterogeneous assemblies. For bacterial biofilms, quantitative parameters of matrix composition are needed to understand how biofilms are assembled, to improve the development of biofilm inhibitors, and to dissect inhibitor modes of action. Solid-state NMR approaches will also be invaluable in obtaining parameters of matrix architecture.

Compliance matrices for cracked bodies

NASA Technical Reports Server (NTRS)

Ballarini, R.

1986-01-01

An algorithm is developed to construct the compliance matrix for a cracked solid in the integral-equation formulation of two-dimensional linear-elastic fracture mechanics. The integral equation is reduced to a system of algebraic equations for unknown values of the dislocation-density function at discrete points on the interval from -1 to 1, using the numerical procedure described by Gerasoulis (1982). Sample numerical results are presented, and it is suggested that the algorithm is especially useful in cases where iterative solutions are required; e.g., models of fiber-reinforced concrete, rocks, or ceramics where microcracking, fiber bridging, and other nonlinear effects are treated as nonlinear springs along the crack surfaces (Ballarini et al., 1984).

Design and preparation of polymeric scaffolds for tissue engineering.

PubMed

Weigel, Thomas; Schinkel, Gregor; Lendlein, Andreas

2006-11-01

Polymeric scaffolds for tissue engineering can be prepared with a multitude of different techniques. Many diverse approaches have recently been under development. The adaptation of conventional preparation methods, such as electrospinning, induced phase separation of polymer solutions or porogen leaching, which were developed originally for other research areas, are described. In addition, the utilization of novel fabrication techniques, such as rapid prototyping or solid free-form procedures, with their many different methods to generate or to embody scaffold structures or the usage of self-assembly systems that mimic the properties of the extracellular matrix are also described. These methods are reviewed and evaluated with specific regard to their utility in the area of tissue engineering.

Directionally solidified iron-base eutectic alloys

NASA Technical Reports Server (NTRS)

Tewari, S. N.

1976-01-01

Pseudobinary eutectic alloys with nominal compositions of Fe-25Ta-22Ni-10Cr and Fe-15.5Nb-14.5Ni-6.0Cr were directionally solidified at 0.5 centimeter per hour. Their microstructure consisted of the fcc, iron solid-solution, matrix phase reinforced by about 41-volume-percent, hcp, faceted Fe2Ta fibers and 41-volume-percent, hcp, Fe2Nb lamellae for the tantalum- and niobium-containing alloys, respectively. The microstructural stability under thermal cycling and the temperature dependence of tensile properties were investigated. These alloys showed low elevated-temperature strength and were not considered suitable for application in aircraft-gas-turbine blades although they may have applicability as vane materials.

A matrix equation solution by an optimization technique

NASA Technical Reports Server (NTRS)

Johnson, M. J.; Mittra, R.

1972-01-01

The computer solution of matrix equations is often difficult to accomplish due to an ill-conditioned matrix or high noise levels. Two methods of solution are compared for matrices of various degrees of ill-conditioning and for various noise levels in the right hand side vector. One method employs the usual Gaussian elimination. The other solves the equation by an optimization technique and employs a function minimization subroutine.

Single crystals of metal solid solutions

NASA Technical Reports Server (NTRS)

Miller, J. F.; Austin, A. E.; Richard, N.; Griesenauer, N. M.; Moak, D. P.; Mehrabian, M. R.; Gelles, S. H.

1974-01-01

The following definitions were sought in the research on single crystals of metal solid solutions: (1) the influence of convection and/or gravity present during crystallization on the substructure of a metal solid solution; (2) the influence of a magnetic field applied during crystallization on the substructure of a metal solid solution; and (3) requirements for a space flight experiment to verify the results. Growth conditions for the selected silver-zinc alloy system are described, along with pertinent technical and experimental details of the project.

Evaluation of the impact of matrix effect on quantification of pesticides in foods by gas chromatography-mass spectrometry using isotope-labeled internal standards.

PubMed

Yarita, Takashi; Aoyagi, Yoshie; Otake, Takamitsu

2015-05-29

The impact of the matrix effect in GC-MS quantification of pesticides in food using the corresponding isotope-labeled internal standards was evaluated. A spike-and-recovery study of nine target pesticides was first conducted using paste samples of corn, green soybean, carrot, and pumpkin. The observed analytical values using isotope-labeled internal standards were more accurate for most target pesticides than that obtained using the external calibration method, but were still biased from the spiked concentrations when a matrix-free calibration solution was used for calibration. The respective calibration curves for each target pesticide were also prepared using matrix-free calibration solutions and matrix-matched calibration solutions with blank soybean extract. The intensity ratio of the peaks of most target pesticides to that of the corresponding isotope-labeled internal standards was influenced by the presence of the matrix in the calibration solution; therefore, the observed slope varied. The ratio was also influenced by the type of injection method (splitless or on-column). These results indicated that matrix-matching of the calibration solution is required for very accurate quantification, even if isotope-labeled internal standards were used for calibration. Copyright © 2015 Elsevier B.V. All rights reserved.

Solid-state and solution /sup 13/C NMR in the conformational analysis of methadone-hydrochloride and related narcotic analgesics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sumner, S.C.J.

1986-01-01

Solid state and solution /sup 13/C NMR have been used to study the conformations of the racemic mixtures and single enantiomers of methadone hydrochloride, alpha and beta methadol hydrochloride, and alpha and beta acetylmethadol hydrochloride. The NMR spectra acquired for the compounds as solids, and in polar and nonpolar solvents are compared, in order to determine the conformation of the molecules in solution. To determine the reliability of assigning solution conformations by comparing solution and solid state chemical shift data, three bond coupling constants measured in solution are compared with those calculated from X-ray data. The conformations of the racemicmore » mixture and plus enantiomer of methadone hydrochloride have been shown to be very similar in the solid state, where minor differences in conformation can be seen by comparing NMR spectra obtained for the solids. Also shown is that the molecules of methadone hydrochloride have conformations in polar and in nonpolar solvents which are very similar to the conformation of the molecules in the solid state.« less

Engineering of layered, lipid-encapsulated drug nanoparticles through spray-drying.

PubMed

Sapra, Mahak; Mayya, Y S; Venkataraman, Chandra

2017-06-01

Drug-containing nanoparticles have been synthesized through the spray-drying of submicron droplet aerosols by using matrix materials such as lipids and biopolymers. Understanding layer formation in composite nanoparticles is essential for the appropriate engineering of particle substructures. The present study developed a droplet-shrinkage model for predicting the solid-phase formation of two non-volatile solutes-stearic acid lipid and a set of drugs, by considering molecular volume and solubility. Nanoparticle formation was simulated to define the parameter space of material properties and process conditions for the formation of a layered structure with the preferential accumulation of the lipid in the outer layer. Moreover, lipid-drug demarcation diagrams representing a set of critical values of ratios of solute properties at which the two solutes precipitate simultaneously were developed. The model was validated through the preparation of stearic acid-isoniazid nanoparticles under controlled processing conditions. The developed model can guide the selection of solvents, lipids, and processing conditions such that drug loading and lipid encapsulation in composite nanoparticles are optimized. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of solution treatment on stress corrosion cracking behavior of an as-forged Mg-Zn-Y-Zr alloy

PubMed Central

Wang, S. D.; Xu, D. K.; Wang, B. J.; Sheng, L. Y.; Han, E. H.; Dong, C.

2016-01-01

Effect of solid solution treatment (T4) on stress corrosion cracking (SCC) behavior of an as-forged Mg-6.7%Zn-1.3%Y-0.6%Zr (in wt.%) alloy has been investigated using slow strain rate tensile (SSRT) testing in 3.5 wt.% NaCl solution. The results demonstrated that the SCC susceptibility index (ISCC) of as-forged samples was 0.95 and its elongation-to-failure (εf) was only 1.1%. After T4 treatment, the SCC resistance was remarkably improved. The ISCC and εf values of T4 samples were 0.86 and 3.4%, respectively. Fractography and surface observation indicated that the stress corrosion cracking mode for as-forged samples was dominated by transgranular and partially intergranular morphology, whereas the cracking mode for T4 samples was transgranular. In both cases, the main cracking mechanism was associated with hydrogen embrittlement (HE). Through alleviating the corrosion attack of Mg matrix, the influence of HE on the SCC resistance of T4 samples can be greatly suppressed. PMID:27387817

Fundamental Flux Equations for Fracture-Matrix Interactions with Linear Diffusion

NASA Astrophysics Data System (ADS)

Oldenburg, C. M.; Zhou, Q.; Rutqvist, J.; Birkholzer, J. T.

2017-12-01

The conventional dual-continuum models are only applicable for late-time behavior of pressure propagation in fractured rock, while discrete-fracture-network models may explicitly deal with matrix blocks at high computational expense. To address these issues, we developed a unified-form diffusive flux equation for 1D isotropic (spheres, cylinders, slabs) and 2D/3D rectangular matrix blocks (squares, cubes, rectangles, and rectangular parallelepipeds) by partitioning the entire dimensionless-time domain (Zhou et al., 2017a, b). For each matrix block, this flux equation consists of the early-time solution up until a switch-over time after which the late-time solution is applied to create continuity from early to late time. The early-time solutions are based on three-term polynomial functions in terms of square root of dimensionless time, with the coefficients dependent on dimensionless area-to-volume ratio and aspect ratios for rectangular blocks. For the late-time solutions, one exponential term is needed for isotropic blocks, while a few additional exponential terms are needed for highly anisotropic blocks. The time-partitioning method was also used for calculating pressure/concentration/temperature distribution within a matrix block. The approximate solution contains an error-function solution for early times and an exponential solution for late times, with relative errors less than 0.003. These solutions form the kernel of multirate and multidimensional hydraulic, solute and thermal diffusion in fractured reservoirs.

Automated MALDI Matrix Coating System for Multiple Tissue Samples for Imaging Mass Spectrometry

NASA Astrophysics Data System (ADS)

Mounfield, William P.; Garrett, Timothy J.

2012-03-01

Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

Automated MALDI matrix coating system for multiple tissue samples for imaging mass spectrometry.

PubMed

Mounfield, William P; Garrett, Timothy J

2012-03-01

Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

Exact solution for four-order acousto-optic Bragg diffraction with arbitrary initial conditions.

PubMed

Pieper, Ron; Koslover, Deborah; Poon, Ting-Chung

2009-03-01

An exact solution to the four-order acousto-optic (AO) Bragg diffraction problem with arbitrary initial conditions compatible with exact Bragg angle incident light is developed. The solution, obtained by solving a 4th-order differential equation, is formalized into a transition matrix operator predicting diffracted light orders at the exit of the AO cell in terms of the same diffracted light orders at the entrance. It is shown that the transition matrix is unitary and that this unitary matrix condition is sufficient to guarantee energy conservation. A comparison of analytical solutions with numerical predictions validates the formalism. Although not directly related to the approach used to obtain the solution, it was discovered that all four generated eigenvalues from the four-order AO differential matrix operator are expressed simply in terms of Euclid's Divine Proportion.

The covariance matrix for the solution vector of an equality-constrained least-squares problem

NASA Technical Reports Server (NTRS)

Lawson, C. L.

1976-01-01

Methods are given for computing the covariance matrix for the solution vector of an equality-constrained least squares problem. The methods are matched to the solution algorithms given in the book, 'Solving Least Squares Problems.'

Thermodynamic Study of Solid-Liquid Equilibrium in NaCl-NaBr-H2O System at 288.15 K

NASA Astrophysics Data System (ADS)

Li, Dan; Meng, Ling-zong; Deng, Tian-long; Guo, Ya-fei; Fu, Qing-Tao

2018-06-01

The solubility data, composition of the solid solution and refractive indices of the NaCl-NaBr-H2O system at 288.15 K were studied with the isothermal equilibrium dissolution method. The solubility diagram and refractive index diagram of this system were plotted at 288.15 K. The solubility diagram consists of two crystallization zones for solid solution Na(Cl,Br) · 2H2O and Na(Cl,Br), one invariant points cosaturated with two solid solution and two univariant solubility isothermal curves. On the basis of Pitzer and Harvie-Weare (HW) chemical models, the composition equations and solubility equilibrium constant equations of the solid solutions at 288.15 K were acquired using the solubility data, the composition of solid solutions, and binary Pitzer parameters. The solubilities calculated using the new method combining the equations are in good agreement with the experimental data.

Electromagnetic energy coupling mechanism with matrix architecture control

NASA Technical Reports Server (NTRS)

Hughes, Eli (Inventor); Knowles, Gareth (Inventor)

2006-01-01

The present invention relates generally to reconfigurable, solid-state matrix arrays comprising multiple rows and columns of reconfigurable secondary mechanisms that are independently tuned. Specifically, the invention relates to reconfigurable devices comprising multiple, solid-state mechanisms characterized by at least one voltage-varied parameter disposed within a flexible, multi-laminate film, which are suitable for use as magnetic conductors, ground surfaces, antennas, varactors, ferrotunable substrates, or other active or passive electronic mechanisms.

Solid-perforated panel layout optimization by topology optimization based on unified transfer matrix.

PubMed

Kim, Yoon Jae; Kim, Yoon Young

2010-10-01

This paper presents a numerical method for the optimization of the sequencing of solid panels, perforated panels and air gaps and their respective thickness for maximizing sound transmission loss and/or absorption. For the optimization, a method based on the topology optimization formulation is proposed. It is difficult to employ only the commonly-used material interpolation technique because the involved layers exhibit fundamentally different acoustic behavior. Thus, an optimization method formulation using a so-called unified transfer matrix is newly proposed. The key idea is to form elements of the transfer matrix such that interpolated elements by the layer design variables can be those of air, perforated and solid panel layers. The problem related to the interpolation is addressed and bench mark-type problems such as sound transmission or absorption maximization problems are solved to check the efficiency of the developed method.

Nanocrystal/sol-gel nanocomposites

DOEpatents

Petruska, Melissa A [Los Alamos, NM; Klimov, Victor L [Los Alamos, NM

2007-06-05

The present invention is directed to solid composites including colloidal nanocrystals within a sol-gel host or matrix and to processes of forming such solid composites. The present invention is further directed to alcohol soluble colloidal nanocrystals useful in formation of sol-gel based solid composites.

Nanocrystal/sol-gel nanocomposites

DOEpatents

Petruska, Melissa A [Los Alamos, NM; Klimov, Victor L [Los Alamos, NM

2012-06-12

The present invention is directed to solid composites including colloidal nanocrystals within a sol-gel host or matrix and to processes of forming such solid composites. The present invention is further directed to alcohol soluble colloidal nanocrystals useful in formation of sol-gel based solid composites

Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

NASA Astrophysics Data System (ADS)

Menon, Sumithra Sivadas; Anitha, R.; Gupta, Bhavana; Baskar, K.; Singh, Shubra

2016-05-01

GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 ° C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.

Ion mobility and conductivity in the M{sub 0.5–x}Pb{sub x}Bi{sub 0.5}F{sub 2+x} (M=K, Rb) solid solutions with fluorite structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kavun, V. Ya., E-mail: kavun@ich.dvo.ru; Uvarov, N.F.; Slobodyuk, A.B.

Ionic mobility and conductivity in the K{sub 0.5–x}Pb{sub x}Bi{sub 0.5}F{sub 2+x} and Rb{sub 0.5–x}Pb{sub x}Bi{sub 0.5}F{sub 2+x} (x=0.05, 0.09) solid solutions with the fluorite structure have been investigated using the methods of {sup 19}F NMR, X-ray diffraction and impedance spectroscopy. Types of ionic motions in the fluoride sublattice of solid solutions have been established and temperature ranges of their realization have been determined (150–450 K). Diffusion of fluoride ions is a dominating type of ionic motions in the fluoride sublattice of solid solutions under study above 350 K. Due to high ionic conductivity, above 10{sup –3} S/cm at 450 K,more » these solid solutions can be used as solid electrolytes in various electrochemical devices and systems. - Graphical abstract: Temperature dependence of the concentration of mobile (2, 4) and immobile (1, 3) F ions in the K{sub 0.5–x}Pb{sub x}Bi{sub 0.5}F{sub 2+x} solid solutions. - Highlights: • Studied the ion mobility, conductivity in M{sub 0.5–x}Pb{sub x}Bi{sub 0.5}F{sub 2+x} solid solutions (M=K, Rb). • An analysis of {sup 19}F NMR spectra made it possible to identify types of ion mobility. • The main type of ion motion above 300 K in solid solutions is a diffusion of ions F{sup –}. • The ionic conductivity of the solid solutions studied more than 10{sup –3} S/cm at 450 K.« less

An added-mass partition algorithm for fluid–structure interactions of compressible fluids and nonlinear solids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Banks, J.W., E-mail: banksj3@rpi.edu; Henshaw, W.D., E-mail: henshw@rpi.edu; Kapila, A.K., E-mail: kapila@rpi.edu

We describe an added-mass partitioned (AMP) algorithm for solving fluid–structure interaction (FSI) problems involving inviscid compressible fluids interacting with nonlinear solids that undergo large rotations and displacements. The computational approach is a mixed Eulerian–Lagrangian scheme that makes use of deforming composite grids (DCG) to treat large changes in the geometry in an accurate, flexible, and robust manner. The current work extends the AMP algorithm developed in Banks et al. [1] for linearly elasticity to the case of nonlinear solids. To ensure stability for the case of light solids, the new AMP algorithm embeds an approximate solution of a nonlinear fluid–solidmore » Riemann (FSR) problem into the interface treatment. The solution to the FSR problem is derived and shown to be of a similar form to that derived for linear solids: the state on the interface being fundamentally an impedance-weighted average of the fluid and solid states. Numerical simulations demonstrate that the AMP algorithm is stable even for light solids when added-mass effects are large. The accuracy and stability of the AMP scheme is verified by comparison to an exact solution using the method of analytical solutions and to a semi-analytical solution that is obtained for a rotating solid disk immersed in a fluid. The scheme is applied to the simulation of a planar shock impacting a light elliptical-shaped solid, and comparisons are made between solutions of the FSI problem for a neo-Hookean solid, a linearly elastic solid, and a rigid solid. The ability of the approach to handle large deformations is demonstrated for a problem of a high-speed flow past a light, thin, and flexible solid beam.« less

Solid-phase reductive amination for glycomic analysis.

PubMed

Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

2017-04-15

Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

Fast acquisition of multidimensional NMR spectra of solids and mesophases using alternative sampling methods.

PubMed

Lesot, Philippe; Kazimierczuk, Krzysztof; Trébosc, Julien; Amoureux, Jean-Paul; Lafon, Olivier

2015-11-01

Unique information about the atom-level structure and dynamics of solids and mesophases can be obtained by the use of multidimensional nuclear magnetic resonance (NMR) experiments. Nevertheless, the acquisition of these experiments often requires long acquisition times. We review here alternative sampling methods, which have been proposed to circumvent this issue in the case of solids and mesophases. Compared to the spectra of solutions, those of solids and mesophases present some specificities because they usually display lower signal-to-noise ratios, non-Lorentzian line shapes, lower spectral resolutions and wider spectral widths. We highlight herein the advantages and limitations of these alternative sampling methods. A first route to accelerate the acquisition time of multidimensional NMR spectra consists in the use of sparse sampling schemes, such as truncated, radial or random sampling ones. These sparsely sampled datasets are generally processed by reconstruction methods differing from the Discrete Fourier Transform (DFT). A host of non-DFT methods have been applied for solids and mesophases, including the G-matrix Fourier transform, the linear least-square procedures, the covariance transform, the maximum entropy and the compressed sensing. A second class of alternative sampling consists in departing from the Jeener paradigm for multidimensional NMR experiments. These non-Jeener methods include Hadamard spectroscopy as well as spatial or orientational encoding of the evolution frequencies. The increasing number of high field NMR magnets and the development of techniques to enhance NMR sensitivity will contribute to widen the use of these alternative sampling methods for the study of solids and mesophases in the coming years. Copyright © 2015 John Wiley & Sons, Ltd.

Investigation of compositional segregation during unidirectional solidification of solid solution semiconducting alloys

NASA Technical Reports Server (NTRS)

Wang, J. C.

1982-01-01

Compositional segregation of solid solution semiconducting alloys in the radial direction during unidirectional solidification was investigated by calculating the effect of a curved solid liquid interface on solute concentration at the interface on the solid. The formulation is similar to that given by Coriell, Boisvert, Rehm, and Sekerka except that a more realistic cylindrical coordinate system which is moving with the interface is used. Analytical results were obtained for very small and very large values of beta with beta = VR/D, where V is the velocity of solidification, R the radius of the specimen, and D the diffusivity of solute in the liquid. For both very small and very large beta, the solute concentration at the interface in the solid C(si) approaches C(o) (original solute concentration) i.e., the deviation is minimal. The maximum deviation of C(si) from C(o) occurs for some intermediate value of beta.

Ultrasound stimulated release of mimosa medicine from cellulose hydrogel matrix.

PubMed

Jiang, Huixin; Tovar-Carrillo, Karla; Kobayashi, Takaomi

2016-09-01

Ultrasound (US) drug release system using cellulose based hydrogel films was developed as triggered to mimosa. Here, the mimosa, a fascinating drug to cure injured skin, was employed as the loading drug in cellulose hydrogel films prepared with phase inversion method. The mimosa hydrogels were fabricated from dimethylacetamide (DMAc)/LiCl solution in the presence of mimosa, when the solution was exposed to ethanol vapor. The US triggered release of the mimosa from the hydrogel matrix was carried out under following conditions of US powers (0-30W) and frequencies (23, 43 and 96kHz) for different mimosa hydrogel matrix from 0.5wt% to 2wt% cellulose solution. To release the drug by US trigger from the matrix, the better medicine release was observed in the matrix prepared from the 0.5wt% cellulose solution when the 43kHz US was exposed to the aqueous solution with the hydrogel matrix. The release efficiency increased with the increase of the US power from 5 to 30W at 43kHz. Viscoelasticity of the hydrogel matrix showed that the hydrogel became somewhat rigid after the US exposure. FT-IR analysis of the mimosa hydrogel matrixes showed that during the US exposure, hydrogen bonds in the structure of mimosa-water and mimosa-cellulose were broken. This suggested that the enhancement of the mimosa release was caused by the US exposure. Copyright © 2016 Elsevier B.V. All rights reserved.

Process for recovering chaotropic anions from an aqueous solution also containing other ions

DOEpatents

Rogers, Robin; Horwitz, E. Philip; Bond, Andrew H.

1999-01-01

A solid/liquid process for the separation and recovery of chaotropic anions from an aqueous solution is disclosed. The solid support comprises separation particles having surface-bonded poly(ethylene glycol) groups, whereas the aqueous solution from which the chaotropic anions are separated contains a poly(ethylene glycol) liquid/liquid biphase-forming amount of a dissolved salt (lyotrope). A solid/liquid phase admixture of separation particles containing bound chaotropic anions in such an aqueous solution is also contemplated, as is a chromatography apparatus containing that solid/liquid phase admixture.

Process for recovering chaotropic anions from an aqueous solution also containing other ions

DOEpatents

Rogers, R.; Horwitz, E.P.; Bond, A.H.

1999-03-30

A solid/liquid process for the separation and recovery of chaotropic anions from an aqueous solution is disclosed. The solid support comprises separation particles having surface-bonded poly(ethylene glycol) groups, whereas the aqueous solution from which the chaotropic anions are separated contains a poly(ethylene glycol) liquid/liquid biphase-forming amount of a dissolved salt (lyotrope). A solid/liquid phase admixture of separation particles containing bound chaotropic anions in such an aqueous solution is also contemplated, as is a chromatography apparatus containing that solid/liquid phase admixture. 19 figs.

Role of lattice distortion on diffuse phase transition temperatures in Bi0.5Na0.5TiO3-BaTiO3 [BNBTO] solid solutions

NASA Astrophysics Data System (ADS)

Pradhan, Lagen Kumar; Pandey, Rabichandra; Kumar, Sunil; Supriya, Sweety; Kar, Manoranjan

2018-04-01

Effect of lattice distortion on diffuse phase transition in BNBTO solid solutions near Morphotropic phase boundary (MPB) has been investigated. Solid solutions of (Bi0.5Na0.5)1-xBaxTiO3 (with mole % of x= 0.04, 0.05, 0.06, 0.07 and 0.08) were prepared by the planetary ball mill method in ethanol medium. Rietveld refinement technique with rhombohedral (R3c) and tetragonal (P4bm) crystal symmetry has been employed for structural as well as phase analysis of the solid solutions. Both rhombohedral and tetragonal lattice distortion (c/a) tends toward the pseudo-cubic crystal symmetry with the increase of mole fraction of Ba2+ near MPB (x= 6 mole %). Also, the average crystallite size and grain size decrease with increase of mole fraction of Ba2+ in BNT ceramic are due to larger ionic radius of Ba2+ and grain boundary pinning process in the solid solutions respectively. Additionally, depolarization temperature (Td) and maximum temperature (Tm) reduces due to the lattice distortion of both the phases in BNBTO solid solutions, which is explained extensively. Significant increase of dielectric constant has been observed near MPB composition (x=6%) in BNBTO solid solutions.

A nonequilibrium model for reactive contaminant transport through fractured porous media: Model development and semianalytical solution

NASA Astrophysics Data System (ADS)

Joshi, Nitin; Ojha, C. S. P.; Sharma, P. K.

2012-10-01

In this study a conceptual model that accounts for the effects of nonequilibrium contaminant transport in a fractured porous media is developed. Present model accounts for both physical and sorption nonequilibrium. Analytical solution was developed using the Laplace transform technique, which was then numerically inverted to obtain solute concentration in the fracture matrix system. The semianalytical solution developed here can incorporate both semi-infinite and finite fracture matrix extent. In addition, the model can account for flexible boundary conditions and nonzero initial condition in the fracture matrix system. The present semianalytical solution was validated against the existing analytical solutions for the fracture matrix system. In order to differentiate between various sorption/transport mechanism different cases of sorption and mass transfer were analyzed by comparing the breakthrough curves and temporal moments. It was found that significant differences in the signature of sorption and mass transfer exists. Applicability of the developed model was evaluated by simulating the published experimental data of Calcium and Strontium transport in a single fracture. The present model simulated the experimental data reasonably well in comparison to the model based on equilibrium sorption assumption in fracture matrix system, and multi rate mass transfer model.

Preparation of Sic/AIN Solid Solutions Using Organometallic Precursors

DTIC Science & Technology

1989-02-15

pyrolysis of organoaluminum and organosilicon compounds was investigated as a potential source of SiC /AUI solid solutions. Using two different co... pyrolysis methods, homogeneous mixtures of organoaluminum amides and both a vinylic polysilane and a poly- carbosilane were convertec to a preceramic ...solid that transformed to crystalline SiC /AiN solid solutions at 򒸀 C. Moreover, the liquid, polymeric , form of these precursor mixtures provides a

Improving tissue preparation for matrix-assisted laser desorption ionization mass spectrometry imaging. Part 1: using microspotting.

PubMed

Franck, Julien; Arafah, Karim; Barnes, Alan; Wisztorski, Maxence; Salzet, Michel; Fournier, Isabelle

2009-10-01

Nowadays, matrix-assisted laser desorption ionization mass spectrometry imaging (MALDI MSI) is a powerful technique to obtain the distribution of endogenous and exogenous molecules within tissue sections. It can, thus, be used to study the evolution of molecules across different physiological stages in order to find out markers or get knowledge on signaling pathways. In order to provide valuable information, we must carefully control the sample preparation to avoid any delocalization of molecules of interest inside the tissue during this step. Currently, two strategies can be used to deposit chemicals, such as the MALDI matrix, onto the tissue both involving generation of microdroplets that will be dropped off onto the surface. First strategy involves microspraying of solutions. Here, we have been interested in the development of a microspotting strategy, where nanodroplets of solvent are ejected by a piezoelectric device to generate microspots at the tissue level. Such systems allow one to precisely control sample preparation by creating an array of spots. In terms of matrix crystallization, a microspotting MALDI matrix is hardly compatible with the results by classical (pipetting) methods. We have thus synthesized and studied new solid ionic matrixes in order to obtain high analytical performance using such a deposition system. These developments have enabled optimization of the preparation time because of the high stability of the printing that is generated in these conditions. We have also studied microspotting for performing on-tissue digestion in order to go for identification of proteins or to work from formalin fixed and paraffin embedded (FFPE) tissue samples. We have shown that microspotting is an interesting approach for on tissue digestion. Peptides, proteins, and lipids were studied under this specific preparation strategy to improve imaging performances for this class of molecules.

Coloring, bleaching, and perming: influence on EtG content in hair.

PubMed

Kerekes, Isabelle; Yegles, Michel

2013-08-01

Hair analysis of ethyl glucuronide (EtG) has become, beside fatty acid ethyl ester, a valuable marker for the detection of moderate and chronic excessive alcohol consumption. So far, only few studies exist about the influence of cosmetic treatment on EtG content in hair. The aim of this study was to evaluate the effect of coloring, bleaching, and perming on the concentration of this alcohol marker in hair. Studies were also performed to evaluate the chemical stability of EtG in the presence of hydrogen peroxide and ammonium thioglycolate. Six air samples were treated in vitro by the different commercial cosmetics following the suppliers' instructions. After washing, pulverization, incubation in ultrasonic bath, and solid phase extraction, EtG was determined by GC/MS-NICI after solid phase extraction and heptafluorobutyric anhydride derivatization. The results showed that samples (n = 10) treated with the coloring product did not show any important change in the EtG results. In the bleaching study (n = 23), a mean decrease of 73.5% was observed. After incubation of a solution of EtG with hydrogen peroxide (15%), a decrease of 45% was shown supporting the hypothesis of a chemical degradation of EtG and a leaching out effect from the hair matrix. In the perm treatment study (n = 23), a mean decrease of 95.7% of EtG was found. Incubation of a solution of EtG with ammonium thioglycolate (5%) showed a total decrease of EtG supporting the hypothesis of a chemical degradation. Coloring treatment did not importantly influence EtG content in hair. However, an important decrease of EtG in hair could be found after bleaching and permanent wave treatment. This decrease seems to be because of a chemical degradation of EtG, after bleaching, and a leaching out effect from the matrix. After perming, it seems to be more of a chemical degradation of EtG. These data have to be considered for the correct interpretation of EtG amounts in hair.

Room-temperature ferromagnetic transitions and the temperature dependence of magnetic behaviors in FeCoNiCr-based high-entropy alloys

NASA Astrophysics Data System (ADS)

Na, Suok-Min; Yoo, Jin-Hyeong; Lambert, Paul K.; Jones, Nicholas J.

2018-05-01

High-entropy alloys (HEAs) containing multiple principle alloying elements exhibit unique properties so they are currently receiving great attention for developing innovative alloy designs. In FeCoNi-based HEAs, magnetic behaviors strongly depend on the addition of alloying elements, usually accompanied by structural changes. In this work, the effect of non-magnetic components on the ferromagnetic transition and magnetic behaviors in equiatomic FeCoNiCrX (X=Al, Ga, Mn and Sn) HEAs was investigated. Alloy ingots of nominal compositions of HEAs were prepared by arc melting and the button ingots were cut into discs for magnetic measurements as functions of magnetic field and temperature. The HEAs of FeCoNiCrMn and FeCoNiCrSn show typical paramagnetic behaviors, composed of solid solution FCC matrix, while the additions of Ga and Al in FeCoNiCr exhibit ferromagnetic behaviors, along with the coexistence of FCC and BCC phases due to spinodal decomposition. The partial phase transition in both HEAs with the additions of Ga and Al would enhance ferromagnetic properties due to the addition of the BCC phase. The saturation magnetization for the base alloy FeCoNiCr is 0.5 emu/g at the applied field of 20 kOe (TC = 104 K). For the HEAs of FeCoNiCrGa and FeCoNiCrAl, the saturation magnetization significantly increased to 38 emu/g (TC = 703 K) and 25 emu/g (TC = 277 K), respectively. To evaluate the possibility of solid solution FCC and BCC phases in FeCoNiCr-type HEAs, we introduced a parameter of valence electron concentration (VEC). The proposed rule for solid solution formation by the VEC was matched with FeCoNiCr-type HEAs.

Multifunctional Au NPs-polydopamine-polyvinylidene fluoride membrane chips as probe for enrichment and rapid detection of organic contaminants.

PubMed

Wang, Saihua; Niu, Hongyun; Cai, Yaqi; Cao, Dong

2018-05-01

High-throughput and rapid detection of hazardous compounds in complicated samples is essential for the solution of environmental problems. We have prepared a "pH-paper-like" chip which can rapidly "indicate" the occurrence of organic contaminants just through dipping the chip in water samples for short time followed by fast analysis with surface-assisted laser desorption/ionization time-of-flight mass spectrometry (SALDI-TOF MS). The chips are composed of polyvinylidene fluoride membrane (PVDFM), polydopamine (PDA) film and Au nanoparticles (Au NPs), which are layer-by-layer assembled according to the adhesion, self-polymerization and reduction property of dopamine. In the Au NPs loaded polydopamine-polyvinylidene fluoride membrane (Au NPs-PDA-PVDFM) chips, PVDFM combined with PDA film are responsible for the enrichment of organic analyte through hydrophobic interactions and π-π stacking; Au NPs serve as effective SALDI matrix for the rapid detection of target analyte. After dipping into water solution for minutes, the Au-PDA-PVDFM chips with enriched organic analytes can be detected directly with SALDI-TOF MS. The good solid-phase extraction performance of the PDA-PVDFM components, remarkable matrix effect of the loaded AuNPs, and sensitivity of the SALDI-TOF MS technique ensure excellent sensitivity and reproducibility for the quantification of trace levels of organic contaminants in environmental water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Atom probe tomographic studies of precipitation in Al-0.1Zr-0.1Ti (at.%) alloys.

PubMed

Knipling, Keith E; Dunand, David C; Seidman, David N

2007-12-01

Atom probe tomography was utilized to measure directly the chemical compositions of Al(3)(Zr(1)-(x)Ti(x)) precipitates with a metastable L1(2) structure formed in Al-0.1Zr-0.1Ti (at.%) alloys upon aging at 375 degrees C or 425 degrees C. The alloys exhibit an inhomogeneous distribution of Al(3)(Zr(1)-(x)Ti(x)) precipitates, as a result of a nonuniform dendritic distribution of solute atoms after casting. At these aging temperatures, the Zr:Ti atomic ratio in the precipitates is about 10 and 5, respectively, indicating that Ti remains mainly in solid solution rather than partitioning to the Al(3)(Zr(1)-(x)Ti(x)) precipitates. This is interpreted as being due to the very small diffusivity of Ti in alpha-Al, consistent with prior studies on Al-Sc-Ti and Al-Sc-Zr alloys, where the slower diffusing Zr and Ti atoms make up a small fraction of the Al(3)(Zr(1)-(x)Ti(x)) precipitates. Unlike those alloys, however, the present Al-Zr-Ti alloys exhibit no interfacial segregation of Ti at the matrix/precipitate heterophase interface, a result that may be affected by a significant disparity in the evaporation fields of the alpha-Al matrix and Al(3)(Zr(1)-(x)Ti(x)) precipitates and/or a lack of local thermodynamic equilibrium at the interface.

Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

2016-12-01

The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

Polar decomposition for attitude determination from vector observations

NASA Technical Reports Server (NTRS)

Bar-Itzhack, Itzhack Y.

1993-01-01

This work treats the problem of weighted least squares fitting of a 3D Euclidean-coordinate transformation matrix to a set of unit vectors measured in the reference and transformed coordinates. A closed-form analytic solution to the problem is re-derived. The fact that the solution is the closest orthogonal matrix to some matrix defined on the measured vectors and their weights is clearly demonstrated. Several known algorithms for computing the analytic closed form solution are considered. An algorithm is discussed which is based on the polar decomposition of matrices into the closest unitary matrix to the decomposed matrix and a Hermitian matrix. A somewhat longer improved algorithm is suggested too. A comparison of several algorithms is carried out using simulated data as well as real data from the Upper Atmosphere Research Satellite. The comparison is based on accuracy and time consumption. It is concluded that the algorithms based on polar decomposition yield a simple although somewhat less accurate solution. The precision of the latter algorithms increase with the number of the measured vectors and with the accuracy of their measurement.

Active subspace: toward scalable low-rank learning.

PubMed

Liu, Guangcan; Yan, Shuicheng

2012-12-01

We address the scalability issues in low-rank matrix learning problems. Usually these problems resort to solving nuclear norm regularized optimization problems (NNROPs), which often suffer from high computational complexities if based on existing solvers, especially in large-scale settings. Based on the fact that the optimal solution matrix to an NNROP is often low rank, we revisit the classic mechanism of low-rank matrix factorization, based on which we present an active subspace algorithm for efficiently solving NNROPs by transforming large-scale NNROPs into small-scale problems. The transformation is achieved by factorizing the large solution matrix into the product of a small orthonormal matrix (active subspace) and another small matrix. Although such a transformation generally leads to nonconvex problems, we show that a suboptimal solution can be found by the augmented Lagrange alternating direction method. For the robust PCA (RPCA) (Candès, Li, Ma, & Wright, 2009 ) problem, a typical example of NNROPs, theoretical results verify the suboptimality of the solution produced by our algorithm. For the general NNROPs, we empirically show that our algorithm significantly reduces the computational complexity without loss of optimality.

New algorithms to compute the nearness symmetric solution of the matrix equation.

PubMed

Peng, Zhen-Yun; Fang, Yang-Zhi; Xiao, Xian-Wei; Du, Dan-Dan

2016-01-01

In this paper we consider the nearness symmetric solution of the matrix equation AXB = C to a given matrix [Formula: see text] in the sense of the Frobenius norm. By discussing equivalent form of the considered problem, we derive some necessary and sufficient conditions for the matrix [Formula: see text] is a solution of the considered problem. Based on the idea of the alternating variable minimization with multiplier method, we propose two iterative methods to compute the solution of the considered problem, and analyze the global convergence results of the proposed algorithms. Numerical results illustrate the proposed methods are more effective than the existing two methods proposed in Peng et al. (Appl Math Comput 160:763-777, 2005) and Peng (Int J Comput Math 87: 1820-1830, 2010).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rai, R.N., E-mail: rn_rai@yahoo.co.in; Kant, Shiva; Reddi, R.S.B.

Urea is an attractive material for frequency conversion of high power lasers to UV (for wavelength down to 190 nm), but its usage is hindered due to its hygroscopic nature, though there is no alternative organic NLO crystal which could be transparent up to 190 nm. The hygroscopic character of urea has been modified by making the solid solution (UCNB) of urea (U) and p-chloronitrobenzene (CNB). The formation of the solid solution of CNB in U is explained on the basis of phase diagram, powder XRD, FTIR, elemental analysis and single crystal XRD studies. The solubility of U, CNB andmore » UCNB in ethanol solution is evaluated at different temperatures. Transparent single crystals of UCNB are grown from its saturated solution in ethanol. Optical properties e.g., second harmonic generation (SHG), refractive index and the band gap for UCNB crystal were measured and their values were compared with the parent compounds. Besides modification in hygroscopic nature, UCNB has also shown the higher SHG signal and mechanical hardness in comparison to urea crystal. - Highlights: • The hygroscopic character of urea was modified by making the solid solution • Solid solution formation is support by elemental, powder- and single crystal XRD • Crystal of solid solution has higher SHG signal and mechanical stability. • Refractive index and band gap of solid solution crystal have determined.« less

Dissolution of aragonite-strontianite solid solutions in nonstoichiometric Sr (HCO3)2-Ca (HCO3)2-CO2-H2O solutions

USGS Publications Warehouse

Plummer, Niel; Busenberg, E.; Glynn, P.D.; Blum, A.E.

1992-01-01

Synthetic strontianite-aragonite solid-solution minerals were dissolved in CO2-saturated non-stoichiometric solutions of Sr(HCO3)2 and Ca(HCO3)2 at 25??C. The results show that none of the dissolution reactions reach thermodynamic equilibrium. Congruent dissolution in Ca(HCO3)2 solutions either attains or closely approaches stoichiometric saturation with respect to the dissolving solid. In Sr(HCO3)2 solutions the reactions usually become incongruent, precipitating a Sr-rich phase before reaching stoichiometric saturation. Dissolution of mechanical mixtures of solids approaches stoichiometric saturation with respect to the least stable solid in the mixture. Surface uptake from subsaturated bulk solutions was observed in the initial minutes of dissolution. This surficial phase is 0-10 atomic layers thick in Sr(HCO3)2 solutions and 0-4 layers thick in Ca(HCO3)2 solutions, and subsequently dissolves and/or recrystallizes, usually within 6 min of reaction. The initial transient surface precipitation (recrystallization) process is followed by congruent dissolution of the original solid which proceeds to stoichiometric saturation, or until the precipitation of a more stable Sr-rich solid. The compositions of secondary precipitates do not correspond to thermodynamic equilibrium or stoichiometric saturation states. X-ray photoelectron spectroscopy (XPS) measurements indicate the formation of solid solutions on surfaces of aragonite and strontianite single crystals immersed in Sr(HCO3)2 and Ca(HCO3)2 solutions, respectively. In Sr(HCO3)2 solutions, the XPS signal from the outer ~ 60 A?? on aragonite indicates a composition of 16 mol% SrCO3 after only 2 min of contact, and 14-18 mol% SrCO3 after 3 weeks of contact. The strontianite surface averages approximately 22 mol% CaCO3 after 2 min of contact with Ca(HCO3)2 solution, and is 34-39 mol% CaCO3 after 3 weeks of contact. XPS analysis suggests the surface composition is zoned with somewhat greater enrichment in the outer ~25 A?? (as much as 26 mol% SrCO3 on aragonite and 44 mol% CaCO3 on strontianite). The results indicate rapid formation of a solid-solution surface phase from subsaturated aqueous solutions. The surface phase continually adjusts in composition in response to changes in composition of the bulk fluid as net dissolution proceeds. Dissolution rates of the endmembers are greatly reduced in nonstoichiometric solutions relative to dissolution rates observed in stoichiometric solutions. All solids dissolve more slowly in solutions spiked with the least soluble component ((Sr(HCO3)2)) than in solutions spiked with the more soluble component (Ca(HCO3)2), an effect that becomes increasingly significant as stoichiometric saturation is approached. It is proposed that the formation of a non-stoichiometric surface reactive zone significantly decreases dissolution rates. ?? 1992.

Influence of formulation technique on acrylate methacrylate copolymer modified paracetamol matrix tablets.

PubMed

Cash-Torunarigha, Omonyemen Edoise; Eichie, Florence Egbomonjiade; Arhewoh, Matthew Ikhuoria

2015-03-01

This work was designed to evaluate the influence of various methods such as dry granulation (DG), wet granulation (using the polymer in an ethanolic solution (WGO) or aqueous dispersion (WGA) and solid dispersion (SD) techniques, on properties of paracetamol matrix tablets prepared using varying concentrations of acrylate methacrylate copolymer. Tablet properties were investigated using official and unofficial standards. Drug dissolution profile assessed at pH 1.2 was studied spectrophotometrically at λ(max) of 245 nm. With the use of various kinetic models, the release mechanism of the drug was analyzed. The parameters, maximum amount of drug release (m(∞)) at time t(∞) were obtained, m(∞) was ≥ 91.36 %, while t(∞) was ≥ 4.5 h. The release rate constant (k) for DG tablets was 15.61 h(sup>-1(/sup>, while, WGO, WGA and SD tablets were 12.90, 11.03 and 10.75 h(-1) respectively. The matrix tablets, which exhibited marked retardation in drug release displayed a Higuchi square root of time model (R(2) > 0.98). The mechanism through which the drug was released was governed by Fickian diffusion release (n values < 0.5). The performance of the drug was affected by the formulation technique in the order of SD > WGO > WGA > DG.

Precipitation in Al–Mg solid solution prepared by solidification under high pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jie, J.C., E-mail: jiejc@dlut.edu.cn; School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001; Wang, H.W.

2014-01-15

The precipitation in Al–Mg solid solution containing 21.6 at.% Mg prepared by solidification under 2 GPa was investigated. The results show that the γ-Al{sub 12}Mg{sub 17} phase is formed and the β′ phase cannot be observed in the solid solution during ageing process. The precipitation of γ and β phases takes place in a non-uniform manner during heating process, i.e. the γ and β phases are first formed in the interdendritic region, which is caused by the inhomogeneous distribution of Mg atoms in the solid solution solidified under high pressure. Peak splitting of X-ray diffraction patterns of Al(Mg) solid solutionmore » appears, and then disappears when the samples are aged at 423 K for different times, due to the non-uniform precipitation in Al–Mg solid solution. The direct transformation from the γ to β phase is observed after ageing at 423 K for 24 h. It is considered that the β phase is formed through a peritectoid reaction of α + γ → β which needs the diffusion of Mg atoms across the interface of α/γ phases. - Highlights: • The γ phase is formed and the β′ phase is be observed in Al(Mg) solid solution. • Peak splitting of XRD pattern of Al(Mg) solid solution appears during aged at 150 °C. • The β phase is formed through a peritectoid reaction of α + γ → β.« less

Enhanced photocatalytic degradation of 2-propanol over macroporous GaN/ZnO solid solution prepared by a novel sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Lizhong; Ouyang, Shuxin; Ren, Bofan

2015-10-01

Macroporous GaN/ZnO solid solution photocatalyst is synthesized through a novel sol-gel method under mild conditions. The performance of as-synthesized solid solution photocatalyst is evaluated for decomposition of gaseous 2-propanol (IPA). It is found that due to enhancement in both the adsorption to gaseous IPA and the absorbance to visible light, the porous GaN/ZnO solid solution exhibits a good photocatalytic performance for IPA decomposition. Moreover, the mechanism for photocatalytic degradation IPA over porous GaN/ZnO solid solution is also investigated in comparison with those for the two end materials ZnO and GaN. The trapping effects with different scavengers prove that both themore » photoexcited electrons and holes affect the IPA photodegradation process, simultaneously.« less

Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Menon, Sumithra Sivadas; Anitha, R.; Baskar, K.

2016-05-23

GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 °more » C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.« less

Solid State Research.

DTIC Science & Technology

1982-11-15

Optics Y-Junction and Mach-Zehnder Interferometric Modulator Using Four -Port Scattering Matrix 7 1.3 Heterodyne and Direct Detection at 10 om with High...and of the Mach-Zehnder interferometric modulator have been analyzed using the four -port scattering i- matrix. The interferometric properties of the Y...USING FOUR -PORT SCATTERING MATRIX The scattering matrix formalism for a lossless four -port device has been used to describe the performance of the

Acoustooptic linear algebra processors - Architectures, algorithms, and applications

NASA Technical Reports Server (NTRS)

Casasent, D.

1984-01-01

Architectures, algorithms, and applications for systolic processors are described with attention to the realization of parallel algorithms on various optical systolic array processors. Systolic processors for matrices with special structure and matrices of general structure, and the realization of matrix-vector, matrix-matrix, and triple-matrix products and such architectures are described. Parallel algorithms for direct and indirect solutions to systems of linear algebraic equations and their implementation on optical systolic processors are detailed with attention to the pipelining and flow of data and operations. Parallel algorithms and their optical realization for LU and QR matrix decomposition are specifically detailed. These represent the fundamental operations necessary in the implementation of least squares, eigenvalue, and SVD solutions. Specific applications (e.g., the solution of partial differential equations, adaptive noise cancellation, and optimal control) are described to typify the use of matrix processors in modern advanced signal processing.

One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion.

PubMed

Tu, Xijuan; Ma, Shuangqin; Gao, Zhaosheng; Wang, Jing; Huang, Shaokang; Chen, Wenbin

2017-11-01

Flavonoids are frequently found as glycosylated derivatives in plant materials. To determine contents of flavonoid aglycones in these matrices, procedures for the extraction and hydrolysis of flavonoid glycosides are required. The current sample preparation method is both labour and time consuming. Develop a modified matrix solid phase dispersion (MSPD) procedure as an alternative methodology for the one-step extraction and hydrolysis of flavonoid glycosides. HPLC-DAD was applied for demonstrating the one-step extraction and hydrolysis of flavonoids in rape bee pollen. The obtained contents of flavonoid aglycones (quercetin, kaempferol, isorhamnetin) were used for the optimisation and validation of the method. The extraction and hydrolysis were accomplished in one step. The procedure completes in 2 h with silica gel as dispersant, a 1:2 ratio of sample to dispersant, and 60% aqueous ethanol with 0.3 M hydrochloric acid as the extraction solution. The relative standard deviations (RSDs) of repeatability were less than 5%, and the recoveries at two fortified levels were between 88.3 and 104.8%. The proposed methodology is simple and highly efficient, with good repeatability and recovery. Compared with currently available methods, the present work has advantages of using less time and labour, higher extraction efficiency, and less consumption of the acid catalyst. This method may have applications for the one-step extraction and hydrolysis of bioactive compounds from plant materials. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero

2014-11-01

The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption-elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L- 1, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64-22.9 μg Pb L- 1).

Exploring hardness enhancement in superhard tungsten tetraboride-based solid solutions using radial X-ray diffraction

DOE PAGES

Xie, Miao; Mohammadi, Reza; Turner, Christopher L.; ...

2015-07-29

In this paper, we explore the hardening mechanisms in WB4-based solid solutions upon addition of Ta, Mn, and Cr using in situ radial X-ray diffraction techniques under nonhydrostatic pressure. By examining the lattice-supported differential strain, we provide insights into the mechanism for hardness increase in binary solid solutions at low dopant concentrations. Speculations on the combined effects of electronic structure and atomic size in ternary WB 4 solid solutions containing Ta with Mn or Cr are also included to understand the extremely high hardness of these materials.

Ion mobility and transport properties of bismuth fluoride-containing solid solutions with tysonite-type structure

NASA Astrophysics Data System (ADS)

Kavun, V. Ya.; Uvarov, N. F.; Slobodyuk, A. B.; Merkulov, E. B.; Polyantsev, M. M.

2018-07-01

The ion mobility and conductivity of solid solutions with tysonite-type structure obtained by doping bismuth trifluoride with lead (II) fluoride, and zirconium and bismuth oxides have been studied using 19F NMR, X-ray diffraction analysis, and impedance spectroscopy. The types of ionic motions in the fluoride sublattice of the synthesized solid solutions in the temperature range 150-450 K have been determined and the energy of their activation has been estimated. Due to high ionic conductivity, above 10-2 S/cm at 570 K, these solid solutions can be considered as superionic conductors.

Solid-solution CrCoCuFeNi high-entropy alloy thin films synthesized by sputter deposition

DOE PAGES

An, Zhinan; Jia, Haoling; Wu, Yueying; ...

2015-05-04

The concept of high configurational entropy requires that the high-entropy alloys (HEAs) yield single-phase solid solutions. However, phase separations are quite common in bulk HEAs. A five-element alloy, CrCoCuFeNi, was deposited via radio frequency magnetron sputtering and confirmed to be a single-phase solid solution through the high-energy synchrotron X-ray diffraction, energy-dispersive spectroscopy, wavelength-dispersive spectroscopy, and transmission electron microscopy. The formation of the solid-solution phase is presumed to be due to the high cooling rate of the sputter-deposition process.

A method for the detection of the refractive index of irregular shape solid pigments in light absorbing liquid matrix.

PubMed

Niskanen, Ilpo; Räty, Jukka; Peiponen, Kai-Erik

2010-06-15

The immersion liquid method is powerful for the measurement of the refractive index of solid particles in a liquid matrix. However, this method applies best for cases when the liquid matrix is transparent. A problem is usually how to assess the refractive index of a pigment when it is in a colored host liquid. In this article we introduce a method, and show that by combining so-called multifunction spectrophotometer, immersion liquid method and detection of light transmission and reflection we can assess the refractive index of a pigment in a colored liquid, and also the extinction or absorption coefficient of the host liquid.

Modelling solid solutions with cluster expansion, special quasirandom structures, and thermodynamic approaches

NASA Astrophysics Data System (ADS)

Saltas, V.; Horlait, D.; Sgourou, E. N.; Vallianatos, F.; Chroneos, A.

2017-12-01

Modelling solid solutions is fundamental in understanding the properties of numerous materials which are important for a range of applications in various fields including nanoelectronics and energy materials such as fuel cells, nuclear materials, and batteries, as the systematic understanding throughout the composition range of solid solutions for a range of conditions can be challenging from an experimental viewpoint. The main motivation of this review is to contribute to the discussion in the community of the applicability of methods that constitute the investigation of solid solutions computationally tractable. This is important as computational modelling is required to calculate numerous defect properties and to act synergistically with experiment to understand these materials. This review will examine in detail two examples: silicon germanium alloys and MAX phase solid solutions. Silicon germanium alloys are technologically important in nanoelectronic devices and are also relevant considering the recent advances in ternary and quaternary groups IV and III-V semiconductor alloys. MAX phase solid solutions display a palette of ceramic and metallic properties and it is anticipated that via their tuning they can have applications ranging from nuclear to aerospace industries as well as being precursors for particular MXenes. In the final part, a brief summary assesses the limitations and possibilities of the methodologies discussed, whereas there is discussion on the future directions and examples of solid solution systems that should prove fruitful to consider.

Quench-age method for the fabrication of niobium-aluminum superconductors

DOEpatents

Pickus, Milton R.; Ciardella, Robert L.

1978-01-01

A flexible Nb.sub.3 Al superconducting wire is fabricated from a niobium-aluminum composite wire by heating to form a solid solution which is retained at room temperature as a metastable solid solution by quenching. The metastable solid solution is then transformed to the stable superconducting A-15 phase by low temperature aging. The transformation induced by aging can be controlled to yield either a multifilamentary or a solid A-15 core surrounded by ductile niobium.

Plastic zone size and crack tip opening displacement of a Dugdale crack interacting with a coated circular inclusion

NASA Astrophysics Data System (ADS)

Hoh, H. J.; Xiao, Z. M.; Luo, J.

2010-09-01

An analytical investigation on the plastic zone size of a crack near a coated circular inclusion under three different loading conditions of uniaxial tension, uniform tension and pure shear was carried out. Both the crack and coated circular inclusion are embedded in an infinite matrix, with the crack oriented along the radial direction of the inclusion. In the solution procedure, the crack is simulated as a continuous distribution of edge dislocations. With the Dugdale model of small-scale yielding [J. Mech. Phys. Solids 8 (1960) p. 100], two thin strips of yielded plastic zones are introduced at both crack tips. Using the solution for a coated circular inclusion interacting with a single dislocation as the Green's function, the physical problem is formulated into a set of singular integral equations. Using the method of Erdogan and Gupta [Q. J. Appl. Math. 29 (1972) p. 525] and iterative numerical procedures, the singular integral equations are solved numerically for the plastic zone sizes and crack tip opening displacement.

Analytical method for predicting the pressure distribution about a nacelle at transonic speeds

NASA Technical Reports Server (NTRS)

Keith, J. S.; Ferguson, D. R.; Merkle, C. L.; Heck, P. H.; Lahti, D. J.

1973-01-01

The formulation and development of a computer analysis for the calculation of streamlines and pressure distributions around two-dimensional (planar and axisymmetric) isolated nacelles at transonic speeds are described. The computerized flow field analysis is designed to predict the transonic flow around long and short high-bypass-ratio fan duct nacelles with inlet flows and with exhaust flows having appropriate aerothermodynamic properties. The flow field boundaries are located as far upstream and downstream as necessary to obtain minimum disturbances at the boundary. The far-field lateral flow field boundary is analytically defined to exactly represent free-flight conditions or solid wind tunnel wall effects. The inviscid solution technique is based on a Streamtube Curvature Analysis. The computer program utilizes an automatic grid refinement procedure and solves the flow field equations with a matrix relaxation technique. The boundary layer displacement effects and the onset of turbulent separation are included, based on the compressible turbulent boundary layer solution method of Stratford and Beavers and on the turbulent separation prediction method of Stratford.

A homogenization approach for the effective drained viscoelastic properties of 2D porous media and an application for cortical bone.

PubMed

Nguyen, Sy-Tuan; Vu, Mai-Ba; Vu, Minh-Ngoc; To, Quy-Dong

2018-02-01

Closed-form solutions for the effective rheological properties of a 2D viscoelastic drained porous medium made of a Generalized Maxwell viscoelastic matrix and pore inclusions are developed and applied for cortical bone. The in-plane (transverse) effective viscoelastic bulk and shear moduli of the Generalized Maxwell rheology of the homogenized medium are expressed as functions of the porosity and the viscoelastic properties of the solid phase. When deriving these functions, the classical inverse Laplace-Carson transformation technique is avoided, due to its complexity, by considering the short and long term approximations. The approximated results are validated against exact solutions obtained from the inverse Laplace-Carson transform for a simple configuration when the later is available. An application for cortical bone with assumption of circular pore in the transverse plane shows that the proposed approximation fit very well with experimental data. Copyright © 2017 Elsevier Ltd. All rights reserved.

Oxidation Behavior of Carbon Fiber-Reinforced Composites

NASA Technical Reports Server (NTRS)

Sullivan, Roy M.

2008-01-01

OXIMAP is a numerical (FEA-based) solution tool capable of calculating the carbon fiber and fiber coating oxidation patterns within any arbitrarily shaped carbon silicon carbide composite structure as a function of time, temperature, and the environmental oxygen partial pressure. The mathematical formulation is derived from the mechanics of the flow of ideal gases through a chemically reacting, porous solid. The result of the formulation is a set of two coupled, non-linear differential equations written in terms of the oxidant and oxide partial pressures. The differential equations are solved simultaneously to obtain the partial vapor pressures of the oxidant and oxides as a function of the spatial location and time. The local rate of carbon oxidation is determined at each time step using the map of the local oxidant partial vapor pressure along with the Arrhenius rate equation. The non-linear differential equations are cast into matrix equations by applying the Bubnov-Galerkin weighted residual finite element method, allowing for the solution of the differential equations numerically.

Effect of solution treatment on the fatigue behavior of an as-forged Mg-Zn-Y-Zr alloy

NASA Astrophysics Data System (ADS)

Wang, S. D.; Xu, D. K.; Wang, B. J.; Han, E. H.; Dong, C.

2016-04-01

Through investigating and comparing the fatigue behavior of an as-forged Mg-6.7Zn-1.3Y-0.6Zr (wt.%) alloy before and after solid solution treatment (T4) in laboratory air, the effect of T4 treatment on fatigue crack initiation was disclosed. S-N curves illustrated that the fatigue strength of as-forged samples was 110 MPa, whereas the fatigue strength of T4 samples was only 80 MPa. Observations to fracture surfaces demonstrated that for as-forged samples, fatigue crack initiation sites were covered with a layer of oxide film. However, due to the coarse grain structure and the dissolution of MgZn2 precipitates, the activation and accumulation of {10-12} twins in T4 samples were much easier, resulting in the preferential fatigue crack initiation at cracked twin boundaries (TBs). Surface characterization demonstrated that TB cracking was mainly ascribed to the incompatible plastic deformation in the twinned area and nearby α-Mg matrix.

Homogeneous hydride formation path in α-Zr: Molecular dynamics simulations with the charge-optimized many-body potential

DOE PAGES

Zhang, Yongfeng; Bai, Xian-Ming; Yu, Jianguo; ...

2016-06-01

A formation path for homogeneous γ hydride formation in hcp α-Zr, from solid solution to the ζ and then the γ hydride, was demonstrated using molecular static calculations and molecular dynamic simulations with the charge-optimized many-body (COMB) potential. Hydrogen has limited solubility in α-Zr. Once the solubility limit is exceeded, the stability of solid solution gives way to that of coherent hydride phases such as the ζ hydride by planar precipitation of hydrogen. At finite temperatures, the ζ hydride goes through a partial hcp-fcc transformation via 1/3 <1¯100> slip on the basal plane, and transforms into a mixture of γmore » hydride and α-Zr. In the ζ hydride, slip on the basal plane is favored thermodynamically with negligible barrier, and is therefore feasible at finite temperatures without mechanical loading. The transformation process involves slips of three equivalent shear partials, in contrast to that proposed in the literature where only a single shear partial was involved. The adoption of multiple slip partials minimizes the macroscopic shape change of embedded hydride clusters and the shear strain accumulation in the matrix, and thus reduces the overall barrier needed for homogeneous γ hydride formation. In conclusion, this formation path requires finite temperatures for hydrogen diffusion without mechanical loading. Therefore, it should be effective at the cladding operating conditions.« less

Inclusion Characteristics and Acicular Ferrite Nucleation in Ti-Containing Weld Metals of X80 Pipeline Steel

NASA Astrophysics Data System (ADS)

Wang, Bingxin; Liu, Xianghua; Wang, Guodong

2018-06-01

X80 steel weld metals with Ti contents of 0.003 to 0.13 pct were prepared by the single-pass submerged-arc welding process. The effects of Ti content in weld metals on the constituent phases of inclusions and chemical compositions of the constituent phases, as well as the potency of acicular ferrite (AF) nucleation on the inclusions were investigated. Moreover, the crystallographic orientation relationship between the AF and inclusion was examined. The results show that with an increase in Ti content, the primary constituent phases of the inclusions change from the (Mn-Al-Si-O) compound to a mixture of spinel and pseudobrookite solid solutions, and eventually to pseudobrookite. The spinel solid solution is characterized by the MnTi2O4 constituent. Compared to pseudobrookite, spinel has a lower Ti concentration, but a significantly higher Mn content. In the case of the presence of a considerable amount of spinel, the Mn element is enriched strongly in the inclusions, resulting in the development of a Mn-depleted zone (MDZ) in the matrix around the inclusions, which enhances the driving force for AF formation. AF shows the Baker-Nutting orientation relationship with MnTi2O4. The formation of MDZ and the presence of the Baker-Nutting orientation relationship promote the ability of inclusions to nucleate the intragranular AF.

Inclusion Characteristics and Acicular Ferrite Nucleation in Ti-Containing Weld Metals of X80 Pipeline Steel

NASA Astrophysics Data System (ADS)

Wang, Bingxin; Liu, Xianghua; Wang, Guodong

2018-03-01

X80 steel weld metals with Ti contents of 0.003 to 0.13 pct were prepared by the single-pass submerged-arc welding process. The effects of Ti content in weld metals on the constituent phases of inclusions and chemical compositions of the constituent phases, as well as the potency of acicular ferrite (AF) nucleation on the inclusions were investigated. Moreover, the crystallographic orientation relationship between the AF and inclusion was examined. The results show that with an increase in Ti content, the primary constituent phases of the inclusions change from the (Mn-Al-Si-O) compound to a mixture of spinel and pseudobrookite solid solutions, and eventually to pseudobrookite. The spinel solid solution is characterized by the MnTi2O4 constituent. Compared to pseudobrookite, spinel has a lower Ti concentration, but a significantly higher Mn content. In the case of the presence of a considerable amount of spinel, the Mn element is enriched strongly in the inclusions, resulting in the development of a Mn-depleted zone (MDZ) in the matrix around the inclusions, which enhances the driving force for AF formation. AF shows the Baker-Nutting orientation relationship with MnTi2O4. The formation of MDZ and the presence of the Baker-Nutting orientation relationship promote the ability of inclusions to nucleate the intragranular AF.

Solid polymer electrolyte lithium batteries

DOEpatents

Alamgir, M.; Abraham, K.M.

1993-10-12

This invention pertains to Lithium batteries using Li ion (Li[sup +]) conductive solid polymer electrolytes composed of solvates of Li salts immobilized in a solid organic polymer matrix. In particular, this invention relates to Li batteries using solid polymer electrolytes derived by immobilizing solvates formed between a Li salt and an aprotic organic solvent (or mixture of such solvents) in poly(vinyl chloride). 3 figures.

Solid polymer electrolyte lithium batteries

DOEpatents

Alamgir, Mohamed; Abraham, Kuzhikalail M.

1993-01-01

This invention pertains to Lithium batteries using Li ion (Li.sup.+) conductive solid polymer electrolytes composed of solvates of Li salts immobilized in a solid organic polymer matrix. In particular, this invention relates to Li batteries using solid polymer electrolytes derived by immobilizing solvates formed between a Li salt and an aprotic organic solvent (or mixture of such solvents) in poly(vinyl chloride).

Polyfluorides and Neat Fluorine as Host Material in Matrix-Isolation Experiments.

PubMed

Brosi, Felix; Vent-Schmidt, Thomas; Kieninger, Stefanie; Schlöder, Tobias; Beckers, Helmut; Riedel, Sebastian

2015-11-09

The use of neat fluorine in matrix isolation is reported, as well as the formation of polyfluoride monoanions under cryogenic conditions. Purification procedures and spectroscopic data of fluorine are described, and matrix shifts of selected molecules and impurities in solid fluorine are compared to those of common matrix gases (Ar, Kr, N2 , Ne). The reaction of neat fluorine and IR-laser ablated metal atoms to yield fluorides of chromium (CrF5 ), palladium (PdF2 ), gold (AuF5 ), and praseodymium (PrF4 ) has been investigated. The fluorides have been characterized in solid fluorine by IR spectroscopy at 5 K. Also the fluorination of Kr and the photo-dismutation of XeO4 have been studied by using IR spectroscopy in neat fluorine. Formation of the [F5 ](-) ion was obtained by IR-laser ablation of platinum in the presence of fluorine and proven in a Ne matrix at 5 K by two characteristic vibrational bands of [F5 ](-) at $\\tilde \

Correlation of Solid State and Solution Coordination Numbers with Infrared Spectroscopy in Five-, Six-, and Eight-Coordinate Transition Metal Complexes of DOTAM.

PubMed

Nagata, Maika K C T; Brauchle, Paul S; Wang, Sen; Briggs, Sarah K; Hong, Young Soo; Laorenza, Daniel W; Lee, Andrea G; Westmoreland, T David

2016-08-16

Three new DOTAM (1,4,7,10-tetrakis(acetamido)-1,4,7,10-tetraazacyclododecane) complexes have been synthesized and characterized by X-ray crystallography: [Co(DOTAM)]Cl 2 •3H 2 O, [Ni(DOTAM)]Cl 2 •4H 2 O, and [Cu(DOTAM)](ClO 4 ) 2 •H 2 O. Solid state and solution IR spectroscopic features for a series of [M(DOTAM)] 2+ complexes (M=Mn, Co, Cu, Ni, Ca, Zn) correlate with solid state and solution coordination numbers. [Co(DOTAM)] 2+ , [Ni(DOTAM)] 2+ , and [Zn(DOTAM)] 2+ are demonstrated to be six-coordinate in both the solid state and in solution, while [Mn(DOTAM)] 2+ and [Ca(DOTAM)] 2+ are eight-coordinate in the solid state and remain so in solution. [Cu(DOTAM)] 2+ , which is five-coordinate by X-ray crystallography, is shown to increase its coordination number in solution to six-coordinate.

Synthesis and electrochemical property of amorphous carbon nanotubes wrapped sulfur particles as cathode material for lithium-sulfur batteries

NASA Astrophysics Data System (ADS)

Hu, Jingtian; Zhao, Tingkai; Ji, Xianglin; Peng, Xiarong; Jin, Wenbo; Yang, Wenbo; Zhang, Lei; Gao, Junjie; Dang, Alei; Li, Hao; Li, Tiehu

2017-11-01

Amorphous carbon nanotube (ACNT)/sulfur composites were prepared by solution reaction method. The electrochemical results showed that both ACNT/S composite and ACNT/S mixture had a first reversible capacity of 1020 mA h·g-1, and the capacity retention of ACNT/S composite was 77% after 100 cycles while that of ACNT/S mixture was only 35% with the initial capacity being 850 mA h·g-1. The experimental results showed that the reversible lithium insertion capacity of the composite was obviously high and the cycling stability was good, which was mainly due to the solid and uniform dispersion of the sulfur and amorphous carbon nanotube matrix in the composite.

Solid/liquid interfacial free energies in binary systems

NASA Technical Reports Server (NTRS)

Nason, D.; Tiller, W. A.

1973-01-01

Description of a semiquantitative technique for predicting the segregation characteristics of smooth interfaces between binary solid and liquid solutions in terms of readily available thermodynamic parameters of the bulk solutions. A lattice-liquid interfacial model and a pair-bonded regular solution model are employed in the treatment with an accommodation for liquid interfacial entropy. The method is used to calculate the interfacial segregation and the free energy of segregation for solid-liquid interfaces between binary solutions for the (111) boundary of fcc crystals. The zone of compositional transition across the interface is shown to be on the order of a few atomic layers in width, being moderately narrower for ideal solutions. The free energy of the segregated interface depends primarily upon the solid composition and the heats of fusion of the component atoms, the composition difference of the solutions, and the difference of the heats of mixing of the solutions.

Composites with improved fiber-resin interfacial adhesion

NASA Technical Reports Server (NTRS)

Cizmecioglu, Muzaffer (Inventor)

1989-01-01

The adhesion of fiber reinforcement such as high modulus graphite to a matrix resin such as polycarbonate is greatly enhanced by applying a very thin layer, suitably from 50 Angstroms to below 1000 Angstroms, to the surface of the fiber such as by immersing the fiber in a dilute solution of the matrix resin in a volatile solvent followed by draining to remove excess solution and air drying to remove the solvent. The thin layer wets the fiber surface. The very dilute solution of matrix resin is able to impregnate multifilament fibers and the solution evenly flows onto the surface of the fibers. A thin uniform layer is formed on the surface of the fiber after removal of the solvent. The matrix resin coated fiber is completely wetted by the matrix resin during formation of the composite. Increased adhesion of the resin to the fibers is observed at fracture. At least 65 percent of the surface of the graphite fiber is covered with polycarbonate resin at fracture whereas uncoated fibers have very little matrix resin adhering to their surfaces at fracture and epoxy sized graphite fibers exhibit only slightly higher coverage with matrix resin at fracture. Flexural modulus of the composite containing matrix resin coated fibers is increased by 50 percent and flexural strength by 37 percent as compared to composites made with unsized fibers.

77 FR 16679 - Emergency Planning and Notification; Emergency Planning and List of Extremely Hazardous...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-03-22

...The U.S. Environmental Protection Agency (EPA or the Agency) is taking final action to revise the manner for applying the threshold planning quantities (TPQs) for those extremely hazardous substances (EHSs) that are non-reactive solid chemicals in solution. This revision allows facilities subject to the Emergency Planning requirements that have a non-reactive solid EHS in solution, to first multiply the amount of the solid chemical in solution on-site by 0.2 before determining if this quantity equals or exceeds the lower published TPQ. This change is based on data that shows less potential for non-reactive solid chemicals in solution to remain airborne and dispersed beyond a facility's fence line in the event of an accidental release. Previously, EPA assumed that 100% of non-reactive solid chemicals in solution could become airborne and dispersed beyond the fenceline in the event of an accidental release.

Immunoaffinity centrifugal precipitation chromatography.

PubMed

Qi, Lin; Ito, Yoichiro

2007-06-01

Purification of proteins based on immunoaffinity has been performed using a solid support coated with antibody against the target proteins. The method requires immobilizing the antibody onto the solid support using protein A or G, and has a risk of adsorptive loss of target proteins onto the solid support. Centrifugal precipitation chromatography has been successfully used to purify enzymes, such as ketosteroid isomerase and hyaluronidase without the use of solid support. The purpose of this study is to demonstrate that immunoaffinity centrifugal precipitation chromatography is capable of isolating an antigen by exploiting antigen-antibody binding. The separation was initiated by filling both channels with 40% saturated ammonium sulfate (AS) of pH 4-4.5 followed by loading 20 microl of human plasma (National Institutes of Health blood bank) mixed with 2 mg of rabbit anti-HSA (human serum protein) antibody (Sigma). Then, the sample channel was eluted with water at 0.03 ml/min and AS channel with 40% AS solution of pH 4-4.5 at 1 ml/min until all non-binding components were eluted. Then, the releasing reagent (50% AS solution containing 0.5 M glycine and 10% ammonium hydroxide at pH 10) was introduced through the AS channel to release the target protein (HSA). The retained antibody was recovered by eluting the sample channel with water at 1 ml/min. A hollow fiber membrane device at the outlet (MicroKros, Spectrum, New Brunswick, NJ, USA) was provided on-line dialysis of the eluent before fractions were collected, so that the fractions could be analyzed by SDS-PAGE (sodium dodecyl sulfate - polyacrylamide gel electrophoresis) without further dialysis. The current method does not require immobilizing the antibody onto a matrix, which is used by the conventional immunoaffinity chromatography. This method ensures full recovery of the antigen and antibody, and it may be applied to purification of other proteins.

System and process for dissolution of solids

DOEpatents

Liezers, Martin; Farmer, III, Orville T.

2017-10-10

A system and process are disclosed for dissolution of solids and "difficult-to-dissolve" solids. A solid sample may be ablated in an ablation device to generate nanoscale particles. Nanoparticles may then swept into a coupled plasma device operating at atmospheric pressure where the solid nanoparticles are atomized. The plasma exhaust may be delivered directly into an aqueous fluid to form a solution containing the atomized and dissolved solids. The composition of the resulting solution reflects the composition of the original solid sample.

Energy Dissipation of Rayleigh Waves due to Absorption Along the Path by the Use of Finite Element Method

DTIC Science & Technology

1979-07-31

3 x 3 t Strain vector a ij,j Space derivative of the stress tensor Fi Force vector per unit volume o Density x CHAPTER III F Total force K Stiffness...matrix 6Vector displacements M Mass matrix B Space operating matrix DO Matrix moduli 2 x 3 DZ Operating matrix in Z direction N Matrix of shape...dissipating medium the deformation of a solid is a function of time, temperature and space . Creep phenomenon is a deformation process in which there is

Thermal Dispersion Within a Porous Medium Near a Solid Wall

NASA Technical Reports Server (NTRS)

Simon, T.; McFadden, G.; Ibrahim, M.

2006-01-01

The regenerator is a key component to Stirling cycle machine efficiency. Typical regenerators are of sintered fine wires or layers of fine-wire screens. Such porous materials are contained within solid-waH casings. Thermal energy exchange between the regenerator and the casing is important to cycle performance for the matrix and casing would not have the same axial temperature profile in an actual machine. Exchange from one to the other may allow shunting of thermal energy, reducing cycle efficiency. In this paper, temperature profiles within the near-wall region of the matrix are measured and thermal energy transport, termed thermal dispersion, is inferred. The data show how the wall affects thermal transport. Transport normal to the mean flow direction is by conduction within the solid and fluid and by advective transport within the matrix. In the near-wall region, both may be interrupted from their normal in-core pattern. Solid conduction paths are broken and scales of advective transport are damped. An equation is presented which describes this change for a wire screen mesh. The near-wall layer typically acts as an insulating layer. This should be considered in design or analysis. Effective thermal conductivity within the core is uniform. In-core transverse thermal effective conductivity values are compared to direct and indirect measurements reported elsewhere and to 3D numerical simulation results, computed previously and reported elsewhere. The 3-D CFD model is composed of six cylinders in cross flow, staggered in arrangement to match the dimensions and porosity of the matrix used in the experiments. The commercial code FLUENT is used to obtain the flow and thermal fields. The thermal dispersion and effective thermal conductivities for the matrix are computed from the results.

Surface modification of an aluminum alloy by electron beam introducing TiCN nanoparticles

NASA Astrophysics Data System (ADS)

Kolev, M.; Dimitrova, R.; Parshorov, St.; Valkov, St.; Lazarova, R.; Petrov, P.

2018-03-01

TiCN nanopowder deposited in an appropriate way on the surface of an AlSi12Cu2NiMg substrate was incorporated in the matrix using an electron beam technology. The samples were studied by means of light microscopy, SEM, and EDX; their microhardness was also determined. The formation was found of a uniform and dense coating with a thickness of 7 – 10 μgm with a good adherence to the substrate. A modified zone appeared under the coating with a thickness of 100 – 150 μgm containing dendrites of an α-solid solution and a fine eutectic between them, as well as primary silicon crystals. The microhardness of this modified zone was up to 2.4 times higher than that of the matrix. The results of SEM and EDX studies revealed unambiguously the presence of titanium in the coating and in the zones below it. Obviously, the electron beam treatment resulted in the TiCN nanoparticles penetrating into the coating and the substrate immediately below the coating.

Near-infrared fluorescence image quality test methods for standardized performance evaluation

NASA Astrophysics Data System (ADS)

Kanniyappan, Udayakumar; Wang, Bohan; Yang, Charles; Ghassemi, Pejhman; Wang, Quanzeng; Chen, Yu; Pfefer, Joshua

2017-03-01

Near-infrared fluorescence (NIRF) imaging has gained much attention as a clinical method for enhancing visualization of cancers, perfusion and biological structures in surgical applications where a fluorescent dye is monitored by an imaging system. In order to address the emerging need for standardization of this innovative technology, it is necessary to develop and validate test methods suitable for objective, quantitative assessment of device performance. Towards this goal, we develop target-based test methods and investigate best practices for key NIRF imaging system performance characteristics including spatial resolution, depth of field and sensitivity. Characterization of fluorescence properties was performed by generating excitation-emission matrix properties of indocyanine green and quantum dots in biological solutions and matrix materials. A turbid, fluorophore-doped target was used, along with a resolution target for assessing image sharpness. Multi-well plates filled with either liquid or solid targets were generated to explore best practices for evaluating detection sensitivity. Overall, our results demonstrate the utility of objective, quantitative, target-based testing approaches as well as the need to consider a wide range of factors in establishing standardized approaches for NIRF imaging system performance.

Production of three-dimensional quantum dot lattice of Ge/Si core-shell quantum dots and Si/Ge layers in an alumina glass matrix.

PubMed

Buljan, M; Radić, N; Sancho-Paramon, J; Janicki, V; Grenzer, J; Bogdanović-Radović, I; Siketić, Z; Ivanda, M; Utrobičić, A; Hübner, R; Weidauer, R; Valeš, V; Endres, J; Car, T; Jerčinović, M; Roško, J; Bernstorff, S; Holy, V

2015-02-13

We report on the formation of Ge/Si quantum dots with core/shell structure that are arranged in a three-dimensional body centered tetragonal quantum dot lattice in an amorphous alumina matrix. The material is prepared by magnetron sputtering deposition of Al2O3/Ge/Si multilayer. The inversion of Ge and Si in the deposition sequence results in the formation of thin Si/Ge layers instead of the dots. Both materials show an atomically sharp interface between the Ge and Si parts of the dots and layers. They have an amorphous internal structure that can be crystallized by an annealing treatment. The light absorption properties of these complex materials are significantly different compared to films that form quantum dot lattices of the pure Ge, Si or a solid solution of GeSi. They show a strong narrow absorption peak that characterizes a type II confinement in accordance with theoretical predictions. The prepared materials are promising for application in quantum dot solar cells.

Analytical solution for the transient wave propagation of a buried cylindrical P-wave line source in a semi-infinite elastic medium with a fluid surface layer

NASA Astrophysics Data System (ADS)

Shan, Zhendong; Ling, Daosheng

2018-02-01

This article develops an analytical solution for the transient wave propagation of a cylindrical P-wave line source in a semi-infinite elastic solid with a fluid layer. The analytical solution is presented in a simple closed form in which each term represents a transient physical wave. The Scholte equation is derived, through which the Scholte wave velocity can be determined. The Scholte wave is the wave that propagates along the interface between the fluid and solid. To develop the analytical solution, the wave fields in the fluid and solid are defined, their analytical solutions in the Laplace domain are derived using the boundary and interface conditions, and the solutions are then decomposed into series form according to the power series expansion method. Each item of the series solution has a clear physical meaning and represents a transient wave path. Finally, by applying Cagniard's method and the convolution theorem, the analytical solutions are transformed into the time domain. Numerical examples are provided to illustrate some interesting features in the fluid layer, the interface and the semi-infinite solid. When the P-wave velocity in the fluid is higher than that in the solid, two head waves in the solid, one head wave in the fluid and a Scholte wave at the interface are observed for the cylindrical P-wave line source.

Laboratory analog and numerical study of groundwater flow and solute transport in a karst aquifer with conduit and matrix domains.

PubMed

Faulkner, Jonathan; Hu, Bill X; Kish, Stephen; Hua, Fei

2009-11-03

New mathematical and laboratory methods have been developed for simulating groundwater flow and solute transport in karst aquifers having conduits imbedded in a porous medium, such as limestone. The Stokes equations are used to model the flow in the conduits and the Darcy equation is used for the flow in the matrix. The Beavers-Joseph interface boundary conditions are adopted to describe the flow exchange at the interface boundary between the two domains. A laboratory analog is used to simulate the conduit and matrix domains of a karst aquifer. The conduit domain is located at the bottom of the transparent plexiglas laboratory analog and glass beads occupy the remaining space to represent the matrix domain. Water flows into and out of the two domains separately and each has its own supply and outflow reservoirs. Water and solute are exchanged through an interface between the two domains. Pressure transducers located within the matrix and conduit domains of the analog provide data that is processed and stored in digital format. Dye tracing experiments are recorded using time-lapse imaging. The data and images produced are analyzed by a spatial analysis program. The experiments provide not only hydraulic head distribution but also capture solute front images and mass exchange measurements between the conduit and matrix domains. In the experiment, we measure and record pressures, and quantify flow rates and solute transport. The results present a plausible argument that laboratory analogs can characterize groundwater water flow, solute transport, and mass exchange between the conduit and matrix domains in a karst aquifer. The analog validates the predictions of a numerical model and demonstrates the need of laboratory analogs to provide verification of proposed theories and the calibration of mathematical models.

Matrix cracking with irregular fracture fronts as observed in fiber reinforced ceramic composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hu, K.X.; Yeh, C.P.; Wyatt, K.W.

1998-01-01

As a result of matrix cracking in fiber reinforced composites, fracture planforms assume a wide variation of profiles due to the fact that fiber bridging strongly affects the behavior of local crack fronts. This observation raises the question on the legitimacy of commonly used penny-shaped crack solutions when applied to fiber reinforced composites. Accordingly, investigation of the effects of fracture front profiles on mechanical responses is the thrust of this paper. The authors start with the solution of a penny-shaped crack in a unidirectional, fiber reinforced composite, which demonstrates necessity of considering wavy fracture fronts in fiber reinforced composites. Amore » theoretical framework for fiber reinforced composites with irregular fracture fronts due to matrix cracking is then established via a micromechanics model. The difference between small crack-size matrix cracking and large crack-size matrix cracking is investigated in detail. It is shown that the bridging effect is insignificant when matrix crack size is small and solution of effective property are obtained using Mori-Tanaka`s method by treating cracks and reinforcing fibers as distinct, but interacting phases. When the crack size becomes large, the bridging effects has to be taken into consideration. With bridging tractions obtained in consistency with the micromechanics solution, and corresponding crack energy backed out, the effective properties are obtained through a modification of standard Mori-Tanaka`s treatment of multiphase composites. Analytical solutions show that the generalization of a crack density of a penny-shaped planform is insufficient in describing the effective responses of fiber-reinforced composites with matrix cracking. Approximate solutions that account for the effects of the irregularity of crack planforms are given in closed forms for several irregular crack planforms, including cracks of cross rectangle, polygon and rhombus.« less

Solid lipid nanoparticles suspension versus commercial solutions for dermal delivery of minoxidil.

PubMed

Padois, Karine; Cantiéni, Céline; Bertholle, Valérie; Bardel, Claire; Pirot, Fabrice; Falson, Françoise

2011-09-15

Solid lipid nanoparticles have been reported as possible carrier for skin drug delivery. Solid lipid nanoparticles are produced from biocompatible and biodegradable lipids. Solid lipid nanoparticles made of semi-synthetic triglycerides stabilized with a mixture of polysorbate and sorbitan oleate were loaded with 5% of minoxidil. The prepared systems were characterized for particle size, pH and drug content. Ex vivo skin penetration studies were performed using Franz-type glass diffusion cells and pig ear skin. Ex vivo skin corrosion studies were realized with a method derived from the Corrositex(®) test. Solid lipid nanoparticles suspensions were compared to commercial solutions in terms of skin penetration and skin corrosion. Solid lipid nanoparticles suspensions have been shown as efficient as commercial solutions for skin penetration; and were non-corrosive while commercial solutions presented a corrosive potential. Solid lipid nanoparticles suspensions would constitute a promising formulation for hair loss treatment. Copyright © 2011 Elsevier B.V. All rights reserved.

A review of the matrix-exponential formalism in radiative transfer

NASA Astrophysics Data System (ADS)

Efremenko, Dmitry S.; Molina García, Víctor; Gimeno García, Sebastián; Doicu, Adrian

2017-07-01

This paper outlines the matrix exponential description of radiative transfer. The eigendecomposition method which serves as a basis for computing the matrix exponential and for representing the solution in a discrete ordinate setting is considered. The mathematical equivalence of the discrete ordinate method, the matrix operator method, and the matrix Riccati equations method is proved rigorously by means of the matrix exponential formalism. For optically thin layers, approximate solution methods relying on the Padé and Taylor series approximations to the matrix exponential, as well as on the matrix Riccati equations, are presented. For optically thick layers, the asymptotic theory with higher-order corrections is derived, and parameterizations of the asymptotic functions and constants for a water-cloud model with a Gamma size distribution are obtained.

Characterization of the Vibrio cholerae extracellular matrix: a top-down solid-state NMR approach.

PubMed

Reichhardt, Courtney; Fong, Jiunn C N; Yildiz, Fitnat; Cegelski, Lynette

2015-01-01

Bacterial biofilms are communities of bacterial cells surrounded by a self-secreted extracellular matrix. Biofilm formation by Vibrio cholerae, the human pathogen responsible for cholera, contributes to its environmental survival and infectivity. Important genetic and molecular requirements have been identified for V. cholerae biofilm formation, yet a compositional accounting of these parts in the intact biofilm or extracellular matrix has not been described. As insoluble and non-crystalline assemblies, determinations of biofilm composition pose a challenge to conventional biochemical and biophysical analyses. The V. cholerae extracellular matrix composition is particularly complex with several proteins, complex polysaccharides, and other biomolecules having been identified as matrix parts. We developed a new top-down solid-state NMR approach to spectroscopically assign and quantify the carbon pools of the intact V. cholerae extracellular matrix using ¹³C CPMAS and ¹³C{(¹⁵N}, ¹⁵N{³¹P}, and ¹³C{³¹P}REDOR. General sugar, lipid, and amino acid pools were first profiled and then further annotated and quantified as specific carbon types, including carbonyls, amides, glycyl carbons, and anomerics. In addition, ¹⁵N profiling revealed a large amine pool relative to amide contributions, reflecting the prevalence of molecular modifications with free amine groups. Our top-down approach could be implemented immediately to examine the extracellular matrix from mutant strains that might alter polysaccharide production or lipid release beyond the cell surface; or to monitor changes that may accompany environmental variations and stressors such as altered nutrient composition, oxidative stress or antibiotics. More generally, our analysis has demonstrated that solid-state NMR is a valuable tool to characterize complex biofilm systems. Copyright © 2014. Published by Elsevier B.V.

Synthesis and characterization of P-doped amorphous and nanocrystalline Si

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Jialing; Ganguly, Shreyashi; Sen, Sabyasachi

Intentional impurity doping lies at the heart of the silicon technology. The dopants provide electrons or holes as necessary carriers of the electron current and can significantly modify the electric, optical and magnetic properties of the semiconductors. P-doped amorphous Si (a-Si) was prepared by a solid state and solution metathesis reaction of a P-doped Zintl phase precursor, NaSi 0.99P 0.01, with an excess of NH 4X (X = Br, I). After the salt byproduct was removed from the solid state reaction, the a-Si material was annealed at 600 °C under vacuum for 2 h, resulting in P-doped nanocrystalline Si (nc-Si)more » material embedded in a-Si matrix. The product from the solution reaction also shows a combination of nc-Si embedded in a-Si; however, it was fully converted to nc-Si after annealing under argon at 650 °C for 30 min. Powder X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) show the amorphous nature of the P-doped Si material before the annealing and the nanocrystallinity after the annealing. Fourier Transform Infrared (FTIR) spectroscopy shows that the P-doped Si material surface is partially capped by H and O or with solvent. Finally, electron microprobe wavelength dispersive spectroscopy (WDS) as well as energy dispersive spectroscopy (EDS) confirm the presence of P in the Si material. 29Si and 31P solid state magic-angle-spinning nuclear magnetic resonance (MAS NMR) spectroscopy data provide the evidence of P doping into the Si structure with the P concentration of approximately 0.07 at.%.« less

Mechanosynthesis of A Ferritic ODS (Oxide Dispersion Strengthened) Steel Containing 14% Chromium and Its Characterization

NASA Astrophysics Data System (ADS)

Rivai, A. K.; Dimyati, A.; Adi, W. A.

2017-05-01

One of the advanced materials for application at high temperatures which is aggressively developed in the world is ODS (Oxide Dispersion strengthened) steel. ODS ferritic steels are one of the candidate materials for future nuclear reactors in the world (Generation IV reactors) because it is able to be used in the reactor above 600 °C. ODS ferritic steels have also been developed for the interconnect material of SOFC (Solid Oxide Fuel Cell) which will be exposed to about 800 °C of temperature. The steel is strengthened by dispersing homogeneously of oxide particles (ceramic) in nano-meter sized in the matrix of the steel. Synthesis of a ferritic ODS steel by dispersion of nano-particles of yttrium oxide (yttria: Y2O3) as the dispersion particles, and containing high-chromium i.e. 14% has been conducted. Synthesis of the ODS steels was done mechanically (mechanosynthesis) using HEM (High Energy ball Milling) technique for 40 and 100 hours. The resulted samples were characterized using SEM-EDS (Scanning Electron Microscope-Energy Dispersive Spectroscope), and XRD (X-ray diffraction) to analyze the microstructure characteristics. The results showed that the crystal grains of the sample with 100 hours milling time was much smaller than the sample with 40 hours milling time, and some amount of alloy was formed during the milling process even for 40 hours milling time. Furthermore, the structure analysis revealed that some amount of iron atom substituted by a slight amount of chromium atom as a solid solution. The quantitative analysis showed that the phase mostly consisted of FeCr solid-solution with the structure was BCC (body-centered cubic).

Analysis of benzylpenicillin in milk using MALDI-TOF mass spectrometry with top-down synthesized TiO2 nanowires as the solid matrix.

PubMed

Kim, Jo-Il; Park, Jong-Min; Noh, Joo-Yoon; Hwang, Seong-Ju; Kang, Min-Jung; Pyun, Jae-Chul

2016-01-01

In this work, the wet-corrosion process for the synthesis of titanium oxide (TiO2) nanowires in the anatase phase was optimized as the solid matrix in MALDI-TOF mass spectrometry, and the solid matrix of the TiO2 nanowires was applied to the detection of antibiotics in a daily milk sample. The influence of the alkali concentration and the heat treatment temperature on the crystal structure of the TiO2 nanowires was investigated. The ionization activity of the TiO2 nanowires was estimated for each synthetic condition using amino acids as model analytes with low molecular weights. For the detection of antibiotics in milk, benzylpenicillin was spiked in daily milk samples, and MALDI-TOF mass spectrometry with the TiO2 nanowires was demonstrated to detect the benzylpenicillin at the cut-off concentration of the EU directive. Copyright © 2015 Elsevier Ltd. All rights reserved.

Graphene-encapsulated silica as matrix solid-phase dispersion extraction sorbents for the analysis of poly-methoxylated flavonoids in the leaves of Murraya panaculata (L.) Jack.

PubMed

Sun, Ting; Li, Xuwen; Yang, Jie; Li, Lanjie; Jin, Yongri; Shi, Xiaolei

2015-06-01

In this study, graphene-encapsulated silica was synthesized by a hydrothermal reduction strategy. The presence of silica in graphene was identified by Fourier-transform infrared spectrometry, X-ray diffraction and scanning electron microscopy. The graphene-encapsulated silica subsequently was used as adsorbent for matrix solid-phase dispersion extraction of poly-methoxylated flavonoids from the dried leaves of Murraya panaculata (L.) Jack. Compared with the other adsorbents (graphene, silica gel, C18 silica, neutral alumina, diatomaceous earth) and without any adsorbents, better results were obtained. Then a method for analysis of poly-methoxylated flavonoids was established by coupling matrix solid-phase dispersion extraction with ultra high performance liquid chromatography and UV detection. Compared with reflux extraction and ultrasonic extraction, the proposed method is quicker, more efficient and more environmental protection. Less than 10 min is needed from extraction to detection. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Absorption, scattering, and radiation force efficiencies in the longitudinal wave scattering by a small viscoelastic particle in an isotropic solid.

PubMed

Lopes, J H; Leão-Neto, J P; Silva, G T

2017-11-01

Analytical expressions of the absorption, scattering, and elastic radiation force efficiency factors are derived for the longitudinal plane wave scattering by a small viscoelastic particle in a lossless solid matrix. The particle is assumed to be much smaller than the incident wavelength, i.e., the so-called long-wavelength (Rayleigh) approximation. The efficiencies are dimensionless quantities that represent the absorbed and scattering powers and the elastic radiation force on the particle. In the quadrupole approximation, they are expressed in terms of contrast functions (bulk and shear moduli, and density) between the particle and solid matrix. The results for a high-density polyethylene particle embedded in an aluminum matrix agree with those obtained with the partial wave expansion method. Additionally, the connection between the elastic radiation force and forward scattering function is established through the optical theorem. The present results should be useful for ultrasound characterization of particulate composites, and the development of implanted devices activated by radiation force.

Difficulty Factors, Distribution Effects, and the Least Squares Simplex Data Matrix Solution

ERIC Educational Resources Information Center

Ten Berge, Jos M. F.

1972-01-01

In the present article it is argued that the Least Squares Simplex Data Matrix Solution does not deal adequately with difficulty factors inasmuch as the theoretical foundation is insufficient. (Author/CB)

Human umbilical cord derived matrix: A scaffold suitable for tissue engineering application.

PubMed

Dan, Pan; Velot, Émilie; Mesure, Benjamin; Groshenry, Guillaume; Bacharouche, Jalal; Decot, Véronique; Menu, Patrick

2017-01-01

Human tissue derived natural extracellular matrix (ECM) has great potential in tissue engineering. We sought to isolate extracellular matrix derived from human umbilical cord and test its potential in tissue engineering. An enzymatic method was applied to isolate and solubilized complete human umbilical cord derived matrix (hUCM). The obtained solution was analyzed for growth factors, collagen and residual DNA contents, then used to coat 2D and 3D surfaces for cell culture application. The hUCM was successfully isolated with trypsin digestion to acquire a solution containing various growth factors and collagen but no residual DNA. This hUCM solution can form a coating on 2D and 3D substrates suitable cell culture. We developed a new matrix derived from human source that can be further used in tissue engineering.

Friction Stir Welding of SiC/Aluminum Metal Matrix Composites

NASA Technical Reports Server (NTRS)

Lee, Jonathan A.

1999-01-01

Friction Stir Welding (FSW) is a new solid state process for joining metals by plasticizing and consolidating materials around the bond line using thermal energy producing from frictional forces. A feasibility study for FSW of Metal Matrix Composites (MMC) was investigated using aluminum 6092 alloy reinforced with 17% SiC particulates. FSW process consists of a special rotating pin tool that is positioned to plunge into the MMC surface at the bond line. As the tool rotates and move forward along the bond line, the material at the bond line is heated up and forced to flow around the rotating tip to consolidate on the tip's backside to form a solid state joint. FSW has the potential for producing sound welds with MMC because the processing temperature occurs well below the melting point of the metal matrix; thereby eliminating the reinforcement-to-matrix solidification defects, reducing the undesirable chemical reactions and porosity problems.

Fused deposition modeling provides solution for magnetic resonance imaging of solid dosage form by advancing design quickly from prototype to final product.

PubMed

Charest, Ken; Mak-Jurkauskas, Melody L; Cinicola, Daniel; Clausen, Andrew M

2013-02-01

The release profile of active pharmaceutical ingredient (API) from its solid dosage form is an important aspect of drug development as it is often used to predict potential drug release characteristics of a product in vivo. In recent years, magnetic resonance imaging has emerged as a nondestructive technique that captures the physical changes of solid dosage forms during dissolution. An example that highlights this application is in the dissolution of modified-release tablet studies. As the tablet dissolves, API disperses in a hydrogel matrix within the tablet, and swelling of the hydrogel layer eventually leads to release of API over time. To achieve optimum signal-to-noise ratios, the tablet should be placed in the most homogeneous region of the magnet and remain there throughout the dissolution experiment. Moreover, the tablet holder must maintain the tablet position without interfering with the natural dissolution process, such as by crushing the softened tablet. This can be difficult because the size, shape, and rigidity of the tablet change during dissolution. This article describes the process, material, and manufacture of a novel device that meets these challenges, with emphasis on how additive manufacturing on a 3D printer enabled an efficient and inexpensive process of design improvements.

Coating solid dispersions on microneedles via a molten dip coating method: development and in vitro evaluation for transdermal delivery of a water insoluble drug

PubMed Central

Ma, Yunzhe; Gill, Harvinder S.

2014-01-01

This study demonstrates for the first time the ability to coat solid dispersions on microneedles as a means to deliver water-insoluble drugs through the skin. Polyethylene glycol (PEG) was selected as the hydrophilic matrix, and lidocaine base was selected as the model hydrophobic drug to create the solid dispersion. First, thermal characterization and viscosity measurements of the PEG-lidocaine mixture at different mass fractions were performed. The results show that lidocaine can remain stable at temperatures up to ~130 °C, and that viscosity of the PEG-lidocaine molten solution increases as the mass fraction of lidocaine decreases. Differential scanning calorimetry demonstrated that at lidocaine mass fraction less than or equal to 50%, lidocaine is well dispersed in the PEG-lidocaine mixture. Uniform coatings were obtained on microneedle surfaces. In vitro dissolution studies in porcine skin showed that microneedles coated with PEG-lidocaine dispersions resulted in significantly higher delivery of lidocaine in just 3 min compared to 1 h topical application of 0.15 g EMLA®, a commercial lidocaine-prilocaine cream. In conclusion, the molten coating process we introduce here offers a practical approach to coat water-insoluble drugs on microneedles for transdermal delivery. PMID:25213295

Simultaneous determination and qualitative analysis of six types of components in Naoxintong capsule by miniaturized matrix solid-phase dispersion extraction coupled with ultra high-performance liquid chromatography with photodiode array detection and quadrupole time-of-flight mass spectrometry.

PubMed

Wang, Huilin; Jiang, Yan; Ding, Mingya; Li, Jin; Hao, Jia; He, Jun; Wang, Hui; Gao, Xiu-Mei; Chang, Yan-Xu

2018-02-03

A simple and effective sample preparation process based on miniaturized matrix solid-phase dispersion was developed for simultaneous determination of phenolic acids (gallic acid, chlorogenic acid, ferulic acid, 3,5-dicaffeoylqunic acid, 1,5-dicaffeoylqunic acid, rosmarinic acid, lithospermic acid, and salvianolic acid B), flavonoids (kaempferol-3-O-rutinoside, calycosin, and formononetin), lactones (ligustilide and butyllidephthalide), monoterpenoids (paeoniflorin), phenanthraquinones (cryptotanshinone), and furans (5-hydroxymethylfurfural) in Naoxintong capsule by ultra high-performance liquid chromatography. The optimized condition was that 25 mg Naoxintong powder was blended homogeneously with 100 mg Florisil PR for 4 min. One milliliter of methanol/water (75:25, v/v) acidified by 0.05% formic acid was selected to elute all components. It was found that the recoveries of the six types of components ranged from 61.36 to 96.94%. The proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography was successfully applied to simultaneous determination of the six types of components in Naoxintong capsules. The results demonstrated that the proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography could be used as an environmentally friendly tool for the extraction and determination of multiple bioactive components in natural products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Potential Use of {sup 18}F-fluorodeoxyglucose Positron Emission Tomography–Based Quantitative Imaging Features for Guiding Dose Escalation in Stage III Non-Small Cell Lung Cancer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fried, David V., E-mail: dvfried@mdanderson.org; Graduate School of Biomedical Sciences, The University of Texas MD Anderson Cancer Center, Houston, Texas; Mawlawi, Osama

2016-02-01

Purpose: To determine whether previously identified quantitative image features (QIFs) based on {sup 18}F-fluorodeoxyglucose positron emission tomography (FDG-PET) (co-occurrence matrix energy and solidity) are able to isolate subgroups of patients who would receive a benefit or detriment from dose escalation in terms of overall survival (OS) or progression-free survival (PFS). Methods and Materials: Subgroups of a previously analyzed 225 patient cohort were generated with the use of 5-percentile increment cutoff values of disease solidity and primary tumor co-occurrence matrix energy. The subgroups were analyzed with a log-rank test to determine whether there was a difference in OS and PFS betweenmore » patients treated with 60 to 70 Gy and those receiving 74 Gy. Results: In the entire patient cohort, there was no statistical difference in terms of OS or PFS between patients receiving 74 Gy and those receiving 60 to 70 Gy. It was qualitatively observed that as disease solidity and primary co-occurrence matrix energy increased, patients receiving 74 Gy had an improved OS and PFS compared with those receiving 60 to 70 Gy. The opposite trend (detriment of receiving 74 Gy) was also observed regarding low values of disease solidity and primary co-occurrence matrix energy. Conclusions: FDG-PET–based QIFs were found to be capable of isolating subgroups of patients who received a benefit or detriment from dose escalation.« less

Role of the chemical substitution on the luminescence properties of solid solutions Ca{sub (1−x)}Cd{sub (x)}WO{sub 4} (0 ≤ x ≤1)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir; CEA, DEN, Département d'Etudes des Réacteurs, Service de Physique Expérimentale, Laboratoire Dosimétrie Capteurs Instrumentation, 13108 Saint-Paul-lez-Durance

2015-10-15

Highlights: • Luminescence can be modified by chemical substitution in solid solutions Ca{sub 1−x}Cd{sub x}WO{sub 4}. • The various emission spectra (charge transfer) were obtained under X-ray excitation. • Scheelite or wolframite solid solutions presented two types of emission spectra. • A luminescence component depended on cadmium substitution in each solid solution. • A component was only characteristic of oxyanion symmetry in each solid solution. - Abstract: We have investigated the chemical substitution effects on the luminescence properties under X-ray excitation of the solid solutions Ca{sub (1−x)}Cd{sub (x)}WO{sub 4} with 0 ≤ x ≤ 1. Two types of wide spectralmore » bands, associated with scheelite-type or wolframite-type solid solutions, have been observed at room temperature. We decomposed each spectral band into several spectral components characterized by energies and intensities varying with composition x. One Gaussian component was characterized by an energy decreasing regularly with the composition x, while the other Gaussian component was only related to the tetrahedral or octahedral configurations of tungstate groups WO{sub 4}{sup 2−} or WO{sub 6}{sup 6−}. The luminescence intensities exhibited minimum values in the composition range x < 0.5 corresponding to scheelite-type structures, then, they regularly increased for cadmium compositions x > 0.5 corresponding to wolframite-type structures.« less

In Situ Determination of Trace Elements in Fish Otoliths by Laser Ablation Double Focusing Sector Field Inductively Coupled Plasma Mass Spectrometry Using a Solution Standard Addition Calibration Method

NASA Astrophysics Data System (ADS)

Chen, Z.; Jones, C. M.

2002-05-01

Microchemistry of fish otoliths (fish ear bones) is a very useful tool for monitoring aquatic environments and fish migration. However, determination of the elemental composition in fish otolith by ICP-MS has been limited to either analysis of dissolved sample solution or measurement of limited number of trace elements by laser ablation (LA)- ICP-MS due to low sensitivity, lack of available calibration standards, and complexity of polyatomic molecular interference. In this study, a method was developed for in situ determination of trace elements in fish otoliths by laser ablation double focusing sector field ultra high sensitivity Finnigan Element 2 ICP-MS using a solution standard addition calibration method. Due to the lack of matrix-match solid calibration standards, sixteen trace elements (Na, Mg, P, Cr, Mn, Fe, Ni, Cu, Rb, Sr, Y, Cd, La, Ba, Pb and U) were determined using a solution standard calibration with Ca as an internal standard. Flexibility, easy preparation and stable signals are the advantages of using solution calibration standards. In order to resolve polyatomic molecular interferences, medium resolution (M/delta M > 4000) was used for some elements (Na, Mg, P, Cr, Mn, Fe, Ni, and Cu). Both external calibration and standard addition quantification strategies are compared and discussed. Precision, accuracy, and limits of detection are presented.

Box-Behnken experimental design for chromium(VI) ions removal by bacterial cellulose-magnetite composites.

PubMed

Stoica-Guzun, Anicuta; Stroescu, Marta; Jinga, Sorin Ion; Mihalache, Nicoleta; Botez, Adriana; Matei, Cristian; Berger, Daniela; Damian, Celina Maria; Ionita, Valentin

2016-10-01

In this study bacterial cellulose-magnetite composites were synthesised for the removal of chromium(VI) from aqueous solutions. Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis and X-ray Photoelectron Spectroscopy (XPS) were used to characterize the bacterial cellulose-magnetite composites and to reveal the uniform dispersion of nanomagnetite in the BC matrix. Magnetic properties were also measured to confirm the magnetite immobilization on bacterial cellulose membrane. The effects of initial Cr(VI) concentration, solution pH and solid/liquid ratio upon chromium removal were examined using the statistical Box-Behnken Design. Because of the possibility of magnetite dissolution during chromium(VI) adsorption, the degree of iron leaching was also analysed in the same conditions as Cr(VI) adsorption. From the factors affecting chromium(VI) adsorption the most important was solution pH. The highest Cr(VI) removal efficiency was observed at pH 4, accompanied by the lowest iron leaching in the solution. The adsorption experiments also indicated that the adsorption process of chromium(VI) is well described by Freundlich adsorption model. Our results proved that the BC-magnetite composites could be used for an efficient removal of chromium(VI) from diluted solutions with a minimum magnetite dissolution during operation. Copyright © 2016 Elsevier B.V. All rights reserved.

In Vitro, Matrix-Free Formation Of Solid Tumor Spheroids

NASA Technical Reports Server (NTRS)

Gonda, Steve R.; Marley, Garry M.

1993-01-01

Cinostatic bioreactor promotes formation of relatively large solid tumor spheroids exhibiting diameters from 750 to 2,100 micrometers. Process useful in studying efficacy of chemotherapeutic agents and of interactions between cells not constrained by solid matrices. Two versions have been demonstrated; one for anchorage-independent cells and one for anchorage-dependent cells.

Vertically Aligned and Continuous Nanoscale Ceramic-Polymer Interfaces in Composite Solid Polymer Electrolytes for Enhanced Ionic Conductivity.

PubMed

Zhang, Xiaokun; Xie, Jin; Shi, Feifei; Lin, Dingchang; Liu, Yayuan; Liu, Wei; Pei, Allen; Gong, Yongji; Wang, Hongxia; Liu, Kai; Xiang, Yong; Cui, Yi

2018-06-13

Among all solid electrolytes, composite solid polymer electrolytes, comprised of polymer matrix and ceramic fillers, garner great interest due to the enhancement of ionic conductivity and mechanical properties derived from ceramic-polymer interactions. Here, we report a composite electrolyte with densely packed, vertically aligned, and continuous nanoscale ceramic-polymer interfaces, using surface-modified anodized aluminum oxide as the ceramic scaffold and poly(ethylene oxide) as the polymer matrix. The fast Li + transport along the ceramic-polymer interfaces was proven experimentally for the first time, and an interfacial ionic conductivity higher than 10 -3 S/cm at 0 °C was predicted. The presented composite solid electrolyte achieved an ionic conductivity as high as 5.82 × 10 -4 S/cm at the electrode level. The vertically aligned interfacial structure in the composite electrolytes enables the viable application of the composite solid electrolyte with superior ionic conductivity and high hardness, allowing Li-Li cells to be cycled at a small polarization without Li dendrite penetration.

Colloid transport in dual-permeability media

NASA Astrophysics Data System (ADS)

Leij, Feike J.; Bradford, Scott A.

2013-07-01

It has been widely reported that colloids can travel faster and over longer distances in natural structured porous media than in uniform structureless media used in laboratory studies. The presence of preferential pathways for colloids in the subsurface environment is of concern because of the increased risks for disease caused by microorganisms and colloid-associated contaminants. This study presents a model for colloid transport in dual-permeability media that includes reversible and irreversible retention of colloids and first-order exchange between the aqueous phases of the two regions. The model may also be used to describe transport of other reactive solutes in dual-permeability media. Analytical solutions for colloid concentrations in aqueous and solid phases were obtained using Laplace transformation and matrix decomposition. The solutions proved convenient to assess the effect of model parameters on the colloid distribution. The analytical model was used to describe effluent concentrations for a bromide tracer and 3.2- or 1-μm-colloids that were observed after transport through a composite 10-cm long porous medium made up of a cylindrical lens or core of sand and a surrounding matrix with sand of a different grain size. The tracer data were described very well and realistic estimates were obtained for the pore-water velocity in the two flow domains. An accurate description was also achieved for most colloid breakthrough curves. Dispersivity and retention parameters were typically greater for the larger 3.2-μm-colloids while both reversible and irreversible retention rates tended to be higher for the finer sands than the coarser sand. The relatively small sample size and the complex flow pattern in the composite medium made it difficult to reach definitive conclusions regarding transport parameters for colloid transport.

Remediating munitions-contaminated soil with zerovalent iron and cationic surfactants.

PubMed

Park, J; Comfort, S D; Shea, P J; Machacek, T A

2004-01-01

Soils contaminated from military operations often contain mixtures of HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine), RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine), and TNT (2,4,6-trinitrotoluene) rather than a single explosive. Differences among explosives in solubility and reactivity make developing a single remediation treatment difficult. When Fe(0) was used to treat a munitions-contaminated soil, we observed high rates of destruction for RDX and TNT (98%) but not HMX. Our objective was to determine if HMX destruction by Fe(0) could be enhanced by increasing HMX solubility by physical (temperature) or chemical (surfactants) means. To determine electron acceptor preference, we treated RDX and HMX with Fe(0) in homogeneous solutions and binary mixtures. Increasing aqueous temperature (20 to 55 degrees C) increased HMX solubility (2 to 22 mg L(-1)) but did not increase destruction by Fe(0) in a contaminated soil slurry that also contained RDX and TNT. Batch experiments using equal molar concentrations of RDX and HMX demonstrated that RDX was preferentially reduced over HMX by Fe(0). By testing various surfactants, we found that the cationic surfactants (HDTMA [hexadecyltrimethylammonium bromide], didecyl, and didodecyl) were most effective in increasing HMX concentration in solution. Didecyl and HDTMA were also found to be highly effective in facilitating the transformation of HMX by Fe(0). Using HDTMA or didecyl solutions (3%, w/v) containing solid-phase HMX, we observed that 100% of the added HMX was transformed by Fe(0) in the didecyl matrix and 60% in the HDTMA matrix. These results indicate that cationic surfactants can increase HMX solubility and facilitate Fe(0)-mediated transformation kinetics but HMX destruction rates will be slowed when RDX is present.

Mechanism of Combustion of Heterogeneous Solid Propellants

DTIC Science & Technology

1998-09-01

This suggests that under these conditions the matrix outflow is essentially premixed at the LLEF standoff height and premixed canopy flames (Figs. 4a...graphs like that in Fig. 5 are not available (or economically obtainable) for all the combinations of possible interest (O/F ratio, size of fine AP...HNIW matrix and the AP/matrix/AP sandwiches were essentially the same, suggesting that the matrix controlled the rate. In contrast, the rate of the

Transport properties in dilute UN (X ) solid solutions (X =Xe ,Kr )

NASA Astrophysics Data System (ADS)

Claisse, Antoine; Schuler, Thomas; Lopes, Denise Adorno; Olsson, Pär

2016-11-01

Uranium nitride (UN) is a candidate fuel for current GEN III fission reactors, for which it is investigated as an accident-tolerant fuel, as well as for future GEN IV reactors. In this study, we investigate the kinetic properties of gas fission products (Xe and Kr) in UN. Binding and migration energies are obtained using density functional theory, with an added Hubbard correlation to model f electrons, and the occupation matrix control scheme to avoid metastable states. These energies are then used as input for the self-consistent mean field method which enables to determine transport coefficients for vacancy-mediated diffusion of Xe and Kr on the U sublattice. The magnetic ordering of the UN structure is explicitly taken into account, for both energetic and transport properties. Solute diffusivities are compared with experimental measurements and the effect of various parameters on the theoretical model is carefully investigated. We find that kinetic correlations are very strong in this system, and that despite atomic migration anisotropy, macroscopic solute diffusivities show limited anisotropy. Our model indicates that the discrepancy between experimental measurements probably results from different irradiation conditions, and hence different defect concentrations.

Impact of silk biomaterial structure on proteolysis.

PubMed

Brown, Joseph; Lu, Chia-Li; Coburn, Jeannine; Kaplan, David L

2015-01-01

The goal of this study was to determine the impact of silk biomaterial structure (e.g. solution, hydrogel, film) on proteolytic susceptibility. In vitro enzymatic degradation of silk fibroin hydrogels and films was studied using a variety of proteases, including proteinase K, protease XIV, α-chymotrypsin, collagenase, matrix metalloproteinase-1 (MMP-1) and MMP-2. Hydrogels were used to assess bulk degradation while films were used to assess surface degradation. Weight loss, secondary structure determined by Fourier transform infrared spectroscopy and degradation products analyzed via sodium dodecyl sulfate-polyacrylamide gel electrophoresis were used to evaluate degradation over 5 days. Silk films were significantly degraded by proteinase K, while silk hydrogels were degraded more extensively by protease XIV and proteinase K. Collagenase preferentially degraded the β-sheet content in hydrogels while protease XIV and α-chymotrypsin degraded the amorphous structures. MMP-1 and MMP-2 degraded silk fibroin in solution, resulting in a decrease in peptide fragment sizes over time. The link between primary sequence mapping with protease susceptibility provides insight into the role of secondary structure in impacting proteolytic access by comparing solution vs. solid state proteolytic susceptibility. Copyright © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Determination of 10 sulfonamide residues in meat samples by liquid chromatography with ultraviolet detection.

PubMed

Di Sabatino, Marcello; Di Pietra, Anna Maria; Benfenati, Luigi; Di Simone, Bruno

2007-01-01

A liquid chromatography (LC) method is described for the simultaneous determination of 10 commonly used sulfonamide drug residues in meat. The 10 sulfonamide drugs of interest were sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamethizole, sulfamonomethoxine, sulfachloropyridazine, sulfadoxine, sulfadimethoxine, and sulfaquinoxaline. The residues were extracted with acetone-chloroform (1 + 1). Sulfonamides were quantitatively retained in the extracting solution and afterwards eluted from a cation-exchanger solid-phase extraction cartridge with a solution of methanol-aqueous ammonia. The solution was dried, reconstituted with 5 mL methanol and filtered before analysis by LC-ultraviolet using a C18 column with a mobile phase gradient of potassium dihydrogen phosphate buffer, pH 2.5, and methanol-acetonitrile (30 + 70, v/v). The method was applied to cattle, swine, chicken, and sheep muscle tissues. The validation was performed with a fortified cattle meat sample at level of 100 ppb, which is the administrative maximum residue limit for sulfonamides in the European Union. The limit of quantitation for all sulfonamides was between 3 and 14 ppb. Recovery was evaluated for different meat matrixes. The mean recovery values were between 66.3% for pork meat samples and 71.5% for cattle meat samples.

Thermosensitive chitosan/glycerophosphate-based hydrogel and its derivatives in pharmaceutical and biomedical applications.

PubMed

Supper, Stephanie; Anton, Nicolas; Seidel, Nina; Riemenschnitter, Marc; Curdy, Catherine; Vandamme, Thierry

2014-02-01

Thermogelling chitosan (CS)/glycerophosphate (GP) solutions have been reported as a new type of parenteral in situ forming depot system. These free-flowing solutions at ambient temperature turn into semi-solid hydrogels after parenteral administration. Formulation parameters such as CS physico-chemical characteristics, CS/gelling agent ratio or pH of the system, were acknowledged as key parameters affecting the solution stability, the sol/gel transition behavior and/or the final hydrogel structure. We discuss also the use of the standard CS/GP thermogels for various biomedical applications, including drug delivery and tissue engineering. Furthermore, this manuscript reviews the different strategies implemented to improve the hydrogel characteristics such as combination with carrier particles, replacement of GP, addition of a second polymer and chemical modification of CS. The recent advances in the formulation of CS-based thermogelling systems already overcame several challenges faced by the standard CS/GP system. Dispersion of drug-loaded carrier particles into the thermogels allowed achieving prolonged release profiles for low molecular weight drugs; incorporation of an additional polymer enabled to strengthen the network, while the use of chemically modified CS led to enhanced pH sensitivity or biodegradability of the matrix.

Eutectics as improved pharmaceutical materials: design, properties and characterization.

PubMed

Cherukuvada, Suryanarayan; Nangia, Ashwini

2014-01-28

Eutectics are a long known class of multi-component solids with important and useful applications in daily life. In comparison to other multi-component crystalline solids, such as salts, solid solutions, molecular complexes and cocrystals, eutectics are less studied in terms of molecular structure organization and bonding interactions. Classically, a eutectic is defined based on its low melting point compared to the individual components. In this article, we attempt to define eutectics not just based on thermal methods but from a structural organization view point, and discuss their microstructures and properties as organic materials vis-a-vis solid solutions and cocrystals. The X-ray crystal structure of a cocrystal is different from that of the individual components whereas the unit cell of a solid solution is similar to that of one of the components. Eutectics are closer to the latter species in that their crystalline arrangement is similar to the parent components but they are different with respect to the structural integrity. A solid solution possesses structural homogeneity throughout the structure (single phase) but a eutectic is a heterogeneous ensemble of individual components whose crystal structures are like discontinuous solid solutions (phase separated). Thus, a eutectic may be better defined as a conglomerate of solid solutions. A structural analysis of cocrystals, solid solutions and eutectics has led to an understanding that materials with strong adhesive (hetero) interactions between the unlike components will lead to cocrystals whereas those having stronger cohesive (homo/self) interactions will more often give rise to solid solutions (for similar structures of components) and eutectics (for different structures of components). We demonstrate that the same crystal engineering principles which have been profitably utilized for cocrystal design in the past decade can now be applied to make eutectics as novel composite materials, illustrated by stable eutectics of the hygroscopic salt of the anti-tuberculosis drug ethambutol as a case study. A current gap in the characterization of eutectic microstructure may be fulfilled through pair distribution function (PDF) analysis of X-ray diffraction data, which could be a rapid signature technique to differentiate eutectics from their components.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garn, Troy G; Law, Jack D; Greenhalgh, Mitchell R

A composite media including at least one crystalline aluminosilicate material in polyacrylonitrile. A method of forming a composite media is also disclosed. The method comprises dissolving polyacrylonitrile in an organic solvent to form a matrix solution. At least one crystalline aluminosilicate material is combined with the matrix solution to form a composite media solution. The organic solvent present in the composite media solution is diluted. The composite media solution is solidified. In addition, a method of processing a fluid stream is disclosed. The method comprises providing a beads of a composite media comprising at least one crystalline aluminosilicate material dispersedmore » in a polyacrylonitrile matrix. The beads of the composite media are contacted with a fluid stream comprising at least one constituent. The at least one constituent is substantially removed from the fluid stream.« less

Solution and solid trinitrotoluene (TNT) photochemistry: persistence of TNT-like ultraviolet (UV) resonance Raman bands.

PubMed

Gares, Katie L; Bykov, Sergei V; Godugu, Bhaskar; Asher, Sanford A

2014-01-01

We examined the 229 nm deep-ultraviolet resonance Raman (DUVRR) spectra of solution and solid-state trinitrotoluene (TNT) and its solution and solid-state photochemistry. Although TNT photodegrades with a solution quantum yield of ϕ ∼ 0.015, the initial photoproducts show DUVRR spectra extraordinarily similar to pure TNT, due to the similar photoproduct enhancement of the -NO2 stretching vibrations. This results in TNT-like DUVRR spectra even after complete TNT photolysis. These ultraviolet resonance Raman spectral bands enable DUVRR of trace as well as DUVRR standoff TNT detection. We determined the structure of various initial TNT photoproducts by using liquid chromatography-mass spectrometry and tandem mass spectrometry. Similar TNT DUVRR spectra and photoproducts are observed in the solution and solid states.

Tritium containing polymers having a polymer backbone substantially void of tritium

DOEpatents

Jensen, G.A.; Nelson, D.A.; Molton, P.M.

1992-03-31

A radioluminescent light source comprises a solid mixture of a phosphorescent substance and a tritiated polymer. The solid mixture forms a solid mass having length, width, and thickness dimensions, and is capable of self-support. In one aspect of the invention, the phosphorescent substance comprises solid phosphor particles supported or surrounded within a solid matrix by a tritium containing polymer. The tritium containing polymer comprises a polymer backbone which is essentially void of tritium. 2 figs.

Tritium containing polymers having a polymer backbone substantially void of tritium

DOEpatents

Jensen, George A.; Nelson, David A.; Molton, Peter M.

1992-01-01

A radioluminescent light source comprises a solid mixture of a phosphorescent substance and a tritiated polymer. The solid mixture forms a solid mass having length, width, and thickness dimensions, and is capable of self-support. In one aspect of the invention, the phosphorescent substance comprises solid phosphor particles supported or surrounded within a solid matrix by a tritium containing polymer. The tritium containing polymer comprises a polymer backbone which is essentially void of tritium.

NEUTRALIZATIONS OF HIGH ALUMINUM LOW URANIUM USED NUCLEAR FUEL SOLUTIONS CONTAINING GADOLINIUM AS A NEUTRON POISON

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taylor-Pashow, K.

2011-06-08

H-Canyon will begin dissolving High Aluminum - Low Uranium (High Al/Low U) Used Nuclear Fuel (UNF) following approval by DOE which is anticipated in CY2011. High Al/Low U is an aluminum/enriched uranium UNF with small quantities of uranium relative to aluminum. The maximum enrichment level expected is 93% {sup 235}U. The High Al/Low U UNF will be dissolved in H-Canyon in a nitric acid/mercury/gadolinium solution. The resulting solution will be neutralized and transferred to Tank 39H in the Tank Farm. To confirm that the solution generated could be poisoned with Gd, neutralized, and discarded to the Savannah River Site (SRS)more » high level waste (HLW) system without undue nuclear safety concerns the caustic precipitation of simulant solutions was examined. Experiments were performed with three simulant solutions representative of the H-Canyon estimated concentrations in the final solutions after dissolution. The maximum U, Gd, and Al concentration were selected for testing from the range of solution compositions provided. Simulants were prepared in three different nitric acid concentrations, ranging from 0.5 to 1.5 M. The simulant solutions were neutralized to four different endpoints: (1) just before a solid phase was formed (pH 3.5-4), (2) the point where a solid phase was obtained, (3) 0.8 M free hydroxide, and (4) 1.2 M free hydroxide, using 50 wt % sodium hydroxide (NaOH). The settling behavior of the neutralized solutions was found to be slower compared to previous studies, with settling continuing over a one week period. Due to the high concentration of Al in these solutions, precipitation of solids was observed immediately upon addition of NaOH. Precipitation continued as additional NaOH was added, reaching a point where the mixture becomes almost completely solid due to the large amount of precipitate. As additional NaOH was added, some of the precipitate began to redissolve, and the solutions neutralized to the final two endpoints mixed easily and had expected densities of typical neutralized waste. Based on particle size and scanning electron microscopy analyses, the neutralized solids were found to be homogeneous and less than 20 microns in size. The majority of solids were less than 4 microns in size. Compared to previous studies, a larger percentage of the Gd was found to precipitate in the partially neutralized solutions (at pH 3.5-4). In addition the Gd:U mass ratio was found to be at least 1.0 in all of the solids obtained after partial or full neutralization. The hydrogen to U (H:U) molar ratios for two accident scenarios were also determined. The first was for transient neutralization and agitator failure. Experimentally this scenario was determined by measuring the H:U ratio of the settled solids. The minimum H:U molar ratio for solids from fully neutralized solutions was 388:1. The second accident scenario is for the solids drying out in an unagitiated pump box. Experimentally, this scenario was determined by measuring the H:U molar ratio in centrifuged solids. The minimum H:U atom ratios for centrifuged precipitated solids was 250:1. It was determined previously that a 30:1 H:Pu atom ratio was sufficient for a 1:1 Gd:Pu mass ratio. Assuming a 1:1 equivalence with {sup 239}Pu, the results of these experiments show Gd is a viable poison for neutralizing U/Gd solutions with the tested compositions.« less

Uranium chemistry in stack solutions and leachates of phosphogypsum disposed at a coastal area in Cyprus.

PubMed

Lysandrou, M; Pashalidis, I

2008-02-01

The effect of the matrix composition (main constituents) on the concentration and chemical behavior of uranium in phosphogypsum stack solutions and leachates has been investigated. Solid and aqueous samples were taken from three different sub-areas of a phosphogypsum stack at a coastal area in Vasilikos (Cyprus). The sub-areas are characterized whether by their acidity (e.g. "aged" and "non-aged" phosphogypsum) or by their salt content, originating from pulping water during wet stacking or (after deposition) from the adjacent sea. Measurements in stack solutions and leachates showed that phosphogypsum characteristics affect both, the concentration and the chemical behavior of uranium in solution. Uranium concentration in solutions of increased salinity is up to three orders of magnitude higher than in solutions of low salinity and this is attributed to the effect of ionic strength on the solubility of phosphogypsum. Modelling showed that uranium in stack solutions is predominantly present in the form of uranium(VI) phosphate complexes (e.g. UO(2)(H(2)PO(4))(2), UO(2)HPO(4)), whereas in leachates uranium(VI) fluoro complexes (e.g. UO(2)F(2), UO(2)F(3)(-)) are predominant in solution. The latter indicates that elution of uranium from phosphogypsum takes places most probably in the form of fluoro complexes. Both, effective elution by saline water and direct migration of uranium to the sea, where it forms very stable uranium(VI) carbonato complexes, indicate that the adjacent sea will be the final receptor of uranium released from Vasilikos phosphogypsum.

Recycling polyethylene terephthalate wastes as short fibers in Strain-Hardening Cementitious Composites (SHCC).

PubMed

Lin, Xiuyi; Yu, Jing; Li, Hedong; Lam, Jeffery Y K; Shih, Kaimin; Sham, Ivan M L; Leung, Christopher K Y

2018-05-26

As an important portion of the total plastic waste bulk but lack of reuse and recycling, the enormous amounts of polyethylene terephthalate (PET) solid wastes have led to serious environmental issues. This study explores the feasibility of recycling PET solid wastes as short fibers in Strain-Hardening Cementitious Composites (SHCCs), which exhibit strain-hardening and multiple cracking under tension, and therefore have clear advantages over conventional concrete for many construction applications. Based on micromechanical modeling, fiber dispersion and alkali resistance, the size of recycled PET fibers was first determined. Then the hydrophobic PET surface was treated with NaOH solution followed by a silane coupling agent to achieve the dual purpose of improving the fiber/matrix interfacial frictional bond (from 0.64 MPa to 0.80 MPa) and enhancing the alkali resistance for applications in alkaline cementitious environment. With surface treatment, recycling PET wastes as fibers in SHCCs is a promising approach to significantly reduce the material cost of SHCCs while disposing hazardous PET wastes in construction industry. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Tagiri-Endo, Misako; Suzuki, Shigeru; Nakamura, Tomoyuki; Hatakeyama, Takashi; Kawamukai, Kazuo

2009-02-01

A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 microl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01-0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.

Matrix Optical Absorption in UV-MALDI MS

NASA Astrophysics Data System (ADS)

Robinson, Kenneth N.; Steven, Rory T.; Bunch, Josephine

2018-03-01

In ultraviolet matrix-assisted laser desorption/ionization mass spectrometry (UV-MALDI MS) matrix compound optical absorption governs the uptake of laser energy, which in turn has a strong influence on experimental results. Despite this, quantitative absorption measurements are lacking for most matrix compounds. Furthermore, despite the use of UV-MALDI MS to detect a vast range of compounds, investigations into the effects of laser energy have been primarily restricted to single classes of analytes. We report the absolute solid state absorption spectra of the matrix compounds α-cyano-4-hydroxycinnamic acid (CHCA), para-nitroaniline (PNA), 2-mercaptobenzothiazole (MBT), 2,5-dihydroxybenzoic acid (2,5-DHB), and 2,4,6-trihydroxyacetophenone (THAP). The desorption/ionization characteristics of these matrix compounds with respect to laser fluence was investigated using mixed systems of matrix with either angiotensin II, PC(34:1) lipid standard, or haloperidol, acting as representatives for typical classes of analyte encountered in UV-MALDI MS. The first absolute solid phase spectra for PNA, MBT, and THAP are reported; additionally, inconsistencies between previously published spectra for CHCA are resolved. In light of these findings, suggestions are made for experimental optimization with regards to matrix and laser wavelength selection. The relationship between matrix optical cross-section and wavelength-dependant threshold fluence, fluence of maximum ion yield, and R, a new descriptor for the change in ion intensity with fluence, are described. A matrix cross-section of 1.3 × 10-17 cm-2 was identified as a potential minimum for desorption/ionization of analytes.

Matrix Optical Absorption in UV-MALDI MS.

PubMed

Robinson, Kenneth N; Steven, Rory T; Bunch, Josephine

2018-03-01

In ultraviolet matrix-assisted laser desorption/ionization mass spectrometry (UV-MALDI MS) matrix compound optical absorption governs the uptake of laser energy, which in turn has a strong influence on experimental results. Despite this, quantitative absorption measurements are lacking for most matrix compounds. Furthermore, despite the use of UV-MALDI MS to detect a vast range of compounds, investigations into the effects of laser energy have been primarily restricted to single classes of analytes. We report the absolute solid state absorption spectra of the matrix compounds α-cyano-4-hydroxycinnamic acid (CHCA), para-nitroaniline (PNA), 2-mercaptobenzothiazole (MBT), 2,5-dihydroxybenzoic acid (2,5-DHB), and 2,4,6-trihydroxyacetophenone (THAP). The desorption/ionization characteristics of these matrix compounds with respect to laser fluence was investigated using mixed systems of matrix with either angiotensin II, PC(34:1) lipid standard, or haloperidol, acting as representatives for typical classes of analyte encountered in UV-MALDI MS. The first absolute solid phase spectra for PNA, MBT, and THAP are reported; additionally, inconsistencies between previously published spectra for CHCA are resolved. In light of these findings, suggestions are made for experimental optimization with regards to matrix and laser wavelength selection. The relationship between matrix optical cross-section and wavelength-dependant threshold fluence, fluence of maximum ion yield, and R, a new descriptor for the change in ion intensity with fluence, are described. A matrix cross-section of 1.3 × 10 -17 cm -2 was identified as a potential minimum for desorption/ionization of analytes. Graphical Abstract ᅟ.

Effect of Degeneration on Fluid-Solid Interaction within Intervertebral Disk Under Cyclic Loading - A Meta-Model Analysis of Finite Element Simulations.

PubMed

Nikkhoo, Mohammad; Khalaf, Kinda; Kuo, Ya-Wen; Hsu, Yu-Chun; Haghpanahi, Mohammad; Parnianpour, Mohamad; Wang, Jaw-Lin

2015-01-01

The risk of low back pain resulted from cyclic loadings is greater than that resulted from prolonged static postures. Disk degeneration results in degradation of disk solid structures and decrease of water contents, which is caused by activation of matrix digestive enzymes. The mechanical responses resulted from internal solid-fluid interactions of degenerative disks to cyclic loadings are not well studied yet. The fluid-solid interactions in disks can be evaluated by mathematical models, especially the poroelastic finite element (FE) models. We developed a robust disk poroelastic FE model to analyze the effect of degeneration on solid-fluid interactions within disk subjected to cyclic loadings at different loading frequencies. A backward analysis combined with in vitro experiments was used to find the elastic modulus and hydraulic permeability of intact and enzyme-induced degenerated porcine disks. The results showed that the averaged peak-to-peak disk deformations during the in vitro cyclic tests were well fitted with limited FE simulations and a quadratic response surface regression for both disk groups. The results showed that higher loading frequency increased the intradiscal pressure, decreased the total fluid loss, and slightly increased the maximum axial stress within solid matrix. Enzyme-induced degeneration decreased the intradiscal pressure and total fluid loss, and barely changed the maximum axial stress within solid matrix. The increase of intradiscal pressure and total fluid loss with loading frequency was less sensitive after the frequency elevated to 0.1 Hz for the enzyme-induced degenerated disk. Based on this study, it is found that enzyme-induced degeneration decreases energy attenuation capability of disk, but less change the strength of disk.

Use of the maximum entropy method to retrieve the vertical atmospheric ozone profile and predict atmospheric ozone content

NASA Technical Reports Server (NTRS)

Turner, B. Curtis

1992-01-01

A method is developed for prediction of ozone levels in planetary atmospheres. This method is formulated in terms of error covariance matrices, and is associated with both direct measurements, a priori first guess profiles, and a weighting function matrix. This is described by the following linearized equation: y = A(matrix) x X + eta, where A is the weighting matrix and eta is noise. The problems to this approach are: (1) the A matrix is near singularity; (2) the number of unknowns in the profile exceeds the number of data points, therefore, the solution may not be unique; and (3) even if a unique solution exists, eta may cause the solution to be ill conditioned.

Reducing Actinide Production Using Inert Matrix Fuels

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deinert, Mark

2017-08-23

The environmental and geopolitical problems that surround nuclear power stem largely from the longlived transuranic isotopes of Am, Cm, Np and Pu that are contained in spent nuclear fuel. New methods for transmuting these elements into more benign forms are needed. Current research efforts focus largely on the development of fast burner reactors, because it has been shown that they could dramatically reduce the accumulation of transuranics. However, despite five decades of effort, fast reactors have yet to achieve industrial viability. A critical limitation to this, and other such strategies, is that they require a type of spent fuel reprocessingmore » that can efficiently separate all of the transuranics from the fission products with which they are mixed. Unfortunately, the technology for doing this on an industrial scale is still in development. In this project, we explore a strategy for transmutation that can be deployed using existing, current generation reactors and reprocessing systems. We show that use of an inert matrix fuel to recycle transuranics in a conventional pressurized water reactor could reduce overall production of these materials by an amount that is similar to what is achievable using proposed fast reactor cycles. Furthermore, we show that these transuranic reductions can be achieved even if the fission products are carried into the inert matrix fuel along with the transuranics, bypassing the critical separations hurdle described above. The implications of these findings are significant, because they imply that inert matrix fuel could be made directly from the material streams produced by the commercially available PUREX process. Zirconium dioxide would be an ideal choice of inert matrix in this context because it is known to form a stable solid solution with both fission products and transuranics.« less

Fabrication and characterization of microstructure of stainless steel matrix composites containing up to 25 vol% NbC

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kan, Wen Hao, E-mail: wkan6795@uni.sydney.edu.au

AISI 440 stainless steels reinforced with various volume fractions of niobium carbide (NbC) particles of up to 25 vol% were fabricated in-situ using an argon arc furnace and then heat-treated to produce a martensitic matrix. Optical and scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and electron back-scatter diffraction (EBSD) techniques were used to analyze the microstructure, phases and composition of these composites. Interestingly, it was found that Chinese-script NbC could nucleate on existing primary NbC particles creating NbC clusters with complex microstructures. Additionally, hardness tests were used to evaluate viability in mining and mineral processing applications. The increasemore » in NbC content resulted in an overall increase in the hardness of the composites while causing a marginal decrease in the amount of Cr in solid solution with the matrix, which could be a concern for corrosion resistance. The latter was due to the fact that the NbC lattice could dissolve a minor amount of Cr. Thermodynamic simulations also attributed this to a slight increase in M{sub 7}C{sub 3} precipitation. Nonetheless, these novel composites show great promise for applications in wear and corrosive environments. - Highlights: •Stainless steels reinforced with NbC particles of up to 25 vol% were fabricated. •NbC was formed in-situ in the steels using an arc melter. •Martensitic transformation of the matrix of each sample was achieved. •NbC reinforcements increased the bulk hardness values of the steels. •Dissolved Cr in the matrix of each sample was sufficient for passivity in theory.« less

Ammonium nitrate-polymer glasses: a new concept for phase and thermal stabilization of ammonium nitrate.

PubMed

Lang, Anthony J; Vyazovkin, Sergey

2008-09-11

Dissolving of ammonium nitrate in highly polar polymers such as poly(vinylpyrrolidone) and/or poly(acrylamide) can result in the formation of single-phase glassy solid materials, in which NH 4 (+) and NO 3 (-) are separated through an ion-dipole interaction with the polymer matrix. Below the glass transition temperature of the polymer matrix the resulting materials remain phase and thermally stable as demonstrated through the absence of decomposition as well as the solid-solid transitions and melting of ammonium nitrate. The structure of the materials is explored by Fourier transform infrared spectroscopy and density functional calculations. Differential scanning calorimetry, thermogravimetry, and isoconversional kinetic analysis are applied to characterize the thermal behavior of the materials.

Rapid Detection and Identification of Candidemia by Direct Blood Culturing on Solid Medium by Use of Lysis-Centrifugation Method Combined with Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry (MALDI-TOF MS).

PubMed

Idelevich, Evgeny A; Grünastel, Barbara; Becker, Karsten

2017-01-01

Candida sepsis is a life-threatening condition with increasing prevalence. In this study, direct blood culturing on solid medium using a lysis-centrifugation procedure enabled successful Candida species identification by matrix-assisted laser desorption-ionization time of flight mass spectrometry on average 3.8 h (Sabouraud agar) or 7.4 h (chocolate agar) before the positivity signal for control samples in Bactec mycosis-IC/F or Bactec Plus aerobic/F bottles, respectively. Direct culturing on solid medium accelerated candidemia diagnostics compared to that with automated broth-based systems. Copyright © 2016 American Society for Microbiology.

Heterogeneous fuel for hybrid rocket

NASA Technical Reports Server (NTRS)

Stickler, David B. (Inventor)

1996-01-01

Heterogeneous fuel compositions suitable for use in hybrid rocket engines and solid-fuel ramjet engines, The compositions include mixtures of a continuous phase, which forms a solid matrix, and a dispersed phase permanently distributed therein. The dispersed phase or the matrix vaporizes (or melts) and disperses into the gas flow much more rapidly than the other, creating depressions, voids and bumps within and on the surface of the remaining bulk material that continuously roughen its surface, This effect substantially enhances heat transfer from the combusting gas flow to the fuel surface, producing a correspondingly high burning rate, The dispersed phase may include solid particles, entrained liquid droplets, or gas-phase voids having dimensions roughly similar to the displacement scale height of the gas-flow boundary layer generated during combustion.

Process for recovering pertechnetate ions from an aqueous solution also containing other ions

DOEpatents

Rogers, Robin; Horwitz, E. Philip; Bond, Andrew H.

1997-01-01

A solid/liquid process for the separation and recovery of TcO.sub.4.sup.-1 ions from an aqueous solution is disclosed. The solid support comprises separation particles having surface-bonded poly(ethylene glycol) groups; whereas the aqueous solution from which the TcO.sub.4.sup.-1 ions are separated contains a poly(ethylene glycol) liquid/liquid biphase-forming amount of a dissolved salt. A solid/liquid phase admixture of separation particles containing bound TcO.sub.4.sup.-1 ions in such an aqueous solution that is free from MoO.sub.4.sup.-2 ions is also contemplated, as is a chromatography apparatus containing that solid/liquid phase admixture.

Comparison of Heat Inactivation and Cell Disruption Protocols for Identification of Mycobacteria from Solid Culture Media by Use of Vitek Matrix-Assisted Laser Desorption Ionization–Time of Flight Mass Spectrometry

PubMed Central

Machen, Alexandra; Kobayashi, Miwako; Connelly, Mary Robin

2013-01-01

Two novel protocols for inactivation and extraction were developed and used to identify 107 Mycobacterium clinical isolates, including Mycobacterium tuberculosis complex, from solid cultures using Vitek matrix-assisted laser desorption ionization–time of flight (MALDI-TOF) mass spectrometry. The protocol using heat inactivation with sonication and cell disruption with glass beads resulted in 82.2% and 88.8% species and genus level identifications, respectively. PMID:24068013

Optimization of microfabricated nanoliter-scale solid-phase extraction device for detection of gel-separated proteins in low abundance by matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Chen, Wenzhang; Shen, Jing; Yin, Xuefeng; Yu, Yingnian

2007-01-01

A nano-scale solid-phase extraction (SPE) device was developed for the detection of gel-separated proteins in low abundance by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) with a simplified microfabrication technology. By using SU-8 photoresist instead of epoxy glue to connect the microchannel and transfer capillary, polymeric contaminant signals in MS analysis were significantly reduced. Micro SPE columns with different capacities and geometric characteristics were investigated in order to increase the detection sensitivity and decrease spot size for MALDI-TOF-MS analysis. It is shown that enhancements in sensitivities for the detection of proteins in low abundance were correlated with the reduction in column capacity and increase in column aspect ratio. Fifty nanoliters of matrix solution were sufficient to elute the sample completely from the optimized micro SPE column with 3.5 nL capacity. The mass spectrum of a 5 fmol in-gel tryptic digest of bovine serum albumin (BSA), processed by the micro SPE column, demonstrated that 29 peptides matched the protein giving a sequence coverage of 51%, which was better than that obtained from analysis of 25 fmol of the same sample prepared by the dried-droplet method. With the micro SPE column treatment of 2 microL of digestion supernatant of a gel spot of the IQGAP1 protein, 15 peptides were detected from the mass spectrum with the highest individual score of 111, while, with a ZipTip procedure, only nine peaks were detected with the highest individual score of 71. Analytical results demonstrated that this approach greatly improved the sequence coverage and identification specificity for the tested protein. It can serve as a very useful tool in proteomics studies, especially for low abundance proteins. Copyright (c) 2006 John Wiley & Sons, Ltd.

LEACHING OF TITANIUM FROM MONOSODIUM TITANATE AND MODIFIED MST

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taylor-Pashow, K.; Fondeur, F.; Fink, S.

2012-08-01

Analysis of a fouled coalescer and pre-filters from Actinide Removal Process/Modular Caustic Side Solvent Extraction Unit (ARP/MCU) operations showed evidence of Ti containing solids. Based on these results a series of tests were planned to examine the extent of Ti leaching from monosodium titanate (MST) and modified monosodium titanate (mMST) in various solutions. The solutions tested included a series of salt solutions with varying free hydroxide concentrations, two sodium hydroxide concentrations, 9 wt % and 15 wt %, nitric and oxalic acid solutions. Overall, the amount of Ti leached from the MST and mMST was much greater in the acidmore » solutions compared to the sodium hydroxide or salt solutions, which is consistent with the expected trend. The leaching data also showed that increasing hydroxide concentration, whether pure NaOH solution used for filter cleaning in ARP or the waste salt solution, increased the amount of Ti leached from both the MST and mMST. For the respective nominal contact times with the MST solids - for filter cleaning or the normal filter operation, the dissolved Ti concentrations are comparable suggesting either cause may contribute to the increased Ti fouling on the MCU coalescers. Tests showed that Ti containing solids could be precipitated from solution after the addition of scrub acid and a decrease in temperature similar to expected in MCU operations. FTIR analysis of these solids showed some similarity to the solids observed on the fouled coalescer and pre-filters. Although only a cursory study, this information suggests that the practice of increasing free hydroxide in feed solutions to MCU as a mitigation to aluminosilicate formation may be offset by the impact of formation of Ti solids in the overall process. Additional consideration of this finding from MCU and SWPF operation is warranted.« less

Electrochromic nanocomposite films

DOEpatents

Milliron, Delia; Llordes, Anna; Buonsanti, Raffaella; Garcia, Guillermo

2018-04-10

The present invention provides an electrochromic nanocomposite film. In an exemplary embodiment, the electrochromic nanocomposite film, includes (1) a solid matrix of oxide based material and (2) transparent conducting oxide (TCO) nanostructures embedded in the matrix. In a further embodiment, the electrochromic nanocomposite film farther includes a substrate upon which the matrix is deposited. The present invention also provides a method of preparing an electrochromic nanocomposite film.

Method of waste stabilization with dewatered chemically bonded phosphate ceramics

DOEpatents

Wagh, Arun; Maloney, Martin D.

2010-06-29

A method of stabilizing a waste in a chemically bonded phosphate ceramic (CBPC). The method consists of preparing a slurry including the waste, water, an oxide binder, and a phosphate binder. The slurry is then allowed to cure to a solid, hydrated CBPC matrix. Next, bound water within the solid, hydrated CBPC matrix is removed. Typically, the bound water is removed by applying heat to the cured CBPC matrix. Preferably, the quantity of heat applied to the cured CBPC matrix is sufficient to drive off water bound within the hydrated CBPC matrix, but not to volatalize other non-water components of the matrix, such as metals and radioactive components. Typically, a temperature range of between 100.degree. C.-200.degree. C. will be sufficient. In another embodiment of the invention wherein the waste and water have been mixed prior to the preparation of the slurry, a select amount of water may be evaporated from the waste and water mixture prior to preparation of the slurry. Another aspect of the invention is a direct anyhydrous CBPC fabrication method wherein water is removed from the slurry by heating and mixing the slurry while allowing the slurry to cure. Additional aspects of the invention are ceramic matrix waste forms prepared by the methods disclosed above.

Preparation and physical properties of (PVA)0.7(NaBr)0.3(H3PO4)xM solid acid membrane for phosphoric acid – Fuel cells

PubMed Central

Ahmad, F.; Sheha, E.

2012-01-01

A solid acid membranes based on poly (vinyl alcohol) (PVA), sodium bromide (NaBr) and phosphoric acid (H3PO4) were prepared by a solution casting method. The morphological, IR, electrical and optical properties of the (PVA)0.7(NaBr)0.3(H3PO4)xM solid acid membranes where x = 0.00, 0.85, 1.7, 3.4, 5.1 M were investigated. The variation of film morphology was examined by scanning electron microscopy (SEM) studies. FTIR spectroscopy has been used to characterize the structure of polymer and confirms the complexation of phosphoric acid with host polymeric matrix. The temperature dependent nature of ionic conductivity and the impedance of the polymer electrolytes were determined along with the associated activation energy. The ionic conductivity at room temperature was found to be strongly depends on the H3PO4 concentration which it has been achieved to be of the order 4.3 × 10−3 S/cm at ambient temperature. Optical measurements showed a decrease in optical band gap and an increase in band tail width with the increase of phosphoric acid. The data shows that the (PVA)0.7(NaBr)0.3(H3PO4)xM solid acid membrane is promising for intermediate temperature phosphoric acid fuel cell applications. PMID:25685413

Innovative design and material solutions of thermal contact layers for high heat flux applications in fusion devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Federici, G.; Matera, R.; Chiocchio, S.

1994-11-01

One difficulty associated with the design and development of sacrificial plasma facing components that have to handle the high heat and particle fluxes in ITER is achieving the necessary contact conductance between the plasma protection material and the high-conductivity substrate in contact with the coolant. This paper presents a novel bond idea which is proposed as one of the options for the sacrificial energy dump targets located at the bottom of the divertor legs. The bonded joint in this design concept provides thermal and electrical contact between the armour and the cooled sub-structure while promoting remote, in-situ maintenance repair andmore » an easy replaceability of the armour part without disturbing the cooling pipes or rewelding neutron irradiated materials. To provide reliable and demountable adhesion, the bond consists of a metal alloy, treated in the semi-solid phase so that it leads to a fine dispersion of a globular solid phase into a liquid matrix (rheocast process). This thermal bond layer would normally operate in the solid state but could be brought reversibly to the semi-solid state during the armour replacement simply by heating it slightly above its solidus temperature. Material and design options are discussed in this paper. Possible methods of installation and removal are described, and lifetime considerations are addressed. In order to validate this concept within the ITER time-frame, a R&D programme must be rapidly implemented.« less

Solid lithium ion conducting electrolytes and methods of preparation

DOEpatents

Narula, Chaitanya K; Daniel, Claus

2013-05-28

A composition comprised of nanoparticles of lithium ion conducting solid oxide material, wherein the solid oxide material is comprised of lithium ions, and at least one type of metal ion selected from pentavalent metal ions and trivalent lanthanide metal ions. Solution methods useful for synthesizing these solid oxide materials, as well as precursor solutions and components thereof, are also described. The solid oxide materials are incorporated as electrolytes into lithium ion batteries.

Solid lithium ion conducting electrolytes and methods of preparation

DOEpatents

Narula, Chaitanya K.; Daniel, Claus

2015-11-19

A composition comprised of nanoparticles of lithium ion conducting solid oxide material, wherein the solid oxide material is comprised of lithium ions, and at least one type of metal ion selected from pentavalent metal ions and trivalent lanthanide metal ions. Solution methods useful for synthesizing these solid oxide materials, as well as precursor solutions and components thereof, are also described. The solid oxide materials are incorporated as electrolytes into lithium ion batteries.

INTERNATIONAL CONFERENCE ON SEMICONDUCTOR INJECTION LASERS SELCO-87: Simple formula for the thermal conductivity of a quaternary solid solution

NASA Astrophysics Data System (ADS)

Nakwaski, W.

1988-11-01

An analysis is made of the thermal conductivity of quaternary solid solutions (alloys) allowing for their disordered structure on the basis of a phenomenological analysis proposed by Abeles. This method is applied to a quaternary solid solution In1 - xGaxAsyP1 - y. A simple analytic expression is derived for the thermal conductivity of this material.

Lattice Parameter Behavior with Different Nd and O Concentrations in (U 1-yNd y)O 2±x Solid Solution

DOE PAGES

Lee, Seung Min; Knight, Travis W.; Voit, Stwart L.; ...

2016-02-02

The solid solution of (U1-yFPy)O- 2±x, has the same fluorite structure as UO 2±x lambda, and the lattice parameter is affected by dissolved fission product and oxygen concentrations. We investigated the relation between the lattice parameter and the concentrations of neodymium and oxygen in the fluorite structure of (U 1-yNd y)O 2±x using X-ray diffraction. Moreover, the lattice parameter behavior in the (U 1-yNd y)O 2±x, solid solution shows a linear change as a function of the oxygen-to-metal ratio and solubility of neodymium. The lattice parameter depends on the radii of ions forming the fluorite structure and also can bemore » expressed by a particular rule (modified Vegard's law). Furthermore, the numerical analyses of the lattice parameters for the stoichiometric and nonstoichionietric solid solutions were conducted, and the lattice parameter model for the (U1-yNdy)O 2±x, solid solution was assessed. There is a very linear relationship between the lattice parameter and the Nd and O concentration for the stoichiometry and nonstoichiometry of the (U 1-yNd y)O 2±x solid solution was verified.« less

Revisiting HgCl 2: A solution- and solid-state 199Hg NMR and ZORA-DFT computational study

NASA Astrophysics Data System (ADS)

Taylor, R. E.; Carver, Colin T.; Larsen, Ross E.; Dmitrenko, Olga; Bai, Shi; Dybowski, C.

2009-07-01

The 199Hg chemical-shift tensor of solid HgCl 2 was determined from spectra of polycrystalline materials, using static and magic-angle spinning (MAS) techniques at multiple spinning frequencies and field strengths. The chemical-shift tensor of solid HgCl 2 is axially symmetric ( η = 0) within experimental error. The 199Hg chemical-shift anisotropy (CSA) of HgCl 2 in a frozen solution in dimethylsulfoxide (DMSO) is significantly smaller than that of the solid, implying that the local electronic structure in the solid is different from that of the material in solution. The experimental chemical-shift results (solution and solid state) are compared with those predicted by density functional theory (DFT) calculations using the zeroth-order regular approximation (ZORA) to account for relativistic effects. 199Hg spin-lattice relaxation of HgCl 2 dissolved in DMSO is dominated by a CSA mechanism, but a second contribution to relaxation arises from ligand exchange. Relaxation in the solid state is independent of temperature, suggesting relaxation by paramagnetic impurities or defects.

Making molecular balloons in laser-induced explosive boiling of polymer solutions.

PubMed

Leveugle, Elodie; Sellinger, Aaron; Fitz-Gerald, James M; Zhigilei, Leonid V

2007-05-25

The effect of the dynamic molecular rearrangements leading to compositional segregation is revealed in coarse-grained molecular dynamics simulations of short pulse laser interaction with a polymer solution in a volatile matrix. An internal release of matrix vapor at the onset of the explosive boiling of the overheated liquid is capable of pushing polymer molecules to the outskirts of a transient bubble, forming a polymer-rich surface layer enclosing the volatile matrix material. The results explain unexpected "deflated balloon" structures observed in films deposited by the matrix-assisted pulsed laser evaporation technique.

Magnetism and Solid Solution Effects in NiAI (40% AI) Alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Chain T; Fu, Chong Long; Chisholm, Matthew F

2007-01-01

The solid solution effects of ternary additions of transition elements in intermetallic Ni-40% Al were investigated by both experimental studies and theoretical calculations. Co solute atoms when sitting at Ni sublattice sites do not affect the lattice parameter and hardening behavior of Ni-40Al. On the other hand, Fe, Mn, and Cr solutes, which are mainly on Al sublattice sites, substantially expand the lattice parameter and produce an unusual solid solution softening effect. First-principles calculations predict that these solute atoms with large unfilled d-band electrons develop large magnetic moments and effectively expand the lattice parameter when occupying Al sublattice sites. Themore » theoretical predictions were verified by both electron loss-energy spectroscopy (EELS) analyses and magnetic susceptibility measurements. The observed softening behavior can be explained quantitatively by the replacement of Ni anti-site defects (potent hardeners) by Fe, Mn, and Cr anti-site defects with smaller atom size mismatch between solute and Al atoms. This study has led to the identification of magnetic interaction as an important physical parameter affecting the solid solution hardening in intermetallic alloys containing transition elements.« less

Hyaluronidase and Collagenase Increase the Transfection Efficiency of Gene Electrotransfer in Various Murine Tumors

PubMed Central

Golzio, Muriel; Sersa, Gregor; Escoffre, Jean-Michel; Coer, Andrej; Vidic, Suzana; Teissie, Justin

2012-01-01

Abstract One of the applications of electroporation/electropulsation in biomedicine is gene electrotransfer, the wider use of which is hindered by low transfection efficiency in vivo compared with viral vectors. The aim of our study was to determine whether modulation of the extracellular matrix in solid tumors, using collagenase and hyaluronidase, could increase the transfection efficiency of gene electrotransfer in histologically different solid subcutaneous tumors in mice. Tumors were treated with enzymes before electrotransfer of plasmid DNA encoding either green fluorescent protein or luciferase. Transfection efficiency was determined 3, 9, and 15 days posttransfection. We demonstrated that pretreatment of tumors with a combination of enzymes significantly increased the transfection efficiency of electrotransfer in tumors with a high extracellular matrix area (LPB fibrosarcoma). In tumors with a smaller extracellular matrix area and less organized collagen lattice, the increase was not so pronounced (SA-1 fibrosarcoma and EAT carcinoma), whereas in B16 melanoma, in which only traces of collagen are present, pretreatment of tumors with hyaluronidase alone was more efficient than pretreatment with both enzymes. In conclusion, our results suggest that modification of the extracellular matrix could improve distribution of plasmid DNA in solid subcutaneous tumors, demonstrated by an increase in transfection efficiency, and thus have important clinical implications for electrogene therapy. PMID:21797718

Research on the synergistic doped effects and the catalysis properties of Cu2+ and Zn2+ co-doped CeO2 solid solutions

NASA Astrophysics Data System (ADS)

Zhang, Guofang; Li, Yiming; Hou, Zhonghui; Xv, Jianyi; Wang, Qingchun; Zhang, Yanghuan

2018-08-01

The Cu2+ and Zn2+ co-doped CeO2-based solid solutions were synthesized via hydrothermal method. The microstructure and the spectra features of the solid solutions were characterized systematically. The XRD results showed that the dopants were incorporated into the CeO2 lattice to form Ce1-xCu0.5xZn0.5xO2 solid solutions when x was lower than 0.14. The cell parameters and the crystalline size decreased linearly, and the lattice strain gradually increased with increasing the doping level. The TEM patterns showed that the particle size in the solid solution was lower than 10 nm which is in accordance with the XRD results. The ICP analysis indicated that the real doped content in the solid solution was close to the nominal proportion. XPS proved that the Ce3+ component was increased by doping. The Raman and PL spectra indicated that the lattice distortion and the oxygen vacancies also increased following the same trend. At the same time, the synergistic effects of two ions co-doped solid solutions were studied by comparing them with that of single ions doped samples. The catalysis effects of Cu2+ and Zn2+ co-doped CeO2-based solid solutions on the hydrogen storage electrochemical and kinetic properties of Mg2Ni alloys were detected. The electrochemistry properties of the Mg2Ni-Ni-5 wt% Ce1-xCu0.5xZn0.5xO2 composites indicated that the doped catalysts could provide better optimizations to improve the maximum discharge capacities and the discharge potentials. On the other hand, the charge transfer abilities on the surface and diffusion rate of H atoms in the bulk of alloys also got improved. The DSC measurements showed that the hydrogen desorption activation of the hydrogenated composites with Ce0.88Cu0.06Zn0.06O2 solid solutions decreased to 77.03 kJ mol-1, while that of the composites with pure CeO2 was 97.62 kJ mol-1. The catalysis effect was enhanced by the doped content increase that means that the catalysis mechanism had close links to the oxygen vacancy concentration and the lattice defects in the solid solutions. On the other hand, the doped Cu2+ and Zn2+ ions could also play an important role in the catalytic process.

Coordination of ScO+ and YO+ by multiple Ar, Kr, and Xe atoms in noble gas matrixes: a matrix isolation infrared spectroscopic and theoretical study.

PubMed

Zhao, Yanying; Gong, Yu; Chen, Mohua; Ding, Chuanfan; Zhou, Mingfei

2005-12-29

The combination of matrix isolation infrared spectroscopic and quantum chemical calculation results provide strong evidence that scandium and yttrium monoxide cations, ScO+ and YO+, coordinate multiple noble gas atoms in forming noble gas complexes. The results showed that ScO+ coordinates five Ar, Kr, or Xe atoms, and YO+ coordinates six Ar or Kr and five Xe atoms in solid noble gas matrixes. Hence, the ScO+ and YO+ cations trapped in solid noble gas matrixes should be regarded as the [ScO(Ng)5]+ (Ng = Ar, Kr, or Xe), [YO(Ng)6]+ (Ng = Ar or Kr) or [YO(Xe)5]+ complexes. Experiments with dilute krypton or xenon in argon or krypton in xenon produced new IR bands, which are due to the stepwise formation of the [ScO(Ar)(5-n)(Kr)n]+, [ScO(Kr)(5-n)(Xe)n]+ (n = 1-5), [YO(Ar)(6-n)(Kr)n]+ (n = 1-6), and [YO(Ar)(6-n)(Xe)n]+ (n = 1-4) complexes.

Spatially and temporally controlled biomineralization is facilitated by interaction between self-assembled dentin matrix protein 1 and calcium phosphate nuclei in solution.

PubMed

He, Gen; Gajjeraman, Sivakumar; Schultz, David; Cookson, David; Qin, Chunlin; Butler, William T; Hao, Jianjun; George, Anne

2005-12-13

Bone and dentin biomineralization are well-regulated processes mediated by extracellular matrix proteins. It is widely believed that specific matrix proteins in these tissues modulate nucleation of apatite nanoparticles and their growth into micrometer-sized crystals via molecular recognition at the protein-mineral interface. However, this assumption has been supported only circumstantially, and the exact mechanism remains unknown. Dentin matrix protein 1 (DMP1) is an acidic matrix protein, present in the mineralized matrix of bone and dentin. In this study, we have demonstrated using synchrotron small-angle X-ray scattering that DMP1 in solution can undergo oligomerization and temporarily stabilize the newly formed calcium phosphate nanoparticle precursors by sequestering them and preventing their further aggregation and precipitation. The solution structure represents the first low-resolution structural information for DMP1. Atomic force microscopy and transmission electron microscopy studies further confirmed that the nascent calcium phosphate nuclei formed in solution were assembled into ordered protein-mineral complexes with the aid of oligomerized DMP1, recombinant and native. This study reveals a novel mechanism by which DMP1 might facilitate initiation of mineral nucleation at specific sites during bone and dentin mineralization and prevent spontaneous calcium phosphate precipitation in areas in which mineralization is not desirable.

User's Manual for PCSMS (Parallel Complex Sparse Matrix Solver). Version 1.

NASA Technical Reports Server (NTRS)

Reddy, C. J.

2000-01-01

PCSMS (Parallel Complex Sparse Matrix Solver) is a computer code written to make use of the existing real sparse direct solvers to solve complex, sparse matrix linear equations. PCSMS converts complex matrices into real matrices and use real, sparse direct matrix solvers to factor and solve the real matrices. The solution vector is reconverted to complex numbers. Though, this utility is written for Silicon Graphics (SGI) real sparse matrix solution routines, it is general in nature and can be easily modified to work with any real sparse matrix solver. The User's Manual is written to make the user acquainted with the installation and operation of the code. Driver routines are given to aid the users to integrate PCSMS routines in their own codes.

Solid lipid nanoparticles for hydrophilic biotech drugs: optimization and cell viability studies (Caco-2 & HEPG-2 cell lines).

PubMed

Severino, Patrícia; Andreani, Tatiana; Jäger, Alessandro; Chaud, Marco V; Santana, Maria Helena A; Silva, Amélia M; Souto, Eliana B

2014-06-23

Insulin was used as model protein to developed innovative Solid Lipid Nanoparticles (SLNs) for the delivery of hydrophilic biotech drugs, with potential use in medicinal chemistry. SLNs were prepared by double emulsion with the purpose of promoting stability and enhancing the protein bioavailability. Softisan(®)100 was selected as solid lipid matrix. The surfactants (Tween(®)80, Span(®)80 and Lipoid(®)S75) and insulin were chosen applying a 2(2) factorial design with triplicate of central point, evaluating the influence of dependents variables as polydispersity index (PI), mean particle size (z-AVE), zeta potential (ZP) and encapsulation efficiency (EE) by factorial design using the ANOVA test. Therefore, thermodynamic stability, polymorphism and matrix crystallinity were checked by Differential Scanning Calorimetry (DSC) and Wide Angle X-ray Diffraction (WAXD), whereas the effect of toxicity of SLNs was check in HepG2 and Caco-2 cells. Results showed a mean particle size (z-AVE) width between 294.6 nm and 627.0 nm, a PI in the range of 0.425-0.750, ZP about -3 mV, and the EE between 38.39% and 81.20%. After tempering the bulk lipid (mimicking the end process of production), the lipid showed amorphous characteristics, with a melting point of ca. 30 °C. The toxicity of SLNs was evaluated in two distinct cell lines (HEPG-2 and Caco-2), showing to be dependent on the concentration of particles in HEPG-2 cells, while no toxicity in was reported in Caco-2 cells. SLNs were stable for 24 h in in vitro human serum albumin (HSA) solution. The resulting SLNs fabricated by double emulsion may provide a promising approach for administration of protein therapeutics and antigens. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Study on quantitative analysis of Ti, Al and V in clinical soft tissues after placing the dental implants by laser ablation inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Sajnóg, Adam; Hanć, Anetta; Makuch, Krzysztof; Koczorowski, Ryszard; Barałkiewicz, Danuta

2016-11-01

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used for in-situ quantitative analysis of oral mucosa of patients before and after implantation with titanium implants and a closing screw based on Ti6Al4V alloy. Two calibration strategies were applied, both were based on matrix matched solid standards with analytes addition. A novel approach was the application of powdered egg white proteins as a matrix material which have a similar composition to the examined tissue. In the another approach, certified reference material Bovine Muscle ERM-BB184 was used. The isotope 34S was found to be the most appropriate as an internal standard since it is homogenously distributed in the examined tissues and resulted in lower relative standard deviation values of signal of analytes of interest. Other isotopes (13C, 26Mg, 43Ca) were also evaluated as potential internal standards. The analytical performance parameters and microwave digestion of solid standards followed by solution nebulization ICP-MS analysis proved that both calibration methods are fit for their intended purpose. The LA-ICP-MS analysis on the surface of tissues after the implantation process revealed an elevated content of elements in comparison to the control group. Analytes are distributed inhomogeneously and display local maximal content of Ti up to ca. 900 μg g- 1, Al up to ca. 760 μg g- 1 and for V up to 160 μg g- 1.

Understanding the solidification and microstructure evolution during CSC-MIG welding of Fe–Cr–B-based alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sorour, A.A., E-mail: ahmad.sorour@mail.mcgill.ca; Chromik, R.R., E-mail: richard.chromik@mcgill.ca; Gauvin, R., E-mail: raynald.gauvin@mcgill.ca

2013-12-15

The present is a study of the solidification and microstructure of Fe–28.2%Cr–3.8%B–1.5%Si–1.5%Mn (wt.%) alloy deposited onto a 1020 plain carbon steel substrate using the controlled short-circuit metal inert gas welding process. The as-solidified alloy was a metal matrix composite with a hypereutectic microstructure. Thermodynamic calculation based on the Scheil–Gulliver model showed that a primary (Cr,Fe){sub 2}B phase formed first during solidification, followed by an eutectic formation of the (Cr,Fe){sub 2}B phase and a body-centered cubic Fe-based solid solution matrix, which contained Cr, Mn and Si. Microstructure analysis confirmed the formation of these phases and showed that the shape of themore » (Cr,Fe){sub 2}B phase was irregular plate. As the welding heat input increased, the weld dilution increased and thus the volume fraction of the (Cr,Fe){sub 2}B plates decreased while other microstructural characteristics were similar. - Highlights: • We deposit Fe–Cr–B-based alloy onto plain carbon steel using the CSC-MIG process. • We model the solidification behavior using thermodynamic calculation. • As deposited alloy consists of (Cr,Fe){sub 2}B plates embedded in Fe-based matrix. • We study the effect of the welding heat input on the microstructure.« less

Numerical solution of quadratic matrix equations for free vibration analysis of structures

NASA Technical Reports Server (NTRS)

Gupta, K. K.

1975-01-01

This paper is concerned with the efficient and accurate solution of the eigenvalue problem represented by quadratic matrix equations. Such matrix forms are obtained in connection with the free vibration analysis of structures, discretized by finite 'dynamic' elements, resulting in frequency-dependent stiffness and inertia matrices. The paper presents a new numerical solution procedure of the quadratic matrix equations, based on a combined Sturm sequence and inverse iteration technique enabling economical and accurate determination of a few required eigenvalues and associated vectors. An alternative procedure based on a simultaneous iteration procedure is also described when only the first few modes are the usual requirement. The employment of finite dynamic elements in conjunction with the presently developed eigenvalue routines results in a most significant economy in the dynamic analysis of structures.

Cavitation Erosion of Cermet-Coated Aluminium Bronzes.

PubMed

Mitelea, Ion; Oancă, Octavian; Bordeaşu, Ilare; Crăciunescu, Corneliu M

2016-03-17

The cavitation erosion resistance of CuAl10Ni5Fe2.5Mn1 following plasma spraying with Al₂O₃·30(Ni 20 Al) powder and laser re-melting was analyzed in view of possible improvements of the lifetime of components used in hydraulic environments. The cavitation erosion resistance was substantially improved compared with the one of the base material. The thickness of the re-melted layer was in the range of several hundred micrometers, with a surface microhardness increasing from 250 to 420 HV 0.2. Compositional, structural, and microstructural explorations showed that the microstructure of the re-melted and homogenized layer, consisting of a cubic Al₂O₃ matrix with dispersed Ni-based solid solution is associated with the hardness increase and consequently with the improvement of the cavitation erosion resistance.

A composite approach boosts transduction coefficients of piezoceramics for energy harvesting

NASA Astrophysics Data System (ADS)

Yu, Xiaole; Hou, Yudong; Zheng, Mupeng; Zhao, Haiyan; Zhu, Mankang

2018-03-01

Piezoelectric energy harvesting is a hotspot in the field of new energy, the core goal of which is to prepare piezoceramics with a high transduction coefficient (d33×g33). The traditional solid-solution design strategy usually causes the same variation trend of d33 and ɛr, resulting in a low d33×g33 value. In this work, a composite design strategy was proposed that uses PZN-PZT/ZnAl2O4 as an example. By introducing ZnAl2O4, which is nonferroelectric with low ɛr, to the PZN-PZT piezoelectric matrix, ɛr decreased rapidly while d33 remained relatively stable. This behavior was ascribed to the increase of Q33 caused by an interfacial effect facilitating the formation of micro-domain structure.

Extraction of mercury(II) with sulfurized jojoba oil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wisniak, J.; Schorr, G.; Zacovsky, D.

1990-09-01

Sulfurized jojoba oil containing 12% by weight S has been tested as an extractant for Hg(II) from aqueous solutions. This paper reports on experiments performed with the extractant dissolved in a solvent (liquid--liquid extraction) or adsorbed in an appropriate resin matrix (solid--liquid extraction). The extraction characteristics of both systems have been measured and show that sulfurized jojoba oil exhibits very good possibilities as an extractant. The performance of several resins treated with sulfurized jojoba oil for adsorbing mercury(II) was studied. The morphology of the different resins was examined by using scanning electron microscopy. The sulfurized oil is attached to themore » resin sites through the sulfur atoms; it is estimated that there are about 2 mol of S active sites per kilogram of resin.« less

Effect of interfacial stresses in an elastic body with a nanoinclusion

NASA Astrophysics Data System (ADS)

Vakaeva, Aleksandra B.; Grekov, Mikhail A.

2018-05-01

The 2-D problem of an infinite elastic solid with a nanoinclusion of a different from circular shape is solved. The interfacial stresses are acting at the interface. Contact of the inclusion with the matrix satisfies the ideal conditions of cohesion. The generalized Laplace - Young law defines conditions at the interface. To solve the problem, Gurtin - Murdoch surface elasticity model, Goursat - Kolosov complex potentials and the boundary perturbation method are used. The problem is reduced to the solution of two independent Riemann - Hilbert's boundary problems. For the circular inclusion, hypersingular integral equation in an unknown interfacial stress is derived. The algorithm of solving this equation is constructed. The influence of the interfacial stress and the dimension of the circular inclusion on the stress distribution and stress concentration at the interface are analyzed.

Structure and microhardness of Al-Si-Cu-Ni alloy after severe plastic deformation and high-temperature annealing

NASA Astrophysics Data System (ADS)

Shvets, Karina; Khalikova, Gulnara; Korznikova, Elena; Trifonov, Vadim

2015-10-01

The effect of severe plastic deformation by high-pressure torsion (HPT) and subsequent annealing on the microstructure and microhardness of squeeze casting Al-22%Si-3%Cu-1.7%Ni alloy was investigated. HPT was performed at room temperature with 5 rotations under the pressure of 4 GPa. Annealing temperature range varied from 300 to 500°C for 5 min. HPT resulted in refinement and partial dissolution of the primary silicon and intermetallic particles in aluminum matrix and structure fragmentation that caused the microhardness increase. Subsequent annealing lead to the decomposition of the supersaturated solid solution that took place simultaneously with recovery and recrystallization of the fragmented structure. Increase of annealing temperature resulted in decrease of microhardness values.

Ne matrix spectra of the sym-C6Br3F3+ radical cation

USGS Publications Warehouse

Bondybey, V.E.; Sears, T.J.; Miller, T.A.; Vaughn, C.; English, J.H.; Shiley, R.S.

1981-01-01

The electronic absorption and laser excited, wavelength resolved fluorescence spectra of the title cation have been observed in solid Ne matrix and vibrationally analysed. The vibrational structure of the excited B2A2??? state shows close similarity to the parent compound. The X2E??? ground state structure is strongly perturbed and irregular owing to a large Jahn-Teller distortion. The data are analysed in terms of a recently developed, sophisticated multimode Jahn-Teller theoretical model. We have generated the sym-C6Br3F3+ cations in solid Ne matrix and obtained their wavelength resolved emission and absorption spectra. T ground electronic X2E??? state exhibits an irregular and strongly perturbed vibrational structure, which can be successfully modeled using sophisticated multimode Jahn-Teller theory. ?? 1981.

Process for recovering pertechnetate ions from an aqueous solution also containing other ions

DOEpatents

Rogers, R.; Horwitz, E.P.; Bond, A.H.

1997-02-18

A solid/liquid process for the separation and recovery of TcO{sub 4}{sup {minus}1} ions from an aqueous solution is disclosed. The solid support comprises separation particles having surface-bonded poly(ethylene glycol) groups; whereas the aqueous solution from which the TcO{sub 4}{sup {minus}1} ions are separated contains a poly(ethylene glycol) liquid/liquid biphase-forming amount of a dissolved salt. A solid/liquid phase admixture of separation particles containing bound TcO{sub 4}{sup {minus}1} ions in such an aqueous solution that is free from MoO{sub 4}{sup {minus}2} ions is also contemplated, as is a chromatography apparatus containing that solid/liquid phase admixture. 15 figs.

Colloid Mobilization in a Fractured Soil: Effect of Pore-Water Exchange between Preferential Flow Paths and Soil Matrix.

PubMed

Mohanty, Sanjay K; Saiers, James E; Ryan, Joseph N

2016-03-01

Exchange of water and solutes between contaminated soil matrix and bulk solution in preferential flow paths has been shown to contribute to the long-term release of dissolved contaminants in the subsurface, but whether and how this exchange can affect the release of colloids in a soil are unclear. To examine this, we applied rainfall solutions of different ionic strength on an intact soil core and compared the resulting changes in effluent colloid concentration through multiple sampling ports. The exchange of water between soil matrix and the preferential flow paths leading to each port was characterized on the basis of the bromide (conservative tracer) breakthrough time at the port. At individual ports, two rainfalls of a certain ionic strength mobilized different amounts of colloids when the soil was pre-exposed to a solution of lower or higher ionic strength. This result indicates that colloid mobilization depended on rainfall solution history, which is referred as colloid mobilization hysteresis. The extent of hysteresis was increased with increases in exchange of pore water and solutes between preferential flow paths and matrix. The results indicate that the soil matrix exchanged the old water from the previous infiltration with new infiltrating water during successive infiltration and changed the pore water chemistry in the preferential flow paths, which in turn affected the release of soil colloids. Therefore, rainfall solution history and soil heterogeneity must be considered to assess colloid mobilization in the subsurface. These findings have implications for the release of colloids, colloid-associated contaminants, and pathogens from soils.

Rapid and sensitive determination of major polyphenolic components in Euphoria longana Lam. seeds using matrix solid-phase dispersion extraction and UHPLC with hybrid linear ion trap triple quadrupole mass spectrometry.

PubMed

Rathore, Atul S; Sathiyanarayanan, L; Deshpande, Shreekant; Mahadik, Kakasaheb R

2016-11-01

A rapid and sensitive method for the extraction and determination of four major polyphenolic components in Euphoria longana Lam. seeds is presented for the first time based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry. Matrix solid-phase dispersion method was designed for the extraction of Euphoria longana seed constituents and compared with microwave-assisted extraction and ultrasonic-assisted extraction methods. An Ultra high performance liquid chromatography with hybrid triple quadrupole linear ion-trap mass spectrometry method was developed for quantitative analysis in multiple-reaction monitoring mode in negative electrospray ionization. The chromatographic separation was accomplished using an ACQUITY UPLC BEH C 18 (2.1 mm × 50 mm, 1.7 μm) column with gradient elution of 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. The developed method was validated with acceptable linearity (r 2 > 0.999), precision (RSD ≤ 2.22%) and recovery (RSD ≤ 2.35%). The results indicated that matrix solid-phase dispersion produced comparable extraction efficiency compared with other methods nevertheless was more convenient and time-saving with reduced requirements on sample and solvent volumes. The proposed method is rapid and sensitive in providing a promising alternative for extraction and comprehensive determination of active components for quality control of Euphoria longana products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of carbonate ion in the crystallization medium on the formation and chemical composition of CaHA-SrHA solid solutions

NASA Astrophysics Data System (ADS)

Nikolaev, Anton; Kuz'mina, Maria; Frank-Kamenetskaya, Olga; Zorina, Maina

2015-06-01

The study of the influence of carbonate ions in a solution to Sr-distribution in system «solution-crystal» and to ion substitutions and the non-stoichiometry of formed CaHA-SrHA solid solutions was carried out. The CaHA-SrHA solid solutions were synthesized by precipitation from aqueous solutions with the atomic C/P ratio equal to 0, 0.05 and 0.1 at T = 90 °C. Resulting precipitates were studied using various methods including X-ray powder diffraction, infrared spectroscopy and different chemical analyses. The results of the study have shown that in the range of values of (Ca + Sr)/P in the water solution from 40% to 85%, the presence of carbonate ions (C/P = 0.05-0.1) promotes the incorporation of strontium in the apatite. Crystalline apatite solid solutions formed from water solutions of such composition are more defective compared to apatites that are mainly calcium or strontium. They are characterized by a smaller size coherence scattering domain length along [0 0 1] direction and a greater number of carbonate ions, water molecules and vacancies at the Ca-sites.