Nanoalloy catalysts inside fuel cells: An atomic-level perspective on the functionality by combined in operando x-ray spectroscopy and total scattering

DOE PAGES

Petkov, Valeri; Maswadeh, Yazan; Zhao, Yinguang; ...

2018-04-18

We introduce an experimental approach for structural characterization of catalysts for fuel cells combining synchrotron x-ray spectroscopy and total scattering. The approach allows probing catalysts inside operating fuel cells with atomic-level precision (~ 0.02 Å) and element specificity (~ 2–3 at%) in both time (~ 1 min) and space (~ μm) resolved manner. The approach is demonstrated on exemplary Pd-Sn and Pt-Ni-Cu nanoalloy catalysts for the oxygen reduction reaction (ORR) deposited on the cathode of an operating proton exchange membrane fuel cell. In operando x-ray data show that under operating conditions, the catalyst particles can undergo specific structural changes, rangingmore » from sub-Å atomic fluctuations and sharp nanophase transitions to a gradual strain relaxation and growth, which inflict significant losses in their ORR activity. Though triggered electrochemically, the changes are not driven solely by differences in the reduction potential and surface energy of the metallic species constituting the nanoalloys but also by the formation energy of competing nanophases, mismatch between the size of individual atomic species and their ability to interdiffuse fast in search of energetically favorable configurations. Given their complexity, the changes are difficult to predict and so the resulting ORR losses remain difficult to limit. We show that in operando knowledge of the structural evolution of nanoalloy catalysts helps create strategies for improving their activity and stability. In particular, we show that shaping Pd-Sn nanoalloys rich in Pd as cubes reduces the interdiffusion of atoms at their surface and so makes them better catalysts for ORR in fuel cells in comparison to other Pd-Sn nanoalloys. In addition, we demonstrate that the approach introduced here can provide knowledge of other major factors affecting the performance of fuel cells such as operating temperature and the overall catalyst utilization, in particular the evolution of

Structure determination in 55-atom Li-Na and Na-K nanoalloys.

PubMed

Aguado, Andrés; López, José M

2010-09-07

The structure of 55-atom Li-Na and Na-K nanoalloys is determined through combined empirical potential (EP) and density functional theory (DFT) calculations. The potential energy surface generated by the EP model is extensively sampled by using the basin hopping technique, and a wide diversity of structural motifs is reoptimized at the DFT level. A composition comparison technique is applied at the DFT level in order to make a final refinement of the global minimum structures. For dilute concentrations of one of the alkali atoms, the structure of the pure metal cluster, namely, a perfect Mackay icosahedron, remains stable, with the minority component atoms entering the host cluster as substitutional impurities. At intermediate concentrations, the nanoalloys adopt instead a core-shell polyicosahedral (p-Ih) packing, where the element with smaller atomic size and larger cohesive energy segregates to the cluster core. The p-Ih structures show a marked prolate deformation, in agreement with the predictions of jelliumlike models. The electronic preference for a prolate cluster shape, which is frustrated in the 55-atom pure clusters due to the icosahedral geometrical shell closing, is therefore realized only in the 55-atom nanoalloys. An analysis of the electronic densities of states suggests that photoelectron spectroscopy would be a sufficiently sensitive technique to assess the structures of nanoalloys with fixed size and varying compositions.

Gas-Flow Tailoring Fabrication of Graphene-like Co-Nx-C Nanosheet Supported Sub-10 nm PtCo Nanoalloys as Synergistic Catalyst for Air-Cathode Microbial Fuel Cells.

PubMed

Cao, Chun; Wei, Liling; Zhai, Qiran; Ci, Jiliang; Li, Weiwei; Wang, Gang; Shen, Jianquan

2017-07-12

In this work, we presented a novel, facile, and template-free strategy for fabricating graphene-like N-doped carbon as oxygen reduction catalyst in sustainable microbial fuel cells (MFCs) by using an ion-inducing and spontaneous gas-flow tailoring effect from a unique nitrogen-rich polymer gel precursor which has not been reported in materials science. Remarkably, by introduction of trace platinum- and cobalt- precursor in polymer gel, highly dispersed sub-10 nm PtCo nanoalloys can be in situ grown and anchored on graphene-like carbon. The as-prepared catalysts were investigated by a series of physical characterizations, electrochemical measurements, and microbial fuel cell tests. Interestingly, even with a low Pt content (5.13 wt %), the most active Co/N codoped carbon supported PtCo nanoalloys (Co-N-C/Pt) exhibited dramatically improved catalytic activity toward oxygen reduction reaction coupled with superior output power density (1008 ± 43 mW m -2 ) in MFCs, which was 29.40% higher than the state of the art Pt/C (20 wt %). Notability, the distinct catalytic activity of Co-N-C/Pt was attributed to the highly efficient synergistic catalytic effect of Co-Nx-C and PtCo nanoalloys. Therefore, Co-N-C/Pt should be a promising oxygen reduction catalyst for application in MFCs. Further, the novel strategy for graphene-like carbon also can be widely used in many other energy conversion and storage devices.

Computational study of AuSi{sub n} (n=1-9) nanoalloy clusters invoking DFT based descriptors

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

Ranjan, Prabhat; Kumar, Ajay; Chakraborty, Tanmoy, E-mail: tanmoy.chakraborty@jaipur.manipal.edu, E-mail: tanmoychem@gmail.com

2016-04-13

Nanoalloy clusters formed between Au and Si are topics of great interest today from both scientific and technological point of view. Due to its remarkable catalytic, electronic, mechanical and magnetic properties Au-Si nanoalloy clusters have extensive applications in the field of microelectronics, catalysis, biomedicine, and jewelry industry. Density Functional Theory (DFT) is a new paradigm of quantum mechanics, which is very much popular to study the electronic properties of materials. Conceptual DFT based descriptors have been invoked to correlate the experimental properties of nanoalloy clusters. In this venture, we have systematically investigated AuSi{sub n} (n=1-9) nanoalloy clusters in the theoreticalmore » frame of the B3LYP exchange correlation. The experimental properties of AuSi{sub n} (n=1-9) nanoalloy clusters are correlated in terms of DFT based descriptors viz. HOMO-LUMO gap, Electronegativity (χ), Global Hardness (η), Global Softness (S) and Electrophilicity Index (ω). The calculated HOMO-LUMO gap exhibits interesting odd-even alteration behaviour, indicating that even numbered clusters possess higher stability as compare to their neighbour odd numbered clusters. This study also reflects a very well agreement between experimental bond length and computed data.« less

Facile and rapid one-pot microwave-assisted synthesis of Pd-Ni magnetic nanoalloys confined in mesoporous carbons

NASA Astrophysics Data System (ADS)

Martínez de Yuso, Alicia; Le Meins, Jean-Marc; Oumellal, Yassine; Paul-Boncour, Valérie; Zlotea, Claudia; Matei Ghimbeu, Camelia

2016-12-01

An easy and rapid one-pot microwave-assisted soft-template synthesis method for the preparation of Pd-Ni nanoalloys confined in mesoporous carbon is reported. This approach allows the formation of mesoporous carbon and the growth of the particles at the same time, under short microwave irradiation (4 h) compared to the several days spent for the classical approach. In addition, the synthesis steps are diminished and no thermopolymerization step or reduction treatment being required. The influence of the Pd-Ni composition on the particle size and on the carbon characteristics was investigated. Pd-Ni solid solutions in the whole composition range could be obtained, and the metallic composition proved to have an important effect on the nanoparticle size but low influence on carbon textural properties. Small and uniformly distributed nanoparticles were confined in mesoporous carbon with uniform pore size distribution, and dependence between the nanoparticle size and the nanoalloy composition was observed, i.e., increase of the particle size with increasing the Ni content (from 5 to 14 nm). The magnetic properties of the materials showed a strong nanoparticle size and/or composition effect. The blocking temperature of Pd-Ni nanoalloys increases with the increase of Ni amount and therefore of particle size. The magnetization values are smaller than the bulk counterpart particularly for the Ni-rich compositions due to the formed graphitic shells surrounding the particles inducing a dead magnetic layer.

Synthesis of FeCo magnetic nanoalloys and investigation of heating properties for magnetic fluid hyperthermia

NASA Astrophysics Data System (ADS)

Çelik, Özer; Fırat, Tezer

2018-06-01

In this study, size controlled FeCo colloidal magnetic nanoalloys in the range of 11.5-37.2 nm were synthesized by surfactant assistant ball milling method. Magnetic separation technique was performed subsequent to synthesis process so as to obtain magnetic nanoalloy fluid with narrow size distribution. Particle distribution was determined by transmission electron microscope (TEM) while X-ray diffraction (XRD) measurements verified FeCo alloy formation as BCC structure. Vibrating sample magnetometer (VSM) method was used to investigate magnetic properties of nanoalloys. Maximum saturation magnetization and maximum coercivity were obtained as 172 Am2/kg for nanoparticles with the mean size of 37.2 nm and 19.4 mT for nanoparticles with the mean size of 13.3 nm, respectively. The heating ability of FeCo magnetic nanoalloys was determined through calorimetrical measurements for magnetic fluid hyperthermia (MFH) applications. Heat generation mechanisms were investigated by using linear response theory and Stoner-Wohlfarth (S-W) model. Specific absorption rate (SAR) values were obtained in the range of 2-15 W/g for magnetic field frequency of 171 kHz and magnetic field strength in between 6 and 14 mT.

High performing and stable supported nano-alloys for the catalytic hydrogenation of levulinic acid to γ-valerolactone

PubMed Central

Luo, Wenhao; Sankar, Meenakshisundaram; Beale, Andrew M.; He, Qian; Kiely, Christopher J.; Bruijnincx, Pieter C. A.; Weckhuysen, Bert M.

2015-01-01

The catalytic hydrogenation of levulinic acid, a key platform molecule in many biorefinery schemes, into γ-valerolactone is considered as one of the pivotal reactions to convert lignocellulose-based biomass into renewable fuels and chemicals. Here we report on the development of highly active, selective and stable supported metal catalysts for this reaction and on the beneficial effects of metal nano-alloying. Bimetallic random alloys of gold-palladium and ruthenium-palladium supported on titanium dioxide are prepared with a modified metal impregnation method. Gold-palladium/titanium dioxide shows a marked,~27-fold increase in activity (that is, turnover frequency of 0.1 s−1) compared with its monometallic counterparts. Although ruthenium-palladium/titanium dioxide is not only exceptionally active (that is, turnover frequency of 0.6 s−1), it shows excellent, sustained selectivity to γ-valerolactone (99%). The dilution and isolation of ruthenium by palladium is thought to be responsible for this superior catalytic performance. Alloying, furthermore, greatly improves the stability of both supported nano-alloy catalysts. PMID:25779385

Evolution of Active Sites in Pt-Based Nanoalloy Catalysts for the Oxidation of Carbonaceous Species by Combined in Situ Infrared Spectroscopy and Total X-ray Scattering.

PubMed

Petkov, Valeri; Maswadeh, Yazan; Lu, Aolin; Shan, Shiyao; Kareem, Haval; Zhao, Yinguang; Luo, Jin; Zhong, Chuan-Jian; Beyer, Kevin; Chapman, Karena

2018-04-04

We present results from combined in situ infrared spectroscopy and total X-ray scattering studies on the evolution of catalytically active sites in exemplary binary and ternary Pt-based nanoalloys during a sequence of CO oxidation-reactivation-CO oxidation reactions. We find that when within a particular compositional range, the fresh nanoalloys may exhibit high catalytic activity for low-temperature CO oxidation. Using surface-specific atomic pair distribution functions (PDFs) extracted from the in situ total X-ray scattering data, we find that, regardless of their chemical composition and initial catalytic activity, the fresh nanoalloys suffer a significant surface structural disorder during CO oxidation. Upon reactivation in oxygen atmosphere, the surface of used nanoalloy catalysts both partially oxidizes and orders. Remarkably, it largely retains its structural state when the nanoalloys are reused as CO oxidation catalysts. The seemingly inverse structural changes of studied nanoalloy catalysts occurring under CO oxidation and reactivation conditions affect the active sites on their surface significantly. In particular, through different mechanisms, both appear to reduce the CO binding strength to the nanoalloy's surface and thus increase the catalytic stability of the nanoalloys. The findings provide clues for further optimization of nanoalloy catalysts for the oxidation of carbonaceous species through optimizing their composition, activation, and reactivation. Besides, the findings demonstrate the usefulness of combined in situ infrared spectroscopy and total X-ray scattering coupled to surface-specific atomic PDF analysis to the ongoing effort to produce advanced catalysts for environmentally and technologically important applications.

Bibliometric trend and patent analysis in nano-alloys research for period 2000-2013.

PubMed

Živković, Dragana; Niculović, Milica; Manasijević, Dragan; Minić, Duško; Ćosović, Vladan; Sibinović, Maja

2015-05-04

This paper presents an overview of current situation in nano-alloys investigations based on bibliometric and patent analysis. Bibliometric analysis data, for period from 2000 to September 2013, were obtained using Scopus database as selected index database, whereas analyzed parameters were: number of scientific papers per years, authors, countries, affiliations, subject areas and document types. Analysis of nano-alloys patents was done with specific database, using the International Patent Classification and Patent Scope for the period from 2003 to 2013 year. Information found in this database was the number of patents, patent classification by country, patent applicators, main inventors and pub date.

Bibliometric trend and patent analysis in nano-alloys research for period 2000-2013.

PubMed

Živković, Dragana; Niculović, Milica; Manasijević, Dragan; Minić, Duško; Ćosović, Vladan; Sibinović, Maja

2015-01-01

This paper presents an overview of current situation in nano-alloys investigations based on bibliometric and patent analysis. Bibliometric analysis data, for the period 2000 to 2013, were obtained using Scopus database as selected index database, whereas analyzed parameters were: number of scientific papers per year, authors, countries, affiliations, subject areas and document types. Analysis of nano-alloys patents was done with specific database, using the International Patent Classification and Patent Scope for the period 2003 to 2013. Information found in this database was the number of patents, patent classification by country, patent applicators, main inventors and publication date.

Nanoalloy Printed and Pulse-Laser Sintered Flexible Sensor Devices with Enhanced Stability and Materials Compatibility

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

Zhao, Wei; Rovore, Thomas; Weerawarne, Darshana

2015-06-02

While conformal and wearable devices have become one of the most desired formats for printable electronics, it is challenging to establish a scalable process that produces stable conductive patterns but also uses substrates compatible with widely available wearable materials. Here, we describe findings of an investigation of a nanoalloy ink printed and pulsed laser sintered conductive patterns as flexible functional devices with enhanced stability and materials compatibility. While nanoparticle inks are desired for printable electronics, almost all existing nanoparticle inks are based on single-metal component, which, as an electronic element, is limited by its inherent stabilities of the metal suchmore » as propensity of metal oxidation and mobility of metal ions, especially in sintering processes. The work here has demonstrated the first example in exploiting plasmonic coupling of nanoalloys and pulsed-laser energy with controllable thermal penetration. The experimental and theoretical results have revealed clear correlation between the pulsed laser parameters and the nanoalloy structural characteristics. The superior performance of the resulting flexible sensor device, upon imparting nanostructured sensing materials, for detecting volatile organic compounds has significant implications to developing stable and wearable sensors for monitoring environmental pollutants and breath biomarkers. This simple “nanoalloy printing 'laser sintering' nanostructure printing” process is entirely general to many different sensor devices and nanostructured sensing materials, enabling the ability to easily construct sophisticated sensor array.« less

Nanoalloy Printed and Pulse-Laser Sintered Flexible Sensor Devices with Enhanced Stability and Materials Compatibility.

PubMed

Zhao, Wei; Rovere, Thomas; Weerawarne, Darshana; Osterhoudt, Gavin; Kang, Ning; Joseph, Pharrah; Luo, Jin; Shim, Bonggu; Poliks, Mark; Zhong, Chuan-Jian

2015-06-23

While conformal and wearable devices have become one of the most desired formats for printable electronics, it is challenging to establish a scalable process that produces stable conductive patterns but also uses substrates compatible with widely available wearable materials. Here, we describe findings of an investigation of a nanoalloy ink printed and pulsed-laser sintered conductive patterns as flexible functional devices with enhanced stability and materials compatibility. While nanoparticle inks are desired for printable electronics, almost all existing nanoparticle inks are based on single-metal component, which, as an electronic element, is limited by its inherent stabilities of the metal such as propensity of metal oxidation and mobility of metal ions, especially in sintering processes. The work here has demonstrated the first example in exploiting plasmonic coupling of nanoalloys and pulsed-laser energy with controllable thermal penetration. The experimental and theoretical results have revealed clear correlation between the pulsed laser parameters and the nanoalloy structural characteristics. The superior performance of the resulting flexible sensor device, upon imparting nanostructured sensing materials, for detecting volatile organic compounds has significant implications to developing stable and wearable sensors for monitoring environmental pollutants and breath biomarkers. This simple "nanoalloy printing-laser sintering-nanostructure printing" process is entirely general to many different sensor devices and nanostructured sensing materials, enabling the ability to easily construct sophisticated sensor array.

Control of Surface Segregation in Bimetallic NiCr Nanoalloys Immersed in Ag Matrix

PubMed Central

Bohra, Murtaza; Singh, Vidyadhar; Grammatikopoulos, Panagiotis; Toulkeridou, Evropi; Diaz, Rosa E.; Bobo, Jean-François; Sowwan, Mukhles

2016-01-01

Cr-surface segregation is a main roadblock encumbering many magneto-biomedical applications of bimetallic M-Cr nanoalloys (where M = Fe, Co and Ni). To overcome this problem, we developed Ni95Cr5:Ag nanocomposite as a model system, consisting of non-interacting Ni95Cr5 nanoalloys (5 ± 1 nm) immersed in non-magnetic Ag matrix by controlled simultaneous co-sputtering of Ni95Cr5 and Ag. We employed Curie temperature (TC) as an indicator of phase purity check of these nanocomposites, which is estimated to be around the bulk Ni95Cr5 value of 320 K. This confirms prevention of Cr-segregation and also entails effective control of surface oxidation. Compared to Cr-segregated Ni95Cr5 nanoalloy films and nanoclusters, we did not observe any unwanted magnetic effects such as presence Cr-antiferromagnetic transition, large non-saturation, exchange bias behavior (if any) or uncompensated higher TC values. These nanocomposites films also lose their unique magnetic properties only at elevated temperatures beyond application requirements (≥800 K), either by showing Ni-type behavior or by a complete conversion into Ni/Cr-oxides in vacuum and air environment, respectively. PMID:26750659

Modelling free and oxide-supported nanoalloy catalysts: comparison of bulk-immiscible Pd-Ir and Au-Rh systems and influence of a TiO2 support.

PubMed

Demiroglu, Ilker; Fan, Tian-E; Li, Z Y; Yuan, Jun; Liu, Tun-Dong; Piccolo, Laurent; Johnston, Roy L

2018-05-24

The relative stabilities of different chemical arrangements of Pd-Ir and Au-Rh nanoalloys (and their pure metal equivalents) are studied, for a range of compositions, for fcc truncated octahedral 38- and 79-atom nanoparticles (NPs). For the 38-atom NPs, comparisons are made of pure and alloy NPs supported on a TiO2(110) slab. The relative energies of different chemical arrangements are found to be similar for Pd-Ir and Au-Rh nanoalloys, and depend on the cohesive and surface energies of the component metals. For supported nanoalloys on TiO2, the interaction with the surface is greater for Ir (Rh) than Pd (Au): most of the pure NPs and nanoalloys preferentially bind to the TiO2 surface in an edge-on configuration. When Au-Rh nanoalloys are bound to the surface through Au, the surface binding strength is lower than for the pure Au NP, while the Pd-surface interaction is found to be greater for Pd-Ir nanoalloys than for the pure Pd NP. However, alloying leads to very little difference in Ir-surface and Rh-surface binding strength. Comparing the relative stabilities of the TiO2-supported NPs, the results for Pd-Ir and Au-Rh nanoalloys are the same: supported Janus NPs, whose Ir (Rh) atoms bind to the TiO2 surface, bind most strongly to the surface, becoming closer in energy to the core-shell configurations (Ir@Pd and Rh@Au) which are favoured for the free particles.

Size effects on melting and wetting in the Ga-Pb nano-alloy

NASA Astrophysics Data System (ADS)

Allione, M.; Kofman, R.; Celestini, F.; Lereah, Y.

2009-04-01

Ga-Pb alloys with 15 at% Pb mean concentration have been prepared at the nanoscale by means of evaporation-condensation technique in ultra high vacuum conditions. Transmission electron microscope images indicate that at room temperature, the system is a two-components breath figure composed of liquid Ga nanodrops containing Pb nanocrystals. Some thermodynamic properties of this nano-alloy are investigated for different temperatures and particle sizes. The results obtained put in evidence a large modification of the Ga-Pb bulk phase diagram: a decrease of the melting temperatures of the two components as well as the ones of the miscibility gap. Changes in the microscopic structure of the system as a function of temperature have been investigated and a full wetting transition from a dry to a completely wet state has been put in evidence.

Symmetry and novelty in the electronic and geometric structure of nanoalloys:. the case of Ag27Cu7

NASA Astrophysics Data System (ADS)

Ortigoza, M. Alcántara; Rahman, T. S.

2008-04-01

Nanoparticles of bimetallic alloys have been shown to possess composition dependent characteristics which distinguish themselves from the corresponding bulk alloys. Taking the 34-atom nanoalloy of Ag and Cu (Ag27Cu7), we show using first principles electronic structure calculations that this core-shell alloy indeed has perfect D5h symmetry and consists of only 6 non-equivalent (2 Cu and 4 Ag) atoms. Analysis of the interatomic bond lengths and detailed electronic structure further reveal that the Cu atoms play a major role in controlling the characteristics of the nanoalloy. The higher cohesive energy, together with shorter bond length for Cu, compared to Ag, conspire to produce a hierarchy in the relative strengths of the Ag - Cu, Ag - Ag, and Cu - Cu bonds and corresponding interatomic bond lengths, point to the uniqueness in the characteristics of this nanoalloy. Charge density plots of Ag27Cu7 provide further insights into the relative strengths of the various interatomic bonds.

Synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel for electrochemical detection of dopamine.

PubMed

Li, Ruiyi; Yang, Tingting; Li, Zaijun; Gu, Zhiguo; Wang, Guangli; Liu, Junkang

2017-02-15

Integration of noble metal nanomaterials on graphene nanosheets potentially paves one way to improve their electronic, chemical and electrochemical properties. The study reported synthesis of palladium@gold nanoalloys/nitrogen and sulphur-functionalized multiple graphene aerogel composite (Pd@Au/N,S-MGA). The as-prepared composite offers a well-defined three-dimensional architecture with rich of mesopores. The Pd@Au nanoalloys were dispersed on the graphene framework networks and their active sites were fully exposed. The unique structure achieves to ultra high electron/ion conductivity, electrocatalytic activity and structural stability. The sensor based on the Pd@Au/N,S-MGA creates ultrasensitive electrochemical response towards dopamine due to significantly electrochemical synergy between Pd, Au and N,S-MGA. Its differential pulse voltammetric signal linearly increases with the increase of dopamine concentration in the range from 1.0 × 10 -9  M to 4.0 × 10 -5  M with the detection limit of 3.6 × 10 -10  M (S/N = 3). The analytical method provides the advantage of sensitivity, reproducibility, rapidity and long-term stability. It has been successfully applied in the detection of trace dopamine in biological samples. The study also opens a window on the electronic properties of graphene aerogel and metal nanomaterials as well their nanohybrids to meet needs of further applications as nanoelectronics in diagnosis, bioanalysis and catalysis. Copyright © 2016 Elsevier B.V. All rights reserved.

c-T phase diagram and Landau free energies of (AgAu)55 nanoalloy via neural-network molecular dynamic simulations.

PubMed

Chiriki, Siva; Jindal, Shweta; Bulusu, Satya S

2017-10-21

For understanding the structure, dynamics, and thermal stability of (AgAu) 55 nanoalloys, knowledge of the composition-temperature (c-T) phase diagram is essential due to the explicit dependence of properties on composition and temperature. Experimentally, generating the phase diagrams is very challenging, and therefore theoretical insight is necessary. We use an artificial neural network potential for (AgAu) 55 nanoalloys. Predicted global minimum structures for pure gold and gold rich compositions are lower in energy compared to previous reports by density functional theory. The present work based on c-T phase diagram, surface area, surface charge, probability of isomers, and Landau free energies supports the enhancement of catalytic property of Ag-Au nanoalloys by incorporation of Ag up to 24% by composition in Au nanoparticles as found experimentally. The phase diagram shows that there is a coexistence temperature range of 70 K for Ag 28 Au 27 compared to all other compositions. We propose the power spectrum coefficients derived from spherical harmonics as an order parameter to calculate Landau free energies.

Catalytic and electrocatalytic oxidation of ethanol over palladium-based nanoalloy catalysts.

PubMed

Yin, Jun; Shan, Shiyao; Ng, Mei Shan; Yang, Lefu; Mott, Derrick; Fang, Weiqin; Kang, Ning; Luo, Jin; Zhong, Chuan-Jian

2013-07-23

The control of the nanoscale composition and structure of alloy catalysts plays an important role in heterogeneous catalysis. This paper describes novel findings of an investigation for Pd-based nanoalloy catalysts (PdCo and PdCu) for ethanol oxidation reaction (EOR) in gas phase and alkaline electrolyte. Although the PdCo catalyst exhibits a mass activity similar to Pd, the PdCu catalyst is shown to display a much higher mass activity than Pd for the electrocatalytic EOR in alkaline electrolyte. This finding is consistent with the finding on the surface enrichment of Pd on the alloyed PdCu surface, in contrast to the surface enrichment of Co in the alloyed PdCo surface. The viability of C-C bond cleavage was also probed for the PdCu catalysts in both gas-phase and electrolyte-phase EOR. In the gas-phase reaction, although the catalytic conversion rate for CO2 product is higher over Pd than PdCu, the nanoalloy PdCu catalyst appears to suppress the formation of acetic acid, which is a significant portion of the product in the case of pure Pd catalyst. In the alkaline electrolyte, CO2 was detected from the gas phase above the electrolyte upon acid treatment following the electrolysis, along with traces of aldehyde and acetic acid. An analysis of the electrochemical properties indicates that the oxophilicity of the base metal alloyed with Pd, in addition to the surface enrichment of metals, may have played an important role in the observed difference of the catalytic and electrocatalytic activities. In comparison with Pd alloyed with Co, the results for Pd alloyed with Cu showed a more significant positive shift of the reduction potential of the oxygenated Pd species on the surface. These findings have important implications for further fine-tuning of the Pd nanoalloys in terms of base metal composition toward highly active and selective catalysts for EOR.

Hydrogel covered bimetallic Co:Ni magnetic nano alloy for protein adsorption in biomedical application

NASA Astrophysics Data System (ADS)

Rajar, Kausar; Alveroglu, Esra

2017-10-01

In this study, polyacrylamide (PAAm) hydrogel covered CoNi magnetic nanoalloys with various Co/Ni molar ratio (from 1/4 to 4/1) were synthesized, characterized and used for adsorption of Bovine Serum Albumin (BSA). XRD, EDS, VSM, SEM, AFM, Automated Gas Sorption Analyzer and Fluorescence measurements were used for characterizations and adsorption studies. The results confirm that all the synthesized nanoalloys have soft ferromagnetic nature and particles size were determined to be in the range of 8.60-12.19 nm. Adsorption performances of magnetic nanoalloys were investigated on bovine serum albumin (BSA) as a model protein. The results showed that prepared CoNi:PAAm composites have multistage adsorption kinetics for BSA and increasing Ni content in the CoNi nanoalloys enhance the adsorption rate constant and the rate constant can be tuned between 0.003 s-1 and 0.009 s-1 and between 0.01 s-1 and 0.60 s-1 for the first order adsorption and the second order adsorption stages, respectively. These results show that CoNi:PAAm composites can open new pathways for preparing a special composite material which has specific adsorption kinetic for bio-separation technology.

Global optimization of small bimetallic Pd-Co binary nanoalloy clusters: a genetic algorithm approach at the DFT level.

PubMed

Aslan, Mikail; Davis, Jack B A; Johnston, Roy L

2016-03-07

The global optimisation of small bimetallic PdCo binary nanoalloys are systematically investigated using the Birmingham Cluster Genetic Algorithm (BCGA). The effect of size and composition on the structures, stability, magnetic and electronic properties including the binding energies, second finite difference energies and mixing energies of Pd-Co binary nanoalloys are discussed. A detailed analysis of Pd-Co structural motifs and segregation effects is also presented. The maximal mixing energy corresponds to Pd atom compositions for which the number of mixed Pd-Co bonds is maximised. Global minimum clusters are distinguished from transition states by vibrational frequency analysis. HOMO-LUMO gap, electric dipole moment and vibrational frequency analyses are made to enable correlation with future experiments.

Calibration-free quantitative analysis of elemental ratios in intermetallic nanoalloys and nanocomposites using Laser Induced Breakdown Spectroscopy (LIBS).

PubMed

Davari, Seyyed Ali; Hu, Sheng; Mukherjee, Dibyendu

2017-03-01

Intermetallic nanoalloys (NAs) and nanocomposites (NCs) have increasingly gained prominence as efficient catalytic materials in electrochemical energy conversion and storage systems. But their morphology and chemical compositions play critical role in tuning their catalytic activities, and precious metal contents. While advanced microscopy techniques facilitate morphological characterizations, traditional chemical characterizations are either qualitative or extremely involved. In this study, we apply Laser Induced Breakdown Spectroscopy (LIBS) for quantitative compositional analysis of NAs and NCs synthesized with varied elemental ratios by our in-house built pulsed laser ablation technique. Specifically, elemental ratios of binary PtNi, PdCo (NAs) and PtCo (NCs) of different compositions are determined from LIBS measurements employing an internal calibration scheme using the bulk matrix species as internal standards. Morphology and qualitative elemental compositions of the aforesaid NAs and NCs are confirmed from Transmission Electron Microscopy (TEM) images and Energy Dispersive X-ray Spectroscopy (EDX) measurements. LIBS experiments are carried out in ambient conditions with the NA and NC samples drop cast on silicon wafers after centrifugation to increase their concentrations. The technique does not call for cumbersome sample preparations including acid digestions and external calibration standards commonly required in Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) techniques. Yet the quantitative LIBS results are in good agreement with the results from ICP-OES measurements. Our results indicate the feasibility of using LIBS in future for rapid and in-situ quantitative chemical characterizations of wide classes of synthesized NAs and NCs. Copyright © 2016 Elsevier B.V. All rights reserved.

Surface enrichment of Pt in stable Pt-Ir nano-alloy particles on MgAl 2 O 4 spinel in oxidizing atmosphere

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

Li, Wei-Zhen; Nie, Lei; Cheng, Yingwen

With the capability of MgAl2O4 spinel {111} nano-facets in stabilizing small Rh, Ir and Pt particles, bimetallic Ir-Pt catalysts on the same support were investigated, aiming at further lowering the catalyst cost by substituting expensive Pt with cheaper Ir in the bulk. Small Pt-Ir nano-alloy particles (< 2nm) were successfully stabilized on the spinel {111} nano-facets as expected. Interestingly, methanol oxidative dehydrogenation (ODH) rate on the surface Pt atoms increases with oxidizing aging but decreases upon reducing treatment, where Ir is almost inactive under the same reaction conditions. Up to three times enhancement in Pt exposure was achieved when themore » sample was oxidized at 800 °C in air for 1 week and subsequently reduced by H2 for 2 h, demonstrating successful surface enrichment of Pt on Pt-Ir nano-alloy particles. A dynamic stabilization mechanism involving wetting\

Surface Atomic Structure and Functionality of Metallic Nanoparticles: A Case Study of Au–Pd Nanoalloy Catalysts

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

Petkov, Valeri; Prasai, Binay; Shastri, Sarvjit

The surface atomic structure of metallic nanoparticles (NPs) plays a key role in shaping their physicochemical properties and response to external stimuli. Not surprisingly, current research increasingly focuses on exploiting its prime characteristics, including the amount, location, coordination, and electronic configuration of distinct surface atomic species, as tunable parameters for improving the functionality of metallic NPs in practical applications. The effort requires clear understanding of the extent to which changes in each of these characteristics would contribute to achieving the targeted functionality. This, in the first place, requires good knowledge of the actual surface of metallic NPs at atomic level.more » Through a case study on Au–Pd nanoalloy catalysts of industrial and environmental importance, we demonstrate that the surface atomic structure of metallic NPs can be determined in good detail by resonant high-energy X-ray diffraction (HE-XRD). Furthermore, using our experimental surface structure and CO oxidation activity data, we shed new light on the elusive origin of the remarkable catalytic synergy between surface Au and Pd atoms in the nanoalloys. In particular, we show that it arises from the formation of a specific “skin” on top of the nanoalloys that involves as many unlike, i.e., Au–Pd and Pd–Au, atomic pairs as possible given the overall chemical composition of the NPs. Moreover, unlike atoms from the “skin” interact strongly, including both changing their size and electronic structure in inverse proportions. That is, Au atoms shrink and acquire a partial positive charge of 5d-character whereas Pd atoms expand and become somewhat 4d-electron deficient. Accordingly, the reactivity of Au increases whereas Pd atoms become less reactive, as compared to atoms at the surface of pure Au and Pd NPs, respectively. Ultimately, this renders Au–Pd alloy NPs superb catalysts for CO oxidation reaction over a broad range of alloy

Surface Atomic Structure and Functionality of Metallic Nanoparticles: A Case Study of Au–Pd Nanoalloy Catalysts

DOE PAGES

Petkov, Valeri; Prasai, Binay; Shastri, Sarvjit; ...

2017-03-23

The surface atomic structure of metallic nanoparticles (NPs) plays a key role in shaping their physicochemical properties and response to external stimuli. Not surprisingly, current research increasingly focuses on exploiting its prime characteristics, including the amount, location, coordination, and electronic configuration of distinct surface atomic species, as tunable parameters for improving the functionality of metallic NPs in practical applications. The effort requires clear understanding of the extent to which changes in each of these characteristics would contribute to achieving the targeted functionality. This, in the first place, requires good knowledge of the actual surface of metallic NPs at atomic level.more » Through a case study on Au–Pd nanoalloy catalysts of industrial and environmental importance, we demonstrate that the surface atomic structure of metallic NPs can be determined in good detail by resonant high-energy X-ray diffraction (HE-XRD). Furthermore, using our experimental surface structure and CO oxidation activity data, we shed new light on the elusive origin of the remarkable catalytic synergy between surface Au and Pd atoms in the nanoalloys. In particular, we show that it arises from the formation of a specific “skin” on top of the nanoalloys that involves as many unlike, i.e., Au–Pd and Pd–Au, atomic pairs as possible given the overall chemical composition of the NPs. Moreover, unlike atoms from the “skin” interact strongly, including both changing their size and electronic structure in inverse proportions. That is, Au atoms shrink and acquire a partial positive charge of 5d-character whereas Pd atoms expand and become somewhat 4d-electron deficient. Accordingly, the reactivity of Au increases whereas Pd atoms become less reactive, as compared to atoms at the surface of pure Au and Pd NPs, respectively. Ultimately, this renders Au–Pd alloy NPs superb catalysts for CO oxidation reaction over a broad range of alloy

Effect of O2, N2 and H2 on annealing of pad printed high conductive Ag-Cu nano-alloy electrodes

NASA Astrophysics Data System (ADS)

Manjunath, G.; Anusha, P.; Salian, Ashritha; Gupta, Bikesh; Mandal, Saumen

2018-01-01

In this study, annealing of pad printed Ag-Cu based conducting ink was studied in oxidizing, inert and reducing atmosphere to verify its oxidation dependent conductivity. Ag-Cu manually was formulated adopting polyol method; where silver nitrate and copper nitrate serve as initial metal precursors. Polyvinylpyrrolidone (PVP), ethylene glycol and sodium borohydride act as a stabilizer, solvent and reducing agent respectively. The nanoalloys were with an average particle size ˜48 ± 15 nm, capped with polyvinylpyrrolidone to avoid agglomeration and stable in non-polar solvents. Formation of nanoalloy, Ag 90 wt%-Cu 10 wt%, was verified through a peak shift in UV-visible spectroscopy, found at 470 nm along with Nelson-Relay curve fitting and x-ray photoelectron spectroscopy study. The calculated lattice parameter of nanoalloy ˜4.034 Å, was in between pure silver and copper. The crystallite size was calculated using Debye-Scherrer, Williamson-Hall isotropic strain model and Halder-Wagner method. Electrode patterns were printed on a glass substrate by pad printing and were annealed under O2, N2 and H2 atmosphere to study the oxidation kinetics of copper. A maximum conductivity of -6.6 × 105 S m-1 was observed in inert atmosphere annealing as the conductivity is solely depends on the oxidation of copper; appears with uttermost Cu0 and least Cu2+ in x-ray photoelectron spectroscopy. High conductive space required between manually and dispersion ink can have a potential application as an electrode in printed electronics. Further refinement of size of the nanopaticles by polyol method could help to obtain the effect of quantum confinement.

Surface enrichment of Pt in stable Pt-Ir nano-alloy particles on MgAl 2O 4 spinel in oxidizing atmosphere

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

Li, Wei -Zhen; Nie, Lei; Cheng, Yingwen

With the capability of MgAl 2O 4 spinel {111} nano-facets in stabilizing small Rh, Ir and Pt particles, bimetallic Ir-Pt catalysts on the same support were investigated in this paper, aiming at further lowering the catalyst cost by substituting expensive Pt with cheaper Ir in the bulk. Small Pt-Ir nano-alloy particles (< 2 nm) were successfully stabilized on the spinel {111} nano-facets as expected. Interestingly, methanol oxidative dehydrogenation (ODH) rate on the surface Pt atoms increases with oxidizing aging but decreases upon reducing treatment, where Ir is almost inactive under the same reaction conditions. Up to three times enhancement inmore » Pt exposure was achieved when the sample was oxidized at 800 °C in air for 1 week and subsequently reduced by H 2 for 2 h, demonstrating successful surface enrichment of Pt on Pt-Ir nano-alloy particles. Finally, a dynamic stabilization mechanism involving wetting/nucleation seems to be responsible for the evolution of surface compositions upon cyclic oxidizing and reducing thermal treatments.« less

Surface enrichment of Pt in stable Pt-Ir nano-alloy particles on MgAl 2O 4 spinel in oxidizing atmosphere

DOE PAGES

Li, Wei -Zhen; Nie, Lei; Cheng, Yingwen; ...

2017-01-13

With the capability of MgAl 2O 4 spinel {111} nano-facets in stabilizing small Rh, Ir and Pt particles, bimetallic Ir-Pt catalysts on the same support were investigated in this paper, aiming at further lowering the catalyst cost by substituting expensive Pt with cheaper Ir in the bulk. Small Pt-Ir nano-alloy particles (< 2 nm) were successfully stabilized on the spinel {111} nano-facets as expected. Interestingly, methanol oxidative dehydrogenation (ODH) rate on the surface Pt atoms increases with oxidizing aging but decreases upon reducing treatment, where Ir is almost inactive under the same reaction conditions. Up to three times enhancement inmore » Pt exposure was achieved when the sample was oxidized at 800 °C in air for 1 week and subsequently reduced by H 2 for 2 h, demonstrating successful surface enrichment of Pt on Pt-Ir nano-alloy particles. Finally, a dynamic stabilization mechanism involving wetting/nucleation seems to be responsible for the evolution of surface compositions upon cyclic oxidizing and reducing thermal treatments.« less

Superconducting properties of Nb-Cu nano-composites and nano-alloys

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

Parab, Pradnya, E-mail: pradnyaprb@gmail.com; Kumar, Sanjeev; Bhui, Prabhjyot

The evolution of the superconducting transition temperature (T{sub c}) in nano-composite and nano-alloys of Nb-Cu, grown by DC magnetron co-sputtering are investigated. Microstructure of these films depends less strongly on the ratio of Nb:Cu but more on the growth temperature. At higher growth temperature, phase separated granular films of Nb and Cu were formed which showed superconducting transition temperatures (T{sub c}) of ~ 7.2±0.5 K, irrespective of the composition. Our results show that this is primarily influenced by the microstructure of the films determined during growth which rules out the superconducting proximity effect expected in these systems. At room temperaturemore » growth, films with nano-scale alloying were obtained at the optimal compositional range of 45-70 atomic% (At%) of Nb. These were also superconducting with a T{sub c} of 3.2 K.« less

A simple resonance Rayleigh scattering method for determination of trace CA125 using immuno-AuRu nanoalloy as probe via ultrasonic irradiation

NASA Astrophysics Data System (ADS)

Tang, Meiling; Wen, Guiqing; Luo, Yanghe; Liang, Aihui; Jiang, Zhiliang

2015-01-01

AuRu nanoalloy (GR) with Au/Ru molar ratio of 32/1 was prepared by the sodium borohydride reduction method. It was used to label the CA125 antibody (Ab) to obtain an immunonanoprobe (GRAb) for cancer antigen 125 (CA125). In pH 7.0 citric acid-Na2HPO4 buffer solution and irradiation of ultrasound, the probes were aggregated nonspecifically to big clusters that showed a strong resonance Rayleigh scattering (RRS) peak at 278 nm. Upon addition of CA125, GRAb reacted specifically with CA125 to form dispersive immunocomplexes of CA125-GRAb in the solution and this process enhanced by the ultrasonic cavitation effect, which led to the RRS intensity decreased greatly. The decreased RRS intensity was linear to the concentration of CA125 in the range of 1.3-80 U/mL, with a detection limit of 0.6 U/mL. The proposed method was applied to detect CA125 in real sample, with satisfactory results.

Composition Dependence of the Properties of Noble-metal Nanoalloys

NASA Astrophysics Data System (ADS)

Fernández Seivane, Lucas; Barrón, Héctor; Benson, James; Weissker, Hans-Christian; López-Lozano, Xochitl

2012-03-01

Bimetallic nanostructured materials are of greater interest both from the scientific and technological points of view due to their potential to improve the catalytic properties of novel materials. Their applicability as well as the performance depends critically on their size, shape and composition, either as alloy or core-shell. In this work, the structural, electronic, magnetic and optical properties of bimetallic Au-Ag nanoclusters have been investigated through density-functional-theory-based calculations with the Siesta and Octopus codes. Different symmetries -tetrahedral, bipyramidal, decahedral and icosahedral- of bimetallic nanoparticles of 4-, 5-, 7- and 13-atoms, were taken into account including all the possibly different Au:Ag ratio concentrations. In combination with a statistical analysis of the performed calculations and the concepts of the Enthalpy of Mixing and Energy Excess, we have been able to predict the most probable gap and magnetic moment for all the composition stoichiometries. This approach allows us to understand the energy differences due to cluster shape effects, the stoichiometry and segregation. In addition, we can also obtain the bulk energy and surface energy of Au-Ag nanoalloys by looking at fixed number of atoms and fixed morphologies.

Oromucosal film preparations: classification and characterization methods.

PubMed

Preis, Maren; Woertz, Christina; Kleinebudde, Peter; Breitkreutz, Jörg

2013-09-01

Recently, the regulatory authorities have enlarged the variety of 'oromucosal preparations' by buccal films and orodispersible films. Various film preparations have entered the market and pharmacopoeias. Due to the novelty of the official monographs, no standardized characterization methods and quality specifications are included. This review reports the methods of choice to characterize oromucosal film preparations with respect to biorelevant characterization and quality control. Commonly used dissolution tests for other dosage forms are not transferable for films in all cases. Alternatives and guidance on decision, which methods are favorable for film preparations are discussed. Furthermore, issues about requirements for film dosage forms are reflected. Oromucosal film preparations offer a wide spectrum of opportunities. There are a lot of suggestions in the literature on how to control the quality of these innovative products, but no standardized tests are available. Regulatory authorities need to define the standards and quality requirements more precisely.

The Preparation and Characterization of Materials.

ERIC Educational Resources Information Center

Wold, Aaron

1980-01-01

Presents several examples illustrating different aspects of materials problems, including problems associated with solid-solid reactions, sintering and crystal growth, characterization of materials, preparation and characterization of stoichiometric ferrites and chromites, copper-sulfur systems, growth of single crystals by chemical vapor…

Synthesis of Bimetallic Platinum Nanoparticles for Biosensors

PubMed Central

Leteba, Gerard M.; Lang, Candace I.

2013-01-01

The use of magnetic nanomaterials in biosensing applications is growing as a consequence of their remarkable properties; but controlling the composition and shape of metallic nanoalloys is problematic when more than one precursor is required for wet chemistry synthesis. We have developed a successful simultaneous reduction method for preparation of near-spherical platinum-based nanoalloys containing magnetic solutes. We avoided particular difficulties in preparing platinum nanoalloys containing Ni, Co and Fe by the identification of appropriate synthesis temperatures and chemistry. We used transmission electron microscopy (TEM) to show that our particles have a narrow size distribution, uniform size and morphology, and good crystallinity in the as-synthesized condition. Energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) confirms the coexistence of Pt with the magnetic solute in a face-centered cubic (FCC) solid solution. PMID:23941910

Intrinsic magnetic properties of bimetallic nanoparticles elaborated by cluster beam deposition.

PubMed

Dupuis, V; Khadra, G; Hillion, A; Tamion, A; Tuaillon-Combes, J; Bardotti, L; Tournus, F

2015-11-14

In this paper, we present some specific chemical and magnetic order obtained very recently on characteristic bimetallic nanoalloys prepared by mass-selected Low Energy Cluster Beam Deposition (LECBD). We study how the competition between d-atom hybridization, complex structure, morphology and chemical affinity affects their intrinsic magnetic properties at the nanoscale. The structural and magnetic properties of these nanoalloys were investigated using various experimental techniques that include High Resolution Transmission Electron Microscopy (HRTEM), Superconducting Quantum Interference Device (SQUID) magnetometry, as well as synchrotron techniques such as Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Magnetic Circular Dichroism (XMCD). Depending on the chemical nature of the nanoalloys we observe different magnetic responses compared to their bulk counterparts. In particular, we show how specific relaxation in nanoalloys impacts their magnetic anisotropy; and how finite size effects (size reduction) inversely enhance their magnetic moment.

Pd surface and Pt subsurface segregation in Pt1-c Pd c nanoalloys

NASA Astrophysics Data System (ADS)

De Clercq, A.; Giorgio, S.; Mottet, C.

2016-02-01

The structure and chemical arrangement of Pt1-c Pd c nanoalloys with the icosahedral and face centered cubic symmetry are studied using Monte Carlo simulations with a tight binding interatomic potential fitted to density-functional theory calculations. Pd surface segregation from the lowest to the highest coordinated sites is predicted by the theory together with a Pt enrichment at the subsurface, whatever the structure and the size of the nanoparticles, and which subsists when increasing the temperature. The onion-shell chemical configuration is found for both symmetries and is initiated from the Pd surface segregation. It is amplified in the icosahedral symmetry and small sizes but when considering larger sizes, the oscillating segregation profile occurs near the surface on about three to four shells whatever the structure. Pd segregation results from the significant lower cohesive energy of Pd as compared to Pt and the weak ordering tendency leads to the Pt subsurface segregation. The very weak size mismatch does not prevent the bigger atoms (Pt) from occupying subsurface sites which are in compression whereas the smaller ones (Pd) occupy the central site of the icosahedra where the compression is an order of magnitude higher.

Charting the relationship between phase type-surface area-interactions between the constituent atoms and oxygen reduction activity of Pd–Cu nanocatalysts inside fuel cells by in operando high-energy X-ray diffraction

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

Maswadeh, Yazan; Shan, Shiyao; Prasai, Binay

The activity and stability of nanoalloy catalysts for chemical reactions driving devices for clean energy conversion, in particular the oxygen reduction reaction (ORR), depend critically on optimizing major structural characteristics of the nanoalloys, such as the phase composition, surface area and bonding interactions between the constituent atoms, for the harsh operating conditions inside the devices. The effort requires good knowledge of the potential effect of changes in these characteristics on the catalytic functionality of the nanoalloys and, hence, on the devices' performance. We present the results from an in operando high-energy X-ray diffraction (HE-XRD) study on the concurrent changes inmore » the structural characteristics and ORR activity of Pd–Cu nanoalloy catalysts as they function at the cathode of a proton exchange membrane fuel cell (PEMFC). We find that the as-prepared Pd–Cu nanoalloys with a chemical composition close to Pd1Cu1 are better ORR catalysts in comparison with Pd1Cu2, i.e. Pd-poor, and Pd3Cu1, i.e. Pd-rich, nanoalloys. Under operating conditions though, the former suffers a big loss in ORR activity appearing as a slow-mode oscillation in the current output of the PEMFC. Losses in ORR activity suffered by the latter also exhibit sudden drops and rises during the PEMFC operation. Through atomic pair distribution function (PDF) analysis of the in operando HE-XRD data, we identify the structural changes of Pd–Cu alloy NPs that are behind the peculiar decay of their ORR activity. The results uncover the instant link between the ever-adapting structural state of ORR nanocatalysts inside an operating PEMFC and the performance of the PEMFC. Besides, our results indicate that, among others, taking control over the intra-particle diffusion of metallic species in nanoalloy catalysts may improve the performance of PEMFCs significantly and, furthermore, in operando HE-XRD can be an effective tool to guide the effort. Finally, we argue

Ruthenium-cobalt nanoalloys encapsulated in nitrogen-doped graphene as active electrocatalysts for producing hydrogen in alkaline media

NASA Astrophysics Data System (ADS)

Su, Jianwei; Yang, Yang; Xia, Guoliang; Chen, Jitang; Jiang, Peng; Chen, Qianwang

2017-04-01

The scalable production of hydrogen could conveniently be realized by alkaline water electrolysis. Currently, the major challenge confronting hydrogen evolution reaction (HER) is lacking inexpensive alternatives to platinum-based electrocatalysts. Here we report a high-efficient and stable electrocatalyst composed of ruthenium and cobalt bimetallic nanoalloy encapsulated in nitrogen-doped graphene layers. The catalysts display remarkable performance with low overpotentials of only 28 and 218 mV at 10 and 100 mA cm-2, respectively, and excellent stability of 10,000 cycles. Ruthenium is the cheapest platinum-group metal and its amount in the catalyst is only 3.58 wt.%, showing the catalyst high activity at a very competitive price. Density functional theory calculations reveal that the introduction of ruthenium atoms into cobalt core can improve the efficiency of electron transfer from alloy core to graphene shell, beneficial for enhancing carbon-hydrogen bond, thereby lowing ΔGH* of HER.

Nanophase diagram of binary eutectic Au-Ge nanoalloys for vapor-liquid-solid semiconductor nanowires growth

NASA Astrophysics Data System (ADS)

Lu, Haiming; Meng, Xiangkang

2015-06-01

Although the vapor-liquid-solid growth of semiconductor nanowire is a non-equilibrium process, the equilibrium phase diagram of binary alloy provides important guidance on the growth conditions, such as the temperature and the equilibrium composition of the alloy. Given the small dimensions of the alloy seeds and the nanowires, the known phase diagram of bulk binary alloy cannot be expected to accurately predict the behavior of the nanowire growth. Here, we developed a unified model to describe the size- and dimensionality-dependent equilibrium phase diagram of Au-Ge binary eutectic nanoalloys based on the size-dependent cohesive energy model. It is found that the liquidus curves reduce and shift leftward with decreasing size and dimensionality. Moreover, the effects of size and dimensionality on the eutectic composition are small and negligible when both components in binary eutectic alloys have the same dimensionality. However, when two components have different dimensionality (e.g. Au nanoparticle-Ge nanowire usually used in the semiconductor nanowires growth), the eutectic composition reduces with decreasing size.

Preparation and Characterization of PETI-330/Multiwalled Carbon Nanotube

NASA Technical Reports Server (NTRS)

Ghose, Sayata; Watson, Kent A.; Working, Dennis C.; Criss, Jim M.; Siochi, Emilie J.; Connell, John W.

2005-01-01

As part of an ongoing effort to incorporate multifunctionality into advanced composites, blends of PETI-330 and multi-walled carbon nanotubes (MWCNTs) were prepared, characterized and fabricated into moldings. The PETI-330/MWCNT mixtures were prepared at concentrations ranging from 3 to 25 weight percent by dry mixing the components in a ball mill. The resulting powders were characterized for degree of mixing, thermal and rheological properties. Based on the characterization results, PETI-330/MWCNT samples were scaled up to 300 g and used to fabricate moldings 10.2 cm x 15.2 cm x 0.32 cm thick. The moldings were made by injecting the mixtures at 260-280 C into an Invar tool followed by curing for 1 h at 371 C. The tool was designed to impart shear during the injection process in an attempt to achieve some alignment of the MWCNTs in the flow direction. Good quality moldings were obtained that were subsequently characterized for thermal, mechanical and electrical properties. The degree of dispersion and alignment of the MWCNTs were investigated using high-resolution scanning electron microscopy. The preparation and preliminary characterization of PETI-330/MWCNT composites will be discussed. Keywords: phenylethynyl terminated imides, high temperature polymers, nanocomposites, moldings

Preparation and Characterization of Natural Rubber/Organophilic Clay Nanocomposites

NASA Astrophysics Data System (ADS)

Gonzales-Fernandes, M.; Esper, F. J.; Silva-Valenzuela, M. G.; Martín-Cortés, G. R.; Valenzuela-Diaz, F. R.; Wiebeck, H.

Natural rubber/organophilic clay nanocomposites were prepared and characterized. A brown bentonite from Paraiba's State, Brazil was modified with a sodium salt and treated with quaternary ammonium salt hexadecyltrimethyl ammonium chloride. The clay in its natural state, after cation exchange with sodium and after organophilization was characterized by XRD, IR, SEM, thermal analysis. Nanocomposite samples were prepared containing 10 resin percent of organophilic clay. The vulcanized samples were analyzed by XRD, SEM. The nanocomposites obtained showed improvement in their mechanical properties in comparison with samples without clay.

Preparation and Characterization of Cabamazepine Cocrystal in Polymer Solution.

PubMed

Zhang, Hao; Zhu, Ying; Qiao, Ning; Chen, Yang; Gao, Linghuan

2017-12-01

In this study, we attempted to prepare carbamazepine (CBZ) cocrystal through the solution method in ethanol-water solvent mixture (volume ratio 1:1) and polyvinyl pyrrolidone (PVP) solution. Nicotinamide (NIC) and saccharin (SAC) were selected as cocrystal coformers. Cocrystal screening products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Powder X-ray Diffraction (PXRD) techniques. Characterization results show that in ethanol-water solvent mixture, pure CBZ-NIC cocrystal can be prepared, while CBZ-SAC cocrystal cannot be obtained. The addition of PVP can inhibit CBZ-NIC cocrystal formation and facilitate CBZ-SAC cocrystal formation.

Preparation and Characterization of Carbamazepine Cocrystal in Polymer Solution

PubMed Central

Zhang, Hao; Zhu, Ying; Chen, Yang; Gao, Linghuan

2017-01-01

In this study, we attempted to prepare carbamazepine (CBZ) cocrystal through the solution method in ethanol-water solvent mixture (volume ratio 1:1) and polyvinyl pyrrolidone (PVP) solution. Nicotinamide (NIC) and saccharin (SAC) were selected as cocrystal coformers. Cocrystal screening products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Powder X-ray Diffraction (PXRD) techniques. Characterization results show that in ethanol-water solvent mixture, pure CBZ-NIC cocrystal can be prepared, while CBZ-SAC cocrystal cannot be obtained. The addition of PVP can inhibit CBZ-NIC cocrystal formation and facilitate CBZ-SAC cocrystal formation. PMID:29194387

Preparation and Characterization of PETI-330/Multiwalled Carbon Nanotube Composites

NASA Technical Reports Server (NTRS)

Ghose, Sayata; Watson, Kent A.; Working, Dennis C.; Delozier, Donavon M.; Criss, Jim M.; Siochi, Emilie J.; Connell, John W.

2005-01-01

As part of an ongoing effort to incorporate multi-functionality into advanced composites, blends of PETI-330 and multi-walled carbon nanotubes (MWCNTs) were prepared, characterized and fabricated into moldings. The PETI-330/MWCNT mixtures were prepared at concentrations ranging from 3 to 25 weight percent by dry mixing the components in a ball mill. The resulting powders were characterized for degree of mixing, thermal and rheological properties. Based on the characterization results, PETI-330/MWCNT samples were scaled up to approx. 300 g and used to fabricate moldings 10.2 cm x 15.2 cm x 0.32 cm thick. The moldings were fabricated by injecting the mixtures at 260-280 C into a stainless steel tool followed by curing for 1 h at 371 C. The tool was designed to impart high shear during the injection process in an attempt to achieve some alignment of the MWCNTs in the flow direction. Good quality moldings were obtained that were subsequently characterized for thermal, mechanical and electrical properties. The degree of dispersion and alignment of the MWCNTs were investigated using high-resolution scanning electron microscopy and Raman spectroscopy. The preparation and preliminary characterization of PETI-330/MWCNT composites will be discussed. Keywords: phenylethynyl terminated imides, high temperature polymers, nanocomposites,

Preparation and Characterization of Hydroxyapatite-Silica Composite Nanopowders

NASA Astrophysics Data System (ADS)

Latifi, S. M.; Fathi, M. H.; Golozar, M. A.

One of the most important objectives in the field of biomaterials science and engineering is development of new materials as bone substitutes. Silica (SiO2) has an important role in the biomineralization and biological responses. The aim of this research was to prepare and characterize hydroxyapatite-silica (HA-SiO2) composite nanopowder with different content of silica. Hydroxyapatite-silica composite nanopowders with 20 and 40 wt% silica were prepared using a sol-gel method at 600°C with phosphoric pentoxide and calcium nitrate tetrahydrate as a source of hydroxyapatite; also, tetraethylorthosilicate and methyltriethoxisilane as a source of silica. Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX) techniques were used for characterization and evaluation of the products. The results indicated the presence of nanocrystalline hydroxyapatite phase beside amorphous silica phase in prepared composite nanopowders. Moreover, by increasing the content of silica in composite nanopowders, the crystallinity will be decreased,and the ability of the product as a bone substitute material might be controlled by changing the content of the ingredients and subsequently its structure.

Preparation of surface enhanced Raman substrate and its characterization

NASA Astrophysics Data System (ADS)

Liu, Y.; Wang, J. Y.; Wang, J. Q.

2017-10-01

Surface enhanced Raman spectroscopy (SERS) is a fast, convenient and highly sensitive detection technique, and preparing the good effect and repeatable substrate is the key to realize the trace amount and quantitative detection in the field of food safety detection. In this paper, a surface enhanced Raman substrate based on submicrometer silver particles structure was prepared by chemical deposition method, and characterized its structure and optical properties.

Chromatography in the detection and characterization of illegal pharmaceutical preparations.

PubMed

Deconinck, Eric; Sacré, Pierre-Yves; Courselle, Patricia; De Beer, Jacques O

2013-09-01

Counterfeit and illegal pharmaceutical products are an increasing worldwide problem and constitute a major challenge for analytical laboratories to detect and characterize them. Spectroscopic techniques such as infrared spectroscopy and Raman spectroscopy have always been the first methods of choice to detect counterfeits and illegal preparations, but due to the evolution in the seized products and the necessity of risk assessment, chromatographic methods are becoming more important in this domain. This review intends to give a general overview of the techniques described in literature to characterize counterfeit and illegal pharmaceutical preparations, focusing on the role of chromatographic techniques with different detection tools.

Advanced Research Projects Agency on Materials Preparation and Characterization Research

DTIC Science & Technology

Briefly summarized is research concerned with such topics as: Preparation of silica glass from amorphous silica; Glass structure by Raman ...ferroelectrics; Silver iodide crystals; Vapor phase growth; Refractory optical host materials; Hydroxyapatite ; Calcite; Characterization of single crystals with a double crystal spectrometer; Characterization of residual strain.

Low temperature synthesis of Ru-Cu alloy nanoparticles with the compositions in the miscibility gap

NASA Astrophysics Data System (ADS)

Martynova, S. A.; Filatov, E. Yu.; Korenev, S. V.; Kuratieva, N. V.; Sheludyakova, L. A.; Plusnin, P. E.; Shubin, Yu. V.; Slavinskaya, E. M.; Boronin, A. I.

2014-04-01

A complex salt [Ru(NH3)5Cl][Cu(C2O4)2H2O]-the precursor of nanoalloys combining ruthenium and copper was prepared. It crystallizes in the monoclinic space group P21/n. Thermal properties of the prepared salt were examined in different atmospheres (helium, hydrogen, oxygen). Thermal decomposition of the precursor in inert atmosphere was thoroughly examined and the intermediate products were characterized. Experimental conditions for preparation of copper-rich (up to 12 at% of copper) metastable solid solution CuxRu1-x (based on Ru structure) were optimized, what is in sharp contrast to the bimetallic miscibility gap known for the bulk counterparts in a wide composition range. Catalytic properties of copper-ruthenium oxide composite were tested in catalytic oxidation of CO.

Pt/Au nanoalloy supported on alumina and chlorided alumina: DFT and experimental analysis

NASA Astrophysics Data System (ADS)

Sharifi, N.; Falamaki, C.; Ghorbanzadeh Ahangari, M.

2018-04-01

Density functional theory (DFT) was used to explore the adsorption of Pt/Au nanoalloy onto a pure and chlorided γ-Al2O3(110) surface, which has been applied in numerous catalytic reactions. First, we considered the adsorption properties of Pt clusters (n ≤ 5) onto the Al2O3(110) surface to determine the most stable Pt cluster on alumina surface in reforming processes. After full structural relaxations of Pt clusters at various configurations on alumina, our computed results expressed that the minimum binding energy (‑5.67 eV) is accrued for Pt4 cluster and the distance between the nearest Pt atom in the cluster to the alumina surface is equal to 1.13 Å. Then, we investigated the binding energies, geometries, and electronic properties of adsorbed Aun clusters (n ≤ 6) on the γ-Al2O3(110) surface. Our studied showed that Au5 was the most thermodynamically stable structure on γ-Al2O3. Finally, we inspected these properties for adsorbed Au clusters onto the Pt4-decorated alumina (Aun/Pt4-alumina) system. The binding energy of the Au4/Pt4-alumina system was ‑5.01 eV, and the distance between Au4 cluster and Pt4-alumina was 1.33 Å. The Au4/Pt4alumina system was found to be the most stable nanometer-sized catalyst design. At last, our first-principles calculations predicted that the best position of embedment Cl on the Au4/Pt4-alumina.

Preparation and Characterization of New Geopolymer-Epoxy Resin Hybrid Mortars

PubMed Central

Colangelo, Francesco; Roviello, Giuseppina; Ricciotti, Laura; Ferone, Claudio; Cioffi, Raffaele

2013-01-01

The preparation and characterization of metakaolin-based geopolymer mortars containing an organic epoxy resin are presented here for the first time. The specimens have been prepared by means of an innovative in situ co-reticulation process, in mild conditions, of commercial epoxy based organic resins and geopolymeric slurry. In this way, geopolymer based hybrid mortars characterized by a different content of normalized sand (up to 66% in weight) and by a homogeneous dispersion of the organic resin have been obtained. Once hardened, these new materials show improved compressive strength and toughness in respect to both the neat geopolymer and the hybrid pastes since the organic polymer provides a more cohesive microstructure, with a reduced amount of microcracks. The microstructural characterization allows to point out the presence of an Interfacial Transition Zone similar to that observed in cement based mortars and concretes. A correlation between microstructural features and mechanical properties has been studied too. PMID:28811418

Preparation and Characterization of Polymeric Nanoparticles: An Interdisciplinary Experiment

ERIC Educational Resources Information Center

Ramalho, Maria J.; Pereira, M. Carmo

2016-01-01

In this work, a laboratory experiment to introduce graduate students to nanotechnology is described. Students prepared poly(lactic-"co"-glycolic acid) (PLGA) nanoparticles using two different synthesis procedures, a single and a double emulsion-solvent evaporation method. The students also performed a physicochemical characterization of…

Preparation and characterization of antimony barium composite oxide photocatalysts

NASA Astrophysics Data System (ADS)

Han, X. P.; Yao, B. H.; Pan, Q. H.; Pen, C.; Zhang, C. L.

2018-01-01

In this paper, two kinds of antimony barium composite oxide photocatalysts have been prepared by two methods and characterized by XRD and SEM. The photocatalytic activity was evaluated by a photocatalytic reactor and an ultraviolet spectrophotometer. The results showed that-BaSb2O5•4H2O, BaSb2O6 two kinds of antimony barium composite oxide photocatalysts were successfully prepared in this experiment and they showed good photocatalytic properties. In addition, BaSb2O6 morphology showed more regular, microstructure and better catalytic performance.

Preparation and characterization of supported magnetic nanoparticles prepared by reverse micelles

PubMed Central

Han, Luyang; Biskupek, Johannes; Kaiser, Ute; Ziemann, Paul

2010-01-01

Summary Monatomic (Fe, Co) and bimetallic (FePt and CoPt) nanoparticles were prepared by exploiting the self-organization of precursor loaded reverse micelles. Achievements and limitations of the preparation approach are critically discussed. We show that self-assembled metallic nanoparticles can be prepared with diameters d = 2–12 nm and interparticle distances D = 20–140 nm on various substrates. Structural, electronic and magnetic properties of the particle arrays were characterized by several techniques to give a comprehensive view of the high quality of the method. For Co nanoparticles, it is demonstrated that magnetostatic interactions can be neglected for distances which are at least 6 times larger than the particle diameter. Focus is placed on FePt alloy nanoparticles which show a huge magnetic anisotropy in the L10 phase, however, this is still less by a factor of 3–4 when compared to the anisotropy of the bulk counterpart. A similar observation was also found for CoPt nanoparticles (NPs). These results are related to imperfect crystal structures as revealed by HRTEM as well as to compositional distributions of the prepared particles. Interestingly, the results demonstrate that the averaged effective magnetic anisotropy of FePt nanoparticles does not strongly depend on size. Consequently, magnetization stability should scale linearly with the volume of the NPs and give rise to a critical value for stability at ambient temperature. Indeed, for diameters above 6 nm such stability is observed for the current FePt and CoPt NPs. Finally, the long-term conservation of nanoparticles by Au photoseeding is presented. PMID:21977392

Preparation and Characterization of Fluorescent SiO2 Microspheres

NASA Astrophysics Data System (ADS)

Xu, Cui; Zhang, Hao; Guan, Ruifang

2018-01-01

Fluorescent compound without typical fluorophores was synthesized with citric acid (CA) and aminopropyltriethoxysilane (APTS) firstly, and then it was grafted to the surface of the prepared SiO2 microspheres by chemical reaction. The fluorescent SiO2 microspheres with good fluorescent properties were obtained by optimizing the reaction conditions. And the morphology and structure of the fluorescent SiO2 microspheres have been characterized by scanning electron microscopy (SEM) and fourier transform infrared (FTIR) spectroscopy. The results showed that the preparation of fluorescent SiO2 microspheres have good monodispersity and narrow particle size distribution. Moreover, the fluorescent SiO2 microspheres can be applied to detect Fe3+ in aqueous solution, prepare fluorescent SiO2 rubber, and have potential to be applied in the fluorescent labeling and fingerprint appearing technique fields.

Tamoxifen citrate loaded ethosomes for transdermal drug delivery system: preparation and characterization.

PubMed

Sarwa, Khomendra Kumar; Suresh, Preeti K; Debnath, Manabendra; Ahmad, Mohammad Zaki

2013-08-01

Long term tamoxifen citrate therapy is imperative to treat several dermatological and hormonal sensitive disorders. Successful oral and parenteral administration of tamoxifen citrate has been challenging since it undergoes enzymatic degradation and has poor aqueous solubility issues. In the present work, tamoxifen citrate loaded ethosomes were prepared and characterized for transdermal applications. The prepared formulations were characterized for morphological features, particle size distribution, calorimetric attributes, zeta potential and drug entrapment. Permeation profile of prepared ethosomes was compared with liposomes and hydroethonalic solution across cellophane membrane and human cadaver skin. Results of the permeation studies indicate that ethosomes were able to deliver >90% drug within 24 hours of application, while liposomes and hydroethanolic solution delivered only 39.04% and 36.55% respectively. Skin deposition and stability studies are also reported.

Preparation, characterization and thermolysis of phenylenediammonium dinitrate salts.

PubMed

Kapoor, Inder Pal Singh; Srivastava, Pratibha; Singh, Gurdip

2008-02-11

Four phenylenediammonium dinitrate salts were prepared and characterized by elemental, Infrared spectroscopy (IR), Ultraviolet spectroscopy (UV) and gravimetric methods. These dinitrates find application in propellant, explosives and pyrotechnics. Their thermal decomposition has been studied using thermogravimetry (TG) and simultaneous thermogravimetry-differential scanning calorimetry (TG-DSC). Kinetics parameters were evaluated by model fitting and isoconversional methods. Their thermolytic pathways have also been suggested, which involves decomposition followed by ignition.

Preparation and Characterization of Activated Alumina

NASA Astrophysics Data System (ADS)

Rabia, A. R.; Ibrahim, A. H.; Zulkepli, N. N.

2018-03-01

Activated alumina is a high surface area and highly porous form of aluminum oxide that can be employed for contaminant species adsorb from ether gases or liquids without changing its form. The research in getting this material has generated huge interested. Thus, this paper presented preparation of activated alumina from chemical process. Pure aluminum (99.9% pure) reacted at room temperature with an aqueous NaOH in a reactor to produce a solution of sodium aluminate (NaAlO2). This solution was passed through filter paper and the clear filtrate was neutralized with H2SO4, to pH 6, 7 or 8, resulting in the precipitation of a white gel, Al(OH)3·XH2O. The washed gel for sulfate ions were dried at 80 °C for 6 h, a 60 mesh sieve was to separate and sort them into different sizes. The samples were then calcined (burn) for 3h in a muffle furnace, in air, at a heating rate of 2 °C min-1. The prepared activated alumina was further characterized for better understanding of its physical properties in order to predict its chemical mechanism.

Characterization and morphology of prepared titanium dioxide nanofibers by electrospinning.

PubMed

Park, Ju-Young; Lee, In-Hwa

2010-05-01

Dispersed titanium dioxide in polymer nanofibers were prepared by sol-gel processing and electrospinning techniques using titanium isopropoxide (TiP)/polyvinylpyrrolidone (PVP) solution. The prepared titanium dioxide nanofibers were characterized by FE-SEM, TEM, XRD, and FT-IR. Pure titanium dioxide nanofibers were obtained from calcination of inorganic-organic composite fiber. The diameter of titanium oxide nanofibers were in the range of 70 nm to 150 nm. Prepared titanium dioxide nanofibers show rough surface and rather small diameter compare with TiP/PVP composite nanofibers. After calcined at 500 degrees C, TiO2 nanofibers convert into anatase and rutile mixed phased from amorphous structure. Calcination of these composite fibers above 600 degrees C resulted in pure rutile TiO2 nanofibers.

Preparation and Characterization of Colloidal Silica Particles under Mild Conditions

ERIC Educational Resources Information Center

Neville, Frances; Zin, Azrinawati Mohd.; Jameson, Graeme J.; Wanless, Erica J.

2012-01-01

A microscale laboratory experiment for the preparation and characterization of silica particles at neutral pH and ambient temperature conditions is described. Students first employ experimental fabrication methods to make spherical submicrometer silica particles via the condensation of an alkoxysilane and polyethyleneimine, which act to catalyze…

Preparation, characterization and antimicrobial efficiency of Ag/PDDA-diatomite nanocomposite.

PubMed

Panáček, Aleš; Balzerová, Anna; Prucek, Robert; Ranc, Václav; Večeřová, Renata; Husičková, Vendula; Pechoušek, Jiří; Filip, Jan; Zbořil, Radek; Kvítek, Libor

2013-10-01

Nanocomposites consisting of diatomaceous earth particles and silver nanoparticles (silver NPs) with high antimicrobial activity were prepared and characterized. For the purpose of nanocomposite preparation, silver NPs with an average size of 28nm prepared by modified Tollens process were used. Nanocomposites were prepared using poly(diallyldimethylammonium) chloride (PDDA) as an interlayer substance between diatomite and silver NPs which enables to change diatomite original negative surface charge to positive one. Due to strong electrostatic interactions between negatively charged silver NPs and positively charged PDDA-modified diatomite, Ag/PDDA-diatomite nanocomposites with a high content of silver (as high as 46.6mgAg/1g of diatomite) were prepared. Because of minimal release of silver NPs from prepared nanocomposites to aqueous media (<0.3mg Ag/1g of nanocomposite), the developed nanocomposites are regarded as a potential useful antimicrobial material with a long-term efficiency showing no risk to human health or environment. All the prepared nanocomposites exhibit a high bactericidal activity against Gram-negative and Gram-positive bacteria and fungicidal activity against yeasts at very low concentrations as low as 0.11g/L, corresponding to silver concentration of 5mg/L. Hence, the prepared nanocomposites constitute a promising candidate suitable for the microbial water treatment in environmental applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Gold-Copper Nanoparticles: Nanostructural Evolution and Bifunctional Catalytic Sites

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

Yin, Jun; Shan, Shiyao; Yang, Lefu

2012-12-12

Understanding of the atomic-scale structure is essential for exploiting the unique catalytic properties of any nanoalloy catalyst. This report describes novel findings of an investigation of the nanoscale alloying of gold-copper (AuCu) nanoparticles and its impact on the surface catalytic functions. Two pathways have been explored for the formation of AuCu nanoparticles of different compositons, including wet chemical synthesis from mixed Au- and Cu-precursor molecules, and nanoscale alloying via an evolution of mixed Au- and Cu-precursor nanoparticles near the nanoscale melting temperatures. For the evolution of mixed precursor nanoparticles, synchrotron x-ray based in-situ real time XRD was used to monitormore » the structural changes, revealing nanoscale alloying and reshaping towards an fcc-type nanoalloy (particle or cube) via a partial melting–resolidification mechanism. The nanoalloys supported on carbon or silica were characterized by in-situ high-energy XRD/PDFs, revealing an intriguing lattice "expanding-shrinking" phenomenon depending on whether the catalyst is thermochemically processed under oxidative or reductive atmosphere. This type of controllable structural changes is found to play an important role in determining the catalytic activity of the catalysts for carbon monoxide oxidation reaction. The tunable catalytic activities of the nanoalloys under thermochemically oxidative and reductive atmospheres are also discussed in terms of the bifunctional sites and the surface oxygenated metal species for carbon monoxide and oxygen activation.« less

Sample preparation for thermo-gravimetric determination and thermo-gravimetric characterization of refuse derived fuel.

PubMed

Robinson, T; Bronson, B; Gogolek, P; Mehrani, P

2016-02-01

Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and characterization of Sb2Se3 devices for memory applications

NASA Astrophysics Data System (ADS)

Shylashree, N.; Uma B., V.; Dhanush, S.; Abachi, Sagar; Nisarga, A.; Aashith, K.; Sangeetha B., G.

2018-05-01

In this paper, A phase change material of Sb2Se3 was proposed for non volatile memory application. The thin film device preparation and characterization were carried out. The deposition method used was vapor evaporation technique and a thickness of 180nm was deposited. The switching between the SET and RESET state is shown by the I-V characterization. The change of phase was studied using R-V characterization. Different fundamental modes were also identified using Raman spectroscopy.

Preparation and characterization of (St-DVB-MAA) ion exchange resins

NASA Astrophysics Data System (ADS)

Jiang, Shanquan; Sun, Xiangwei; Ling, Lixing; Wang, Shumin; Wu, Wufeng; Cheng, Shihong; Hu, Yue; Zhong, Chunyan

2017-08-01

In this paper, used polyvinyl alcohol as dispersing agent, Benzoyl peroxide as initiator of polymerization, Divinyl benzene as cross-linking agent, Styrene and 2-Methylpropenoic acid as monomer, ion exchange resin (copolymer of St-DVB-MAA)were prepared by suspension polymerization on 80°C. The structures, components and properties of the prepared composite micro gels were characterized by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA). The experiment of ion exchange was conducted by resin to deal with copper ions in the solution. The result showed that performance of the ion exchange capacity was excellent, which impacted by pH.

Artemisinin nanoformulation suitable for intravenous injection: Preparation, characterization and antimalarial activities.

PubMed

Ibrahim, Nehal; Ibrahim, Hany; Sabater, Alicia Moreno; Mazier, Dominique; Valentin, Alexis; Nepveu, Françoise

2015-11-30

More than 40 years after its discovery, artemisinin has become the most promising antimalarial agent. However, no intravenous formulation is available due to its poor aqueous solubility. Here, we report the preparation, characterization, and in vitro and in vivo biological evaluation of biodegradable albumin-bound artemisinin nanoparticles. The nanoparticles were prepared by a combination of a bottom-up and a top-down processes and characterized by different spectroscopic techniques. The preparation process was optimized to develop a nanoformulation with the smallest possible diameter and good homogeneity suitable for intravenous injection enabling direct contact of artemisinin with infected erythrocytes. Chemically and physically stable artemisinin nanoparticles were obtained with excellent entrapment efficiency. In in vitro experiments, the artemisinin nanoformulation was interestingly more effective than non-formulated artemisinin. In Plasmodiumm falciparum-infected 'humanized' mice, the nanoparticles proved to be highly effective with 96% parasitemia inhibition at 10mg/kg/day, prolonging mean survival time without recrudescence. This nanoparticulate albumin-bound system allows the intravenous administration of artemisinin for the first time without harsh organic solvents or cosolvents with 100% bioavailability. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and characterization of triclosan nanoparticles for periodontal treatment.

PubMed

Piñón-Segundo, E; Ganem-Quintanar, A; Alonso-Pérez, V; Quintanar-Guerrero, D

2005-04-27

The aim of this work was to produce and characterize triclosan-loaded nanoparticles (NPs) by the emulsification-diffusion process, in an attempt to obtain a novel delivery system adequate for the treatment of periodontal disease. The NPs were prepared using poly(D,L-lactide-co-glycolide) (PLGA), poly(D,L-lactide) (PLA) and cellulose acetate phthalate (CAP). Poly(vinyl alcohol) (PVAL) was used as stabilizer. Batches were prepared with different amounts of triclosan (TCS) in order to evaluate the influence of drug on NP properties. Solid NPs of less than 500 nm in diameter were obtained. Entrapment efficiencies were higher than 63.8%. The characterization by scanning electron microscopy and light scattering indicated that high concentrations of TCS seemingly caused the increase of NP mean size. A decrease in the PLGA glass transition temperature was observed by differential scanning calorimetry. This could indicate that TCS in PLGA-NPs behaves as a non-conventional plasticizer. Subsequently, in vitro release studies were carried out under sink conditions using a device designed in our laboratory to allow a direct contact between the particles and the dissolution medium. A fast release of TCS from NPs was detected. A preliminary in vivo study in dogs with induced periodontal defects suggested that TCS-loaded NPs penetrate through the junctional epithelium.

Preparation and characterization of triple shape memory composite foams.

PubMed

Nejad, Hossein Birjandi; Baker, Richard M; Mather, Patrick T

2014-10-28

Foams prepared from shape memory polymers (SMPs) offer the potential for low density materials that can be triggered to deploy with a large volume change, unlike their solid counterparts that do so at near-constant volume. While examples of shape memory foams have been reported in the past, they have been limited to dual SMPs: those polymers featuring one switching transition between an arbitrarily programmed shape and a single permanent shape established by constituent crosslinks. Meanwhile, advances by SMP researchers have led to several approaches toward triple- or multi-shape polymers that feature more than one switching phase and thus a multitude of temporary shapes allowing for a complex sequence of shape deployments. Here, we report the design, preparation, and characterization of a triple shape memory polymeric foam that is open cell in nature and features a two phase, crosslinked SMP with a glass transition temperature of one phase at a temperature lower than a melting transition of the second phase. The soft materials were observed to feature high fidelity, repeatable triple shape behavior, characterized in compression and demonstrated for complex deployment by fixing a combination of foam compression and bending. We further explored the wettability of the foams, revealing composition-dependent behavior favorable for future work in biomedical investigations.

Preparation and biophysical characterization of recombinant Pseudomonas aeruginosa phosphorylcholine phosphatase.

PubMed

Beassoni, Paola R; Berti, Federico Pérez de; Otero, Lisandro H; Risso, Valeria A; Ferreyra, Raul G; Lisa, Angela T; Domenech, Carlos E; Ermácora, Mario R

2010-06-01

Pseudomonas aeruginosa infections constitute a widespread health problem with high economical and social impact, and the phosphorylcholine phosphatase (PchP) of this bacterium is a potential target for antimicrobial treatment. However, drug design requires high-resolution structural information and detailed biophysical knowledge not available for PchP. An obstacle in the study of PchP is that current methods for its expression and purification are suboptimal and allowed only a preliminary kinetic characterization of the enzyme. Herein, we describe a new procedure for the efficient preparation of recombinant PchP overexpressed in Escherichia coli. The enzyme is purified from urea solubilized inclusion bodies and refolded by dialysis. The product of PchP refolding is a mixture of native PchP and a kinetically-trapped, alternatively-folded aggregate that is very slowly converted into the native state. The properly folded and fully active enzyme is isolated from the refolding mixture by size-exclusion chromatography. PchP prepared by the new procedure was subjected to chemical and biophysical characterization, and its basic optical, hydrodynamic, metal-binding, and catalytic properties are reported. The unfolding of the enzyme was also investigated, and its thermal stability was determined. The obtained information should help to compare PchP with other phosphatases and to obtain a better understanding of its catalytic mechanism. In addition, preliminary trials showed that PchP prepared by the new protocol is suitable for crystallization, opening the way for high-resolution studies of the enzyme structure.

Characterization of factor VIII pharmaceutical preparations by means of MudPIT proteomic approach.

PubMed

Basilico, Fabrizio; Nardini, Ilaria; Mori, Filippo; Brambilla, Elena; Benazzi, Louise; De Palma, Antonella; Rosti, Enrico; Farina, Claudio; Mauri, PierLuigi

2010-09-21

For a good clinical outcome of Haemophilia A substitutive therapy a detailed characterization of factor VIII (FVIII) concentrates is required, in order to disclose the eventual relations between differently composed concentrates and their biological effects. This preliminary work could be a first step towards a deep structural characterization of FVIII concentrates, using the fast and simply manageable MudPIT technology, which enables the identification and characterization of protein mixtures taking advantage of both the high separation capacity of two-dimensional chromatography and the powerful peptide characterization ability of tandem mass spectrometry. The aim of this study was to evaluate the suitability of for the characterization of FVIII molecule in complex mixtures such its commercial concentrates, both plasma-derived and recombinant, and for the determination of the protein composition of different FVIII preparations. By means of Multidimensional Protein Identification Technology (MudPIT) it was possible to assess the presence of factor VIII in its preparations and to identify most of the contaminant proteins without gel separation. In particular, 125 and 42 proteins were identified in plasma-derived and recombinant concentrates, respectively. Concerning investigation of FVIII, 24 different peptides were identified in plasma-derived corresponding to 7, 29, 27, 19 and 67 of percentage coverage for A1, A2, A3, C1 and C2 domains, respectively. About its multimeric carrier von Willebrand factor (VWF), we have sequenced 42% of domain interacting with A3 and C2 domains of FVIII. Finally, it has been observed that normalized parameters, such as total peptide hits obtained by SEQUEST may be used for evaluation of the relative abundance of FVIII in different preparations. Copyright 2010 Elsevier B.V. All rights reserved.

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

Carreras, Alejo C., E-mail: acarreras@famaf.unc.edu.ar; Cangiano, María de los A.; Ojeda, Manuel W.

The influence of the amount of complexing agent added to the starting solution on the physicochemical properties of Cu–Ni nanostructured alloys obtained through a chemical route, was studied. For this purpose, three Cu–Ni nanoalloy samples were synthesized by a previously developed procedure, starting from solutions with citric acid to metal molar ratios (C/Me) of 0.73, 1.00 and 1.50. The synthesis technique consisted in preparing a precursor via the citrate-gel method, and carrying out subsequent thermal treatments in controlled atmospheres. Sample characterization was performed by scanning electron microscopy, X-ray microanalysis, X-ray diffraction, transmission electron microscopy, X-ray nanoanalysis and electron diffraction. Inmore » the three cases, copper and nickel formed a solid solution with a Cu/Ni atomic ratio close to 50/50, and free of impurities inside the crystal structure. The citric acid content of the starting solution proved to have an important influence on the morphology, size distribution, porosity, and crystallinity of the Cu–Ni alloy microparticles obtained, but a lesser influence on their chemical composition. The molar ratio C/Me = 1.00 resulted in the alloy with the Cu/Ni atomic ratio closest to 50/50. - Highlights: • We synthesize Cu–Ni nanoalloys by a chemical route based on the citrate-gel method. • We study the influence of the complexing agent content of the starting solution. • We characterize the samples by electron microscopy and X-ray techniques. • Citric acid influences the shape, size, porosity and crystallinity of the alloys.« less

Supercritical antisolvent versus coevaporation: preparation and characterization of solid dispersions.

PubMed

Majerik, Viktor; Horváth, Géza; Szokonya, László; Charbit, Gérard; Badens, Elisabeth; Bosc, Nathalie; Teillaud, Eric

2007-09-01

The objective of this work was to improve the dissolution rate and aqueous solubility of oxeglitazar. Solid dispersions of oxeglitazar in PVP K17 (polyvinilpyrrolidone) and poloxamer 407 (polyoxyethylene-polyoxypropylene block copolymer) were prepared by supercritical antisolvent (SAS) and coevaporation (CoE) methods. Drug-carrier formulations were characterized by powder X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, gas chromatography, UV/VIS spectroscopy and in vitro dissolution tests. The highest dissolution rate (nearly 3-fold higher than raw drug) was achieved by preparation of drug/PVP K17 coevaporate. Oxeglitazar/PVP K17 solid dispersions were stabilized by hydrogen bonding but contained higher amount of residual dichloromethane (DCM) than poloxamer 407 formulations regardless of the method of preparation. SAS prepared oxeglitazar/poloxamer 407 dissolved more than two times faster than raw drug. However, unlike PVP K17, poloxamer 407 did not form a single phase amorphous solid solution with oxeglitazar which has been manifested in higher degrees of crystallinity, too. Among the two techniques, evaluated in this work, conventional coevaporation resulted in higher amorphous content but SAS reduced residual solvent content more efficiently.

Preparation and Characterization of Nano-CL-20 Explosive

NASA Astrophysics Data System (ADS)

Bayat, Yadollah; Zeynali, Vida

2011-10-01

Nano-CL-20 was prepared via precipitative crystallization by spraying a solution of CL-20 in a solvent (ethyl acetate) into a nonsolvent (isooctane). Scanning electron microscopy (SEM) and X-ray powder diffraction (XRD) were used to characterize the appearance and the size of the particles. The results revealed that nano-CL-20 particles have the shape of spheres or ellipsoids with an average size of 95 nm. Due to their small diameter and high surface energy, the particles tended to agglomerate. Impact sensitivity of nanosize CL-20 was decreased in comparison to micrometer-size CL-20.

Preparation, characterization and properties of ZnO nanomaterials

NASA Astrophysics Data System (ADS)

Luo, Jiaolian; Zhang, Xiaoming; Chen, Ruxue; Wang, Xiaohui; Zhu, Ji; Wang, Xiaomin

2017-06-01

In this paper, using the hydrothermal synthesis method, NaOH, Zn(NO3)2, anhydrous ethanol, deionized water as raw material to prepare ZnO nanomaterial, and by X ray diffraction (XRD), scanning electron microscopy (SEM) and photoluminescence spectroscopy (PL) on the synthesis of nano materials, surface morphology and phase luminescence characterization. The results show that the nano materials synthesized for single-phase ZnO, belonging to the six wurtzite structure; material surface shaped, arranged evenly distributed, and were the top six party structure; ZnO nano materials synthesized with strong emission spectra, emission peak is located at 394nm.

Preparation and characterization of conjugated polymers made by postpolymerization reactions of alternating polyketones.

PubMed

Cheng, Chen; Guironnet, Damien; Barborak, James; Brookhart, Maurice

2011-06-29

Conjugated polymers possessing a poly(2,5-dimethylene-2,5-dihydrofuran) backbone were prepared through postpolymerization reaction of styrenic polyketones with bromine in one-pot reactions. The modification is proposed to proceed via condensation of two repeating units to form a fully characterized polymer with a poly(2,5-dimethylenetetrahydrofuran) backbone. Subsequent bromination and elimination of HBr yield a polymer with a fully conjugated carbon backbone. The new conjugated polymers were characterized by NMR, IR, and UV-vis spectroscopies and by CV. These polymers have strong absorption in the visible region, with the absorption peaks shifted to the NIR region upon doping with acids. The ease of the synthesis of the starting polyketone and of the modifications allows large-scale preparation of those conjugated polymers.

Colloidal nickel/gallium nanoalloys obtained from organometallic precursors in conventional organic solvents and in ionic liquids: noble-metal-free alkyne semihydrogenation catalysts

NASA Astrophysics Data System (ADS)

Schütte, Kai; Doddi, Adinarayana; Kroll, Clarissa; Meyer, Hajo; Wiktor, Christian; Gemel, Christian; van Tendeloo, Gustaaf; Fischer, Roland A.; Janiak, Christoph

2014-04-01

Efforts to replace noble-metal catalysts by low-cost alternatives are of constant interest. The organometallic, non-aqueous wet-chemical synthesis of various hitherto unknown nanocrystalline Ni/Ga intermetallic materials and the use of NiGa for the selective semihydrogenation of alkynes to alkenes are reported. Thermal co-hydrogenolysis of the all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in high-boiling organic solvents mesitylene and n-decane in molar ratios of 1 : 1, 2 : 3 and 3 : 1 yields the nano-crystalline powder materials of the over-all compositions NiGa, Ni2Ga3 and Ni3Ga, respectively. Microwave induced co-pyrolysis of the same precursors without additional hydrogen in the ionic liquid [BMIm][BF4] (BMIm = 1-butyl-3-methyl-imidazolium) selectively yields the intermetallic phases NiGa and Ni3Ga from the respective 1 : 1 and 3 : 1 molar ratios of the precursors. The obtained materials are characterized by transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), IR, powder X-ray diffraction (PXRD) and atomic absorption spectroscopy (AAS). The single-source precursor [Ni(GaCp*)(PMe3)3] with a fixed Ni : Ga stoichiometry of 1 : 1 was employed as well. In comparison with the co-hydrogenolytic dual precursor source approach it turned out to be less practical due to inefficient nickel incorporation caused by the parasitic formation of stable [Ni(PMe3)4]. The use of ionic liquid [BMIm][BF4] as a non-conventional solvent to control the reaction and stabilize the nanoparticles proved to be particularly advantageous and stable colloids of the nanoalloys NiGa and Ni3Ga were obtained. A phase-selective Ni/Ga colloid synthesis in conventional solvents and in the presence of surfactants such as hexadecylamine (HDA) was not feasible due to the undesired reactivity of HDA with GaCp* leading to inefficient gallium incorporation. Recyclable NiGa nanoparticles selectively

Polymeric nanoparticles: A study on the preparation variables and characterization methods.

PubMed

Crucho, Carina I C; Barros, Maria Teresa

2017-11-01

Since the emergence of Nanotechnology in the past decades, the development and design of nanomaterials has become an important field of research. An emerging component in this field is nanomedicine, wherein nanoscale materials are being developed for use as imaging agents or for drug delivery applications. Much work is currently focused in the preparation of well-defined nanomaterials in terms of size and shape. These factors play a significantly role in the nanomaterial behavior in vivo. In this context, this review focuses on the toolbox of available methods for the preparation of polymeric nanoparticles. We highlight some recent examples from the literature that demonstrate the influence of the preparation method on the physicochemical characteristics of the nanoparticles. Additionally, in the second part, the characterization methods for this type of nanoparticles are discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and characterization of bio-composite PEEK/nHA

NASA Astrophysics Data System (ADS)

Jin, Y. S.; Bian, C. C.; Zhang, Z. Q.; Zhao, Y.; Yang, L.

2017-01-01

PEEK/nHA composite material, with excellent mechanical property as polyetheretherketone (PEEK) and biological activity as hydroxyapatite (HA), has attracted wide attention of medical experts and materials science experts. The addition of hydroxyapatite was the decisive factor for biological activity in PEEK/nHA composite. In this paper, acicular nanohydroxyapatite was prepared by chemical precipitation method with Ca(NO3)2, (NH4)2HPO4 as raw material; PEEK/nHA composite was prepared by solution blending and vacuum sintering method. The composite was characterized with FT-IR, XRD, DSC, TG and mechanical property test. Results showed that the composite has good thermal stability and compressive property when the mass ratio of PEEK to nHA is 10:3; and high nHA content can improve the biological activity of the composite, which can meet the basic requirements for bone tissue engineering scaffold.

Preparation and characterization of progesterone dispersions using supercritical carbon dioxide.

PubMed

Falconer, James R; Wen, Jingyuan; Zargar-Shoshtari, Sara; Chen, John J; Farid, Mohammed; Tallon, Stephen J; Alany, Raid G

2014-04-01

Supercritical fluid methods offer an alternative to conventional mixing methods, particularly for heat sensitive drugs and where an organic solvent is undesirable. To design, develop and construct a unit for the particles from a gas-saturated suspension/solution (PGSS) method and form endogenous progesterone (PGN) dispersion systems using SC-CO2. The PGN dispersions were manufactured using three selected excipients: polyethylene glycol (PEG) 400/4000 (50:50), Gelucire 44/14 and D-α-tocopheryl PEG 1000 succinate (TPGS). Semisolid dispersions of PGN prepared by PGSS method were compared to the conventional methods; comelting (CM), cosolvent (CS) and physical mixing (PM). The dispersion systems made were characterized by Raman and Fourier transform infrared (FTIR) spectroscopies, X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), PGN recovery, uniformity and in vitro dissolution, analyzed by high-performance liquid chromatography (HPLC). Raman spectra revealed no changes in the crystalline structure of PGN treated with SC-CO2 compared to that of untreated PGN. XRPD and FTIR showed the presence of peaks and bands for PGN confirming that PGN has been incorporated well with each individual excipient. All PGN dispersions prepared by the PGSS method resulted in the improvement of PGN dissolution rates compared to that prepared by the conventional methods and untreated PGN after 60 min (p value < 0.05). The novel PGN dispersions prepared by the PGSS method offer the great potential to enhance PGN dissolution rate, reduce preparation time and form stable crystalline dispersion systems over those prepared by conventional methods.

Piroxicam cocrystals with phenolic coformers: preparation, characterization, and dissolution properties.

PubMed

Emami, Shahram; Adibkia, Khosro; Barzegar-Jalali, Mohammad; Siahi-Shadbad, Mohammadreza

2018-04-04

This study explores the preparation and investigation of dissolution properties of piroxicam cocrystals. Differential scanning calorimetry (DSC) was used to determine the capability of resorcinol (RES), methylparaben (MPB), and vanillin (VAN) to form cocrystals with piroxicam (PRX). Generation of cocrystals was attempted by liquid assisted grinding and slurry methods. Cocrystals were characterized by thermal methods, powder X-ray diffraction, and Fourier-transform infrared spectroscopy. Apparent solubility, intrinsic dissolution rate (IDR), and powder dissolution profile of cocrystals were compared with anhydrous piroxicam, piroxicam monohydrate (PRXMH), and previously reported piroxicam-succinic acid cocrystal. Contact angles and particle sizes of the studied solids were also measured. Based on the DSC screening results, we prepared and characterized PRX-RES and PRX-MPB cocrystals. Interestingly, the cocrystals not only failed to improve apparent solubility and IDR of PRX but also showed lower values than PRX that were attributed to induction of phase transformation of PRX to PRXMH. In contrary, cocrystals performed better than PRX in powder dissolution studies. The higher dissolution rates of cocrystals were explained by improved wettability and reduced sizes. This study has highlighted the complexity of solid state properties of cocrystals and has provided new evidence for the in-solution stability issues of cocrystals.

Metal oxide nanostructures: preparation, characterization and functional applications as chemical sensors.

PubMed

Zappa, Dario; Bertuna, Angela; Comini, Elisabetta; Kaur, Navpreet; Poli, Nicola; Sberveglieri, Veronica; Sberveglieri, Giorgio

2017-01-01

Preparation and characterization of different metal oxide (NiO, WO 3 , ZnO, SnO 2 and Nb 2 O 5 ) nanostructures for chemical sensing are presented. p-Type (NiO) and n-type (WO 3 , SnO 2 , ZnO and Nb 2 O 5 ) metal oxide nanostructures were grown on alumina substrates using evaporation-condensation, thermal oxidation and hydrothermal techniques. Surface morphologies and crystal structures were investigated through scanning electron microscopy and Raman spectroscopy. Furthermore, different batches of sensors have been prepared, and their sensing performances towards carbon monoxide and nitrogen dioxide have been explored. Moreover, metal oxide nanowires have been integrated into an electronic nose and successfully applied to discriminate between drinking and contaminated water.

Preparation and characterization of biodegradable magnetic carriers by single emulsion-solvent evaporation

NASA Astrophysics Data System (ADS)

Liu, Xianqiao; Kaminski, Michael D.; Riffle, Judy S.; Chen, Haitao; Torno, Michael; Finck, Martha R.; Taylor, LaToyia; Rosengart, Axel J.

2007-04-01

This paper describes a single emulsion-solvent evaporation protocol to prepare PEGylated biodegradable/biocompatible magnetic carriers by utilizing hydrophobic magnetite and a mixture of poly( D,L lactide-co-glycolide) (PLGA) and poly(lactic acid-block-polyethylene glycol) (PLA-PEG) (26:1 by mass) polymers. We characterized the magnetic microspheres in terms of morphology, composite microstructure, size and size distribution, and magnetic properties. Results show that the preparation produces magnetic microspheres with a good spherical morphology, small size (mean diameter of 1.2-1.5 μm) by means of large size distributions, and magnetizations up to 20-30 emu/g of microspheres.

Preparation and characterization of PEGylated chitosan nanocapsules as a carrier for pharmaceutical application

NASA Astrophysics Data System (ADS)

Najafabadi, Alireza Hassani; Abdouss, Majid; Faghihi, Shahab

2014-03-01

A new method to conjugate methoxy polyethylene glycol (mPEG) to C6 position of chitosan under the mild condition is introduced that improves the biocompatibility and water solubility of chitosan. Harsh deprotecting step and several purification cycles are two major disadvantages of the current methods for preparing PEGylated chitosan. In this study, the amine groups at C2 position of chitosan are protected using SDS followed by grafting the PEG. The protecting group of chitosan is simply removed by dialyzing against Tris solution. The chemical structure of the prepared polymer is characterized by FTIR and 1H NMR spectroscopy. Fourier transformed-infrared (FT-IR) and 1H NMR spectra confirmed that the mPEG is successfully grafted to C6 position of chitosan. Prepared methoxy polyethylene glycol (mPEG) is then employed to prepare the nanocapsules for the encapsulation of poor water-soluble drug, propofol. The TEM, AFM, and DLS techniques are used to characterize the prepared nanocapsules size and morphology. The results show a size of about 80 nm with spherical shape for nanocapsules. In vitro drug release is carried out to evaluate the potential of nanocarriers for the intravenous delivery of drugs. The profile of release from formulated nanocapsules is similar to those of commercial lipid emulsion (CLE). In vivo animal sleep-recovery test on rats shows a close similarity between the time of unconsciousness and recovery of righting reflex between nanoparticles and CLE. This study provides an efficient, novel, and easy method for preparing a carrier system that requires less intensive reaction conditions, fewer reaction steps, and less purification steps. In addition, the nanocapsules introduced here could be a promising nano carrier for the delivery of poor water-soluble drugs.

Preparation and characterization of ultraflat Pt facets by atom-height-resolved differential optical microscopy

NASA Astrophysics Data System (ADS)

Azhagurajan, M.; Wen, R.; Kim, Y. G.; Itoh, T.; Sashikata, K.; Itaya, K.

2015-01-01

We recently demonstrated that improvements to our technique, laser confocal microscopy with differential interference microscopy (LCM-DIM), has rendered it fully capable of resolving monatomic steps with heights of ca. 0.25 nm on Au(111) and Pd(111) surfaces, even as low as 0.14 nm on Si(100), in aqueous solution. In this paper, we describe in detail a method to prepare and characterize, via atomic-layer-resolved LCM-DIM, ultraflat Pt(111) and Pt(100) facets over a wide surface area. The preparation of ultraflat surfaces is important in the characterization at the atomic scale of electrochemical processes under reaction conditions. To showcase the elegance of LCM-DIM, the anodic dissolution of Pt in aqueous HCl is briefly recounted.

Preparation, characterization, and activity of a peptide-cellulosic aerogel protease sensor from cotton

USDA-ARS?s Scientific Manuscript database

Nanocellulosic aerogels (NA) provide a lightweight biocompatible material with structural properties of both high porosity and specific surface area for biosensor design. We report here the preparation, characterization, and activity of a peptide-nanocellulose aerogel (PA) made from unprocessed cot...

Preparation and Characterization of an Amphipathic Magnetic Nanosphere

PubMed Central

Ji, Yongsheng; Lv, Ruihong; Xu, Zhigang; Zhao, Chuande; Zhang, Haixia

2014-01-01

The amphipathic magnetic nanospheres were synthesized using C8 and polyethylene glycol as ligands. Their morphology, structure, and composition were characterized by transmission electron microscope, Fourier transform infrared, and elementary analysis. The prepared materials presented uniform sphere with size distribution about 200 nm. The magnetic characteristics of magnetic nanomaterials were measured by vibrating sample magnetometer. The target products had a saturation magnetization value of 50 emu g−1 and superparamagnetism. The adsorption capability was also studied by static tests, and the material was applied to enrich benzenesulfonamide from calf serum. The results exhibited that the C8-PEG phase owned better adsorption capability, biocompatible property, and dispersivity in aqueous samples. PMID:24729917

Preparation and Characterization of Nano Gold Supported over Montmorillonite Clays

NASA Astrophysics Data System (ADS)

Suraja, P. V.; Binitha, N. N.; Yaakob, Z.; Silija, P. P.

2011-02-01

The use of montmorillonite clays as a matrix, or as a host, for obtaining intercalated/supported metal particles has potential applications in catalysis and other areas. The gold nanoparticles were obtained from the most common anionic gold precursor HAuCl4·3H2O by deposition-precipitation (DP) methods. However, it is difficult to prepare nanoscale gold catalysts supported on silica surfaces with lower isoelectric point (IEP). Homogeneous precipitation method using urea also fails on silica surfaces. Reasons for the inefficiency of these methods are the negative charge of the metal precursor as well as the support surface and the high pH required for depositing gold nanoparticles. In the present work, we use glucose as the reductant in the presence of stabilizer for preparation of nano gold supported on montmorillonite clay. There is no need of increasing the pH of the solution to reduce the Au3+ ions. The prepared systems are characterized using various techniques such as using X-ray fluorescence (XRF), UV-VIS Diffuse reflectance spectra (DRS) and Fourier Transform infra red spectra (FTIR) to prove the efficiency of the present method.

Characterization and preparation of Aspergillus niger naringinase for debittering citrus juice.

PubMed

Ni, Hui; Chen, Feng; Cai, Huinong; Xiao, Anfeng; You, Qi; Lu, Yunzhen

2012-01-01

Naringinase from Aspergillus niger was prepared and characterized to evaluate its effectiveness in debittering citrus juice. The enzyme was purified to homogeneity by sulfate fractionation and chromatographies on Q-Sepharose, Sephacryl S-200, and S-100 HR columns, and estimated by gel filtration chromatography (GFC) to have a molecular weight (MW) of 131 kDa, of which its subunit was measured by sodium dodecyl sulfate-polyacrylamide gel electrophoresis to be around 65.5 kDa. The enzyme showed active and stable pH ranges both within 4.5 to 5.0. Its optimal temperature was in the range of 45 to 55 °C. Freeze drying provided an estimated enzymatic recovery of 95.9%, greater than spray drying with the recovery at 55.6%. The freeze-drying powder could retain its enzymatic activity stably at 4 °C for 6 mo. Also, the enzyme in 0.220 U/mL citrus juice could sufficiently remove the naringin for the bitterness. Oral acute toxicity study revealed the maximum tolerated dose (MTD) of the naringinase powder was >10 g/kg in mice. The contents of arsenic (As), lead (Pb), mercury (Hg), the aerobic plate count, and coliform number in the enzyme powder all met the criteria for food use. These characteristics suggest that the naringinase from A. niger is efficient and suitable for debittering the citrus juice, and the process consisting of fermentation, salt precipitation, ion exchange, ultrafiltration, and freeze drying is a promising means to prepare the naringinase for food industry, setting up a strong base to enzymatically debitter citrus juice. This study focused on characterization, preparation, and validation of naringinase from A. niger, which provided useful information on how to prepare, store, and use the naringinase. In addition, this naringinase met the safety standards for food use and showed strong ability to remove the bitter taste from citrus juice, which provided useful information for interested readers, and the food industry. © 2011 Institute of Food

Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium.

PubMed

Kaltenbach, Angela; Noordmann, Janine; Görlitz, Volker; Pape, Carola; Richter, Silke; Kipphardt, Heinrich; Kopp, Gernot; Jährling, Reinhard; Rienitz, Olaf; Güttler, Bernd

2015-04-01

Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.

Submicron magnetic core conducting polypyrrole polymer shell: Preparation and characterization.

PubMed

Tenório-Neto, Ernandes Taveira; Baraket, Abdoullatif; Kabbaj, Dounia; Zine, Nadia; Errachid, Abdelhamid; Fessi, Hatem; Kunita, Marcos Hiroiuqui; Elaissari, Abdelhamid

2016-04-01

Magnetic particles are of great interest in various biomedical applications, such as, sample preparation, in vitro biomedical diagnosis, and both in vivo diagnosis and therapy. For in vitro applications and especially in labs-on-a-chip, microfluidics, microsystems, or biosensors, the needed magnetic dispersion should answer various criteria, for instance, submicron size in order to avoid a rapid sedimentation rate, fast separations under an applied magnetic field, and appreciable colloidal stability (stable dispersion under shearing process). Then, the aim of this work was to prepare highly magnetic particles with a magnetic core and conducting polymer shell particles in order to be used not only as a carrier, but also for the in vitro detection step. The prepared magnetic seed dispersions were functionalized using pyrrole and pyrrole-2-carboxylic acid. The obtained core-shell particles were characterized in terms of particle size, size distribution, magnetization properties, FTIR analysis, surface morphology, chemical composition, and finally, the conducting property of those particles were evaluated by cyclic voltammetry. The obtained functional submicron highly magnetic particles are found to be conducting material bearing function carboxylic group on the surface. These promising conducting magnetic particles can be used for both transport and lab-on-a-chip detection. Copyright © 2015. Published by Elsevier B.V.

TiO2 nanocomposites: Preparation, characterization, mechanical and biological properties

NASA Astrophysics Data System (ADS)

Koşarsoy, Gözde; Şen, Elif Hilal; Aksöz, Nilüfer; İde, Semra; Aksoy, Hüsnü

2014-11-01

Some novel nanocomposites, which contain different concentrations of TiO2 nanopowders, were firstly prepared by using marble dust with convenient chemical components. Their nano structures characterized and distributions of the nano-aggregations related with internal structural content of the samples have been determined by X-ray Scattering Methods (SAXS and WAXS) and mechanical properties were determined by using strain-stress measurements to increase their potential usage possibility as building materials in health and research centers. In the last and important part of the study, Candida albicans and Aspergillus niger which are a significant risk to medical patients were used to investigate originally prepared nanostructured samples' photocatalyst effect. During the last part of the study, effect of UV and visible light on photocatalyst nanocomposites were also researched. Heterogeneous photocatalysts can carry out advanced oxidation processes used for an antimicrobial effect on microorganisms. TiO2 nanoparticles as one of heterogeneous photocatalysts have been shown to exhibit strong cytotoxicity when exposed to UV and visible light.

Characterization of nanodimensional Ni-Zn ferrite prepared by mechanochemical and thermal methods

NASA Astrophysics Data System (ADS)

Manova, E.; Paneva, D.; Kunev, B.; Rivière, E.; Estournès, C.; Mitov, I.

2010-03-01

Nickel zinc ferrite nanoparticles, Ni1-xZnxFe2O4 (x = 0, 0.2, 0.5, 0.8, 1.0), with dimensions below 10 nm have been prepared by combining chemical precipitation with high-energy ball milling. For comparison, their analogues obtained by thermal synthesis have also been studied. Mössbauer spectroscopy, X-ray diffraction, and magnetic measurements are used for the characterization of the obtained materials. X-ray diffraction shows that after 3h of mechanical treatment ferrites containing zinc are formed, while 6h of treatment is needed to obtain NiFe2O4. The magnetic properties of the samples exhibit a strong dependence on the phase composition, particle size and preparation method.

[A new method for the preparation of potassium ferrate and spectroscopic characterization].

PubMed

Zheng, Huai-li; Deng, Lin-li; Ji, Fang-ying; Jiang, Shao-jie; Zhang, Peng

2010-10-01

Calcium hypochlorite was used as the raw material for preparation of the high purity potassium ferrate. The study includes the effects of reaction temperature, recrystallization temperature, reaction time, Ca(ClO)2 dosage, and the amount of calcium hypochlorite on the yield. It was determined that when the reaction temperature was 25 degrees C, recrystallization temperature 0 degree C and reaction time 40 min, the yield was more than 75%. The purity was detected by direct spectrophotometric method to be more than 92%. The product was characterized by infrated spectrum(IR), X-ray diffraction (XRD) and ultraviolet spectrum (UV) methods and proved to be potassium ferrate that was prepared by calcium hypochlorite as the raw material.

Preparation and characterizations of activated carbon monolith from rubber wood and its effect on supercapacitor performances

NASA Astrophysics Data System (ADS)

Taer, E.; Taslim, R.; Deraman, M.

2016-02-01

Preparation of activated carbon monolith (ACM) from rubber wood was investigated. Two kind of preparation method were carried out by pre-carbonized of rubber wood saw dust and rubber wood material as it is naturally. The samples were prepared with pelletizing method and small cutting of rubber wood in cross sectional method. Both of samples were characterized by physical and electrochemical technique. The physical properties such as morphology and porosity were investigated. The electrochemical properties of both samples such as equivalent series resistances (ESR) and specific capacitances were also compared. In conclusion, this study showed that both of different preparation method would propose a simple method of ACM electrode preparation technique for supercapacitor applications.

Preparation and characterization of the silicon clathrate NaxSi{136} (x -> 0)

NASA Astrophysics Data System (ADS)

Ammar, A.; Cros, C.; Pouchard, M.; Jaussaud, N.; Bassat, J.-M.; Villeneuve, G.; Reny, E.

2005-03-01

The type-II silicon clathrate, NaxSi{136}, having a residual sodium content as low as 37 ppm (x = 0.0062) has been prepared by thermal decomposition of NaSi under high vacuum in the temperature range 340-420 ° C followed by subsequent treatments under high vacuum, and completed by several treaments with iodine at 300-350 ° C. The final sample was characterized by XRD, chemical analysis and EPR spectroscopy. This latter technique proved to be particularly suitable to the characterization of highly diluted sodium atoms in the open host lattice of a type II clathrate of silicon and the quantitaive determination of the residual sodium content

Preparation and Characterization of Novel Montmorillonite Nanocomposites

NASA Astrophysics Data System (ADS)

Mansa, Rola

Clay minerals have historically played a consequential role in human health. While the beginnings were rooted in geophagy, a primitive act of consuming earth, the health-related uses of clay minerals have evolved and diversified over time.. As excipients in pharmaceutical formulations, clay minerals can attribute novel properties onto intercalated compounds. Intercalating oxybenzone, a UV filter, within the interlamellar space of montmorillonite is desirable in order to minimize direct contact with skin. Intercalating resveratrol, a compound known for attributing beneficial effects onto human health, may be advantageous since this compound is susceptible to cis-trans isomerisation. The strategy of using alkylammonium--modified clay was undertaken and proved successful for the intercalation of oxybenzone. The field of biopolymer/layered silicate nanocomposites is heavily researched for use in a multitude of applications. Novel montmorillonite nanocomposites were prepared with neutral guar gum and cationic guar gum, using an environmentally friendly process and are fully characterized.

Preparation, Modification, Characterization, and Biosensing Application of Nanoporous Gold Using Electrochemical Techniques.

PubMed

Bhattarai, Jay K; Neupane, Dharmendra; Nepal, Bishal; Mikhaylov, Vasilii; Demchenko, Alexei V; Stine, Keith J

2018-03-16

Nanoporous gold (np-Au), because of its high surface area-to-volume ratio, excellent conductivity, chemical inertness, physical stability, biocompatibility, easily tunable pores, and plasmonic properties, has attracted much interested in the field of nanotechnology. It has promising applications in the fields of catalysis, bio/chemical sensing, drug delivery, biomolecules separation and purification, fuel cell development, surface-chemistry-driven actuation, and supercapacitor design. Many chemical and electrochemical procedures are known for the preparation of np-Au. Recently, researchers are focusing on easier and controlled ways to tune the pores and ligaments size of np-Au for its use in different applications. Electrochemical methods have good control over fine-tuning pore and ligament sizes. The np-Au electrodes that are prepared using electrochemical techniques are robust and are easier to handle for their use in electrochemical biosensing. Here, we review different electrochemical strategies for the preparation, post-modification, and characterization of np-Au along with the synergistic use of both electrochemistry and np-Au for applications in biosensing.

Experimental preparation and characterization of four-dimensional quantum states using polarization and time-bin modes of a single photon

NASA Astrophysics Data System (ADS)

Yoo, Jinwon; Choi, Yujun; Cho, Young-Wook; Han, Sang-Wook; Lee, Sang-Yun; Moon, Sung; Oh, Kyunghwan; Kim, Yong-Su

2018-07-01

We present a detailed method to prepare and characterize four-dimensional pure quantum states or ququarts using polarization and time-bin modes of a single-photon. In particular, we provide a simple method to generate an arbitrary pure ququart and fully characterize the state with quantum state tomography. We also verify the reliability of the recipe by showing experimental preparation and characterization of 20 ququart states in mutually unbiased bases. As qudits provide superior properties over qubits in many fundamental tests of quantum physics and applications in quantum information processing, the presented method will be useful for photonic quantum information science.

Preparation and characterization of strontium-fluorapatite nanopowders by sol-gel method

NASA Astrophysics Data System (ADS)

Kamaei, Maryam; Fathi, Mohammad Hossein

2018-01-01

Biomaterials based on calcium orthophosphate are especially attractive for use in medicine, for bone and teeth implants due to their biological properties, such as biocompatibility and bioactivity. Among them, hydroxyapatite (HAP; Ca10(PO4)6(OH)2) is used particularly because of its similarities to the inorganic component of bone. Hydroxyapatite has been widely used for biomedical applications. Despite desirable properties such as bioactivity, biocompatibility, solubility and adsorption, synthetic HA is limited in application due to poor thermostability and poor mechanical properties. Properties of HA can be tailored over a wide range by incorporating different ions into HA lattice. Use of the sol-gel technique is technically simple, cost effective and beneficial for fabrication biomaterials. This research aimed to prepare and characterize Sr-doped FA nanopowders (Sr-FA). Sr-FA with different Sr contents was prepared by sol-gel method. The designated degree of substitution of Ca by Sr in the mixture was determined by the x value in the general formula of (Ca10-x Srx(PO4)6F2), where x=0,0.5,1. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques were utilized to characterize the obtained nano powders. Results showed that Sr ions entered into the fluorapatite lattice and occupied Ca sites. The incorporation of Sr ions into the fluorapatite resulted in the increase of the lattice parameters.

Synthesis and characterization of potential iron–platinum drugs and supplements by laser liquid photolysis

PubMed Central

Nkosi, Steven S; Mwakikunga, Bonex W; Sideras-Haddad, Elias; Forbes, Andrew

2012-01-01

Highly crystalline nanospherical iron–platinum systems were produced by 248 nm laser irradiation of a liquid precursor at different laser fluences, ranging from 100–375 mJ/cm2. The influence of laser intensity on particle size, iron composition, and structure was systematically investigated. Different nanostructures of iron–platinum alloy and chemically disordered iron–platinum L10 phase were obtained without annealing. The prepared precursor solution underwent deep photolysis to polycrystalline iron–platinum nanoalloys through Fe(III) acetylacetonate and Pt(II) acetylacetonate. Fe(II) and Pt(I) acetylacetone decomposed into Fe0 and Pt0 nanoparticles. We found that the (001) diffraction peak shifted linearly to a lower angle, with the last peak shifting in opposition to the others. This caused the face-centered cubic L10 structure to change its composition according to laser fluence. The nanostructures were shown to contain iron and platinum only by energy-dispersive spectroscopy at several spots. The response of these iron–platinum nanoparticles to infrared depends on their stoichiometric composition, which is controlled by laser fluence. PMID:24198494

Preparation and characterization of polystyrene/neodymium hydroxide (PS/Nd(OH)3) nano-composites

NASA Astrophysics Data System (ADS)

Alsewailem, Fares D.; Bagabas, Abdulaziz A.; Binkhodor, Yazeed A.

2018-03-01

Composites of polystyrene and Neodymium hydroxide nanrods (PS/Nd(OH)3) were formulated and characterized in this study. Cetyl (1-hexadccyl) trimethyl ammonium bromide (CTAB) was used as dispersion agent for the Nd(OH)3 rods in the PS matrix. PS/Nd(OH)3 composites were prepared by solution and melt compounding. Morphological, thermal, and mechanical properties of the prepared composites were investigated. CTAB was found to be more effective as dispersion agent in composites prepared by solution compounding in comparison with those prepared by melt compounding, and that was due to the mild conditions used in solution compounding. Nonetheless, impact strength of the composite at 0.5 wt% Nd(OH)3 was drastically reduced in the absence of CTAB. Both tensile and impact strengths were found to greatly decreased at higher loading of Nd(OH)3, e.g. 5 wt%, even with the use of CTAB. Thermal stability of the PS/Nd(OH)3 composites was noticeably increased at relatively low loading of Nd(OH)3, e.g. 0.5 wt%.

Preparation and characterization of Fe50Co50 nanostructured alloy

NASA Astrophysics Data System (ADS)

Yepes, N.; Orozco, J.; Caamaño, Z.; Mass, J.; Pérez, G.

2014-04-01

Nanostructured Fe50Co50 alloy was prepared by mechanical alloying of Fe and Co powders in a planetary high energy ball milling. The microstructure and structural evolution of the alloy have been investigated as a function of milling time (0 h, 8 h, 20 h and 35 h) by scanning electron microscopy (SEM) and X-Ray diffraction (XRD) characterization techniques. SEM micrographs showed different powder particles morphologies during the mechanical alloying stages. By XRD analysis it could be identified the structural phases of the alloy and the crystallite size was calculated as a function of the milling time.

Preparation and characterization of a siloxane containing bismaleimide

NASA Technical Reports Server (NTRS)

Maudgal, S.; St. Clair, T. L.

1984-01-01

A novel siloxane containing bismaleimide has been prepared by reacting maleic anhydride, benzophenonetetracarboxylic dianhydride and bis(gamma-aminopropyl)tetramethyldisiloxane. Characterization of this monomer was done by comparing its nuclear magnetic resonance spectrum (NMR) to those of model compounds. Solubility of the prepolymer was tested in amide, chlorinated and ether solvents. Films were cast from solution as well as by melt processing and a cure cycle was determined. Infrared spectrum (IR) of the resulting film was obtained. Thermal polymerization was investigated by differential scanning calorimetry (DSC). Thermal properties of the cured resin were followed by means of thermogravimetric analysis (TGA), torsional braid analysis (TBA) and dynamic mechanical analysis (DMA). Thermomechanical analysis (TMA) was used to study the effect of postcure on the glass transition temperature (Tg) of the resin. Adhesive strength of the resin was obtained at ambient temperature.

Preparation and Characterization of Polyimide/Organoclay Nanocomposites

NASA Technical Reports Server (NTRS)

Delozier, D. M.; Orwoll, R. A.; Cahoon, J. F.; Johnston, N. J.; Smith, J. G., Jr.; Connell, J. W.

2002-01-01

Organically modified montmorrrillonite clay, containing a long chain aliphatic quarternary ammonium cation, was used to prepare polyimide/organoclay hybrids. Several approaches were examined in an attempt to achieve fully exfoliated nanocomposites. These included simple mixing of the clay in a pre-made high molecular weight poly(amide acid) solution; simple mixing followed by sonication of the organoclay/poly(amide acid) solutions; and the preparation of high molecular weight poly(amide acid)s in the presence of the organoclay dispersed in N-methyl-2-pyrrolidinone (NMP). The best results were obtained using the in-situ polymerization approach. The resulting nanocomposite films (both amide acid and imide), containing 3-8% by weight of organoclay, were characterized by differential scanning calorimetry (DSC), dynamic thermogravimetric analysis (TGA), transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin film tensile properties. A significant degree of dispersion was observed in the nanocomposite films of the amide acid and the imide. After thermal treatment of amide acid films to effect imidization, in both air and nitrogen, the films were visually darker than control films without clay and the level of clay dispersion appeared to have decreased. In the latter case, the separation between the layers of the clay decreased to a spacing less than that present in the original organoclay. These observations suggest that thermal degradation of the aliphatic quarternary ammonium cation occurred likely during thermal treatment to effect imidization and solvent removal. These thermal degradation effects were less pronounced when thermal treatment was performed under nitrogen. The polyimide/organoclay hybrid films exhibited higher room temperature tensile moduli and lower strength and elongation to break than the control films.

Characterization of silver/polystyrene nanocomposites prepared by in situ bulk radical polymerization

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

Vukoje, Ivana D., E-mail: ivanav@vinca.rs; Vodnik, Vesna V., E-mail: vodves@vinca.rs; Džunuzović, Jasna V., E-mail: jasnav2002@googlemail.com

2014-01-01

Graphical abstract: - Highlights: • Synthesis and characterization of polystyrene nanocomposites based on Ag nanoparticles. • The glass transition temperature decreased in nanocomposites with respect to the pure polymer. • Resistance of the polymer to thermal degradation enhanced with Ag nanoparticles content. - Abstract: Nanocomposites (NCs) with different content of silver nanoparticles (Ag NPs) embeded in polystyrene (PS) matrix were prepared by in situ bulk radical polymerization. The nearly monodisperse Ag NPs protected with oleylamine were synthesized via organic solvo-thermal method and further used as a filler. The as-prepared spherical Ag NPs with diameter of 7.0 ± 1.5 nm weremore » well dispersed in the PS matrix. The structural properties of the resulting Ag/PS NCs were characterized by transmission electron microscope (TEM) and Fourier transform infrared (FTIR) spectroscopy, while optical properties were characterized using optical absorption measurements. The gel permeation chromatography (GPC) measurements showed that the presence of Ag NPs stabilized with oleylamine has no influence on the molecular weight and polydispersity of the PS matrix. The influence of silver content on the thermal properties of Ag/PS NCs was investigated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The results indicated that resistance of PS to thermal degradation was improved upon incorporation of Ag NPs. The Ag/PS NCs have lower glass transition temperatures than neat PS because loosely packed oleylamine molecules at the interface caused the increase of free volume and chain segments mobility near the surface of Ag NPs.« less

Preparation and characterization of Fe3O4-Pt nanoparticles

NASA Astrophysics Data System (ADS)

Andrade, Ângela Leão; Cavalcante, Luis Carlos Duarte; Fabris, José Domingos; Pereira, Márcio César; Ardisson, José Domingos; Domingues, Rosana Zacarias

2017-11-01

Pt and Pt-based nanomaterials are active anticancer drugs for their ability to inhibit the division of living cells. Nanoparticles of magnetite containing variable proportions of platinum were prepared in the laboratory. The magnetite nanoparticles with platinum (Pt-Fe3O4) were obtained by reducing the Fe3+ of the maghemite ( γ Fe2O3) mixed with platinum (II) acetylacetonate and sucrose in two inversely coupled ceramic crucibles and heated in a furnace at 400 °C for 20 min. The formed carbon during this preparation acts to chemically reduce the ferric iron in maghemite. Moreover, its residual layer on the particle surface prevents the forming magnetite from oxidizing in air and helps retain the platinum in the solid mixture. The produced Pt-magnetite samples were characterized by 57Fe-Mössbauer spectroscopy, powder X-ray diffraction, scanning electron microscopy, and magnetization measurements. Measurements of AC magnetic-field-induced heating properties of the obtained nanocomposites, in aqueous solution, showed that they are suitable as a hyperthermia agent for biological applications.

Preparation and characterization of bagasse/HDPE composites using multi-walled carbon nanotubes.

PubMed

Ashori, Alireza; Sheshmani, Shabnam; Farhani, Foad

2013-01-30

This article presents the preparation and characterization of bagasse/high density polyethylene (HDPE) composites. The effects of multi-walled carbon nanotubes (MWCNTs), as reinforcing agent, on the mechanical and physical properties were also investigated. In order to increase the interphase adhesion, maleic anhydride grafted polyethylene (MAPE) was added as a coupling agent to all the composites studied. In the sample preparation, MWCNTs and MAPE contents were used as variable factors. The morphology of the specimens was characterized using scanning electron microscopy (SEM) technique. The results of strength measurement indicated that when 1.5 wt% MWCNTs were added, tensile and flexural properties reached their maximum values. At high level of MWCNTs loading (3 or 4 wt%), increased population of MWCNTs lead to agglomeration and stress transfer gets blocked. The addition of MWCNTs filler slightly decreased the impact strength of composites. Both mechanical and physical properties were improved when 4 wt% MAPE was applied. SEM micrographs also showed that the surface roughness improved with increasing MAPE loading from 0 to 4 wt%. The improvement of physicomechanical properties of composites confirmed that MWCNTs have good reinforcement and the optimum synergistic effect of MWCNTs and MAPE was achieved at the combination of 1.5 and 4 wt%, respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Preparation, Modification, Characterization, and Biosensing Application of Nanoporous Gold Using Electrochemical Techniques

PubMed Central

Neupane, Dharmendra; Nepal, Bishal; Mikhaylov, Vasilii; Stine, Keith J.

2018-01-01

Nanoporous gold (np-Au), because of its high surface area-to-volume ratio, excellent conductivity, chemical inertness, physical stability, biocompatibility, easily tunable pores, and plasmonic properties, has attracted much interested in the field of nanotechnology. It has promising applications in the fields of catalysis, bio/chemical sensing, drug delivery, biomolecules separation and purification, fuel cell development, surface-chemistry-driven actuation, and supercapacitor design. Many chemical and electrochemical procedures are known for the preparation of np-Au. Recently, researchers are focusing on easier and controlled ways to tune the pores and ligaments size of np-Au for its use in different applications. Electrochemical methods have good control over fine-tuning pore and ligament sizes. The np-Au electrodes that are prepared using electrochemical techniques are robust and are easier to handle for their use in electrochemical biosensing. Here, we review different electrochemical strategies for the preparation, post-modification, and characterization of np-Au along with the synergistic use of both electrochemistry and np-Au for applications in biosensing. PMID:29547580

Preparation and characterization of kefiran electrospun nanofibers.

PubMed

Esnaashari, Seyedeh Sara; Rezaei, Sasan; Mirzaei, Esmaeil; Afshari, Hamed; Rezayat, Seyed Mahdi; Faridi-Majidi, Reza

2014-09-01

In this study, we report the first successful production of kefiran nanofibers through electrospinning process using distilled water as solvent. For this purpose, kefiran was extracted from cultured kefir grains, and homogenous kefiran solutions with different concentrations were prepared and then electrospun to obtain uniform nanofibers. The effect of main process parameters, including applied voltage, tip-to-collector distance, and feeding rate, on diameter and morphology of produced nanofibers, was studied. Scanning electron microscopy (SEM) and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy were used to characterize electrospun mats. Rheological behavior of the kefiran solution was evaluated via a cone and plate rheometer too. The results exhibited that diameter of kefiran nanofibers increased with increasing polymer concentration, applied voltage, and polymer feeding rate, while tip-to-collector distance did not have significant effect on nanofiber diameter. ATR-FTIR spectra showed that kefiran has maintained its molecular structure during electrospinning process. Flow curves also demonstrated shear thinning behavior for kefiran solutions. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and characterizations of EGDE crosslinked chitosan electrospun membranes.

PubMed

Aqil, A; Tchemtchoua, V T; Colige, A; Atanasova, G; Poumay, Y; Jérôme, C

2015-01-01

Composite Crosslinked nanofibrous membranes of chitosan, ethylene glycol diglycidyl ether (EGDE) and polyethylene oxide was successfully prepared with bead free morphology via electrospinning technique followed by heat mediated chemical crosslinking. Architectural stability of nanofiber mat in aqueous medium was achieved by chemical crosslinking of only 1% EGDE, and tensile strength tests revealed that increasing EGDE content has considerably enhance the elastic modulus of nanofibers. The structure, morphology and mechanical properties of nanofibers were characterized by Attenuated Total Reflection-Fourier Transform Infrared spectroscopy (ATR-FTIR), scanning electron microscopy (SEM) and Instron machine, respectively. Skin fibroblasts and endothelial cells showed good attachment, proliferation and viability on crosslinked electrospun membranes. The results indicate a good biocompatibility and non-toxic nature of the resulted membrane.

Characterization of Polysulfone Membranes Prepared with Thermally Induced Phase Separation Technique

NASA Astrophysics Data System (ADS)

Tiron, L. G.; Pintilie, Ș C.; Vlad, M.; Birsan, I. G.; Baltă, Ș

2017-06-01

Abstract Membrane technology is one of the most used water treatment technology because of its high removal efficiency and cost effectiveness. Preparation techniques for polymer membranes show an important aspect of membrane properties. Generally, polysulfone (PSf) and polyethersulfone (PES) are used for the preparation of ultrafiltration (UF) membranes. Polysulfone (PSf) membranes have been widely used for separation and purification of different solutions because of their excellent chemical and thermal stability. Polymeric membranes were obtained by phase inversion method. The polymer solution introduced in the nonsolvent bath (distilled water) initiate the evaporation of the solvent from the solution, this phenomenon has a strong influence on the transport properties. The effect of the coagulation bath temperature on the membrane properties is of interest for this study. Membranes are characterized by pure water flux, permeability, porosity and retention of methylene blue. The low temperature of coagulation bath improve the membrane’s rejection and its influence was most notable.

Preparation and Characterization of Fluorescent Derivatives of Lysozyme

NASA Technical Reports Server (NTRS)

Smith, Lori; Pusey, Marc

1998-01-01

Fluorescence is one of the most versatile and powerful tools for the study of macromolecules. However, its use in macromolecular crystal growth studies is hampered by the necessity of preparing fluorescent derivatives where the probe does not markedly affect the crystal packing. Alternatively, one can prepare derivatives of limited utility if it is known that they will not affect the specific goals of a given study. We have prepared a number of fluorescent derivatives of chicken egg white lysozyme, covalently attaching fluorescent probes to two different sites on the protein molecule. The first site is the side chain carboxyl group of ASP 101. Amine containing probes such as lucifer yellow, cascade blue, and 5- (2-aminoethyl) aminonapthalene-l-sulfonic acid (EDANS) have been attached using a carbodiimide coupling procedure. ASP 101 lies within the active site cleft, and it is believed that the probes are "buried" within that cleft. This is supported by the fact that all such derivatives have been found to crystallize, with the crystals being fluorescent. Tetragonal crystals of the lucifer yellow derivative have been found to diffract to at least 1.9 A resolution. X-ray diffraction data has been acquired and we are now working on the structure of this derivative. The second group of derivatives is to the N-terminal amine group. The derivatization reaction is performed by using a succinimidyl ester of the probe to be attached. Fluorescent probes such as pyrene acetic acid, 5-carboxyfluorescein, and Oregon green have been attached to this site. We have had little success in crystallizing these derivatives, probably because this site is part of the contact region between the 43 helix chains. However, these sites do not interfere with formation of the 43 helices and the derivatives are suitable for study of their formation in solution. The derivatives are being characterized by steady state and lifetime fluorescence methods, and the presentation will discuss these

Preparation and characterization of graphene/turbostratic carbon derived from chitosan film for supercapacitor electrodes

NASA Astrophysics Data System (ADS)

Hanappi, M. F. Y. M.; Deraman, M.; Suleman, M.; Othman, M. A. R.; Basri, N. H.; Nor, N. S. M.; Hamdan, E.; Sazali, N. E. S.; Tajuddin, N. S. M.

2018-04-01

Electrochemical capacitors or supercapacitors are the potential energy storage devices which are known for having higher specific capacitance and specific energy than electrolytic capacitors. Electric double-layer capacitors (EDLCs) also referred as ultracapacitors is a class of supercapacitors that employ different forms of carbon like activated carbon, CNT, graphene etc., as electrodes. The performance of the supercapacitors is determined by its components namely electrolyte, electrode, etc. Carbon electrodes with high surface area and desired pore size distribution are always preferred and which can be tailored by varying the precursor and method of preparation. In recent years, owing to their low cost, ease of synthesis, high stability and conductivity, the activated carbons derived from biomass precursors have been investigated as potential electrode material for the EDLCs. In this report, we present the preparation and characterization of graphene/turbostratic carbon monolith (CM) electrodes from the carbon grains (CGs) obtained by carbonization (under the flow of nitrogen, N2 gas and over a temperature range from 600 °C to 1000 °C) of biomass precursor chitosan film. The procedure to prepare the chitosan film is described elsewhere. The carbon grains are characterized using Raman spectroscopy (RS) and X-ray diffraction (XRD). We expect that the CGs would have the similar characteristics as graphene and would be a potential electrode material for EDLCs application.

Preparation and characterization of nanosilica from oil shale ash.

PubMed

Li, Jinhong; Qian, Tingting; Tong, Lingxin; Shen, Jie

2014-05-01

Nano-sized silica powders was prepared using oil shale ash (OSA) as starting materials. A combined process was proposed for the utilization of OSA in the production of the nanosilica, including three stages: calcination, alkaline leaching and carbon dioxide separation. Effects of the calcining temperature, sodium hydroxide concentration and holding time on the desilication ratio were investigated. The microstructure and morphologies of the nano-sized silica were characterized by X-ray diffraction, transmission electron microscopy, and Brunauer-Emmett-Teller nitrogen-gas adsorption method. The results indicated that the obtained powders with particle size of about 40 nm are homegeneously dispersed and its specific surface area is 387 m2/g. The properties of the nano-sized silica powder meet the requirements of the Chinese Chemical Industry Standard HG/T 3061-1999.

Preparation and characterization of graphene/CdS nanocomposites

NASA Astrophysics Data System (ADS)

Wu, Jili; Bai, Song; Shen, Xiaoping; Jiang, Lei

2010-11-01

Graphene-based nanocomposites are emerging as a new class of materials that hold promise for many applications. In this paper, we present a facile approach for the preparation of graphene/CdS nanocomposites through simple reflux processes, in which thiourea (CS(NH 2) 2) and thioacetamide (C 2H 5NS) act as a sulphide source, respectively. The samples were characterized by the X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectrum (FT-IR), ultraviolet-visible (UV-vis) spectroscopy and thermogravimetry analysis. It was shown that in the nanocomposites, the CdS nanoparticles were densely and uniformly deposited on the graphene sheets, and the sulphide source used has a great influence on the morphology, structure and property of the graphene/CdS nanocomposites. The good distribution of CdS nanoparticles on graphene sheets guarantees the efficient optoelectronic properties of graphene/CdS and would be promising for practical applications in future nanotechnology.

Preparation and characterization of biocompatible magnetic carbon nanotubes

NASA Astrophysics Data System (ADS)

Shan, Yan; Chen, Kezheng; Yu, Xuegang; Gao, Lian

2010-11-01

Magnetic carbon nanotubes consisting of multi-wall carbon nanotubes (MWNTs) core and Fe3O4 shell were successfully prepared by in situ thermal decomposition of Fe(acac)3 or FeCl3 or Fe(CO)5 in 2-pyrrolidone containing acid treated MWNTs at 240 °C with the protection of nitrogen gas. The samples were characterized by TEM, XRD, SEAD, XPS and superconducting quantum interference device. Also, their biocompatibility was compared with naked carbon nanotubes. The results showed that after coated with Fe3O4 nanoparticles, the obtained magnetic carbon nanotubes show superparamagnetic characteristic at room temperature, and their blocking temperature is about 80 K. The magnetic properties of the nanotubes are relevant to the content of magnetic particles, increasing content of magnetic nanoparticles leads to higher blocking temperature and saturation magnetization. The results of antimicrobial activities to bacterial cells (Escherichia coli) showed that the MWNTs have antimicrobial activity, while the magnetic nanotubes are biocompatible even with a higher concentration than that of MWNTs.

Preparation, characterization, and in vitro release study of albendazole-encapsulated nanosize liposomes

PubMed Central

Panwar, Preety; Pandey, Bhumika; Lakhera, P C; Singh, K P

2010-01-01

The purpose of the present study was to formulate effective and controlled release albendazole liposomal formulations. Albendazole, a hydrophobic drug used for the treatment of hydatid cysts, was encapsulated in nanosize liposomes. Rapid evaporation method was used for the preparation of albendazole-encapsulated conventional and PEGylated liposomes consisting of egg phosphatidylcholine (PC) and cholesterol (CH) in the molar ratios of (6:4) and PC:CH: polyethylene glycol (PEG) (5:4:1), respectively. In this study, PEGylated and conventional liposomes containing albendazole were prepared and their characteristics, such as particle size, encapsulation efficiency, and in vitro drug release were investigated. The drug encapsulation efficiency of PEGylated and conventional liposomes was 81% and 72%, respectively. The biophysical characterization of both conventional and PEG-coated liposomes were done by transmission electron microscopy and UV-vis spectrophotometry. Efforts were made to study in vitro release of albendazole. The drug release rate showed decrease in albendazole release in descending order: free albendazole, albendazole-loaded conventional liposomes, and least with albendazole-loaded PEG-liposomes. Biologically relevant vesicles were prepared and in vitro release of liposome-entrapped albendazole was determined. PMID:20309396

Kombucha-synthesized bacterial cellulose: preparation, characterization, and biocompatibility evaluation.

PubMed

Zhu, Changlai; Li, Feng; Zhou, Xinyang; Lin, Lin; Zhang, Tianyi

2014-05-01

Bacterial cellulose (BC) is a natural biomaterial with unique properties suitable for tissue engineering applications, but it has not yet been used for preparing nerve conduits to repair peripheral nerve injuries. The objectives of this study were to prepare and characterize the Kampuchea-synthesized bacterial cellulose (KBC) and further evaluate the biocompatibility of KBC with peripheral nerve cells and tissues in vitro and in vivo. KBC membranes were composed of interwoven ribbons of about 20-100 nm in width, and had a high purity and the same crystallinity as that of cellulose Iα. The results from light and scanning electron microscopy, MTT assay, flow cytometry, and RT-PCR indicated that no significant differences in the morphology and cell function were observed between Schwann cells (SCs) cultured on KBC membranes and glass slips. We also fabricated a nerve conduit using KBC, which was implanted into the spatium intermusculare of rats. At 1, 3, and 6 weeks post-implantation, clinical chemistry and histochemistry showed that there were no significant differences in blood counts, serum biochemical parameters, and tissue reactions between implanted rats and sham-operated rats. Collectively, our data indicated that KBC possessed good biocompatibility with primary cultured SCs and KBC did not exert hematological and histological toxic effects on nerve tissues in vivo. Copyright © 2013 Wiley Periodicals, Inc.

Cholesterol-imprinted macroporous monoliths: Preparation and characterization.

PubMed

Stepanova, Mariia А; Kinziabulatova, Lilia R; Nikitina, Anna A; Korzhikova-Vlakh, Evgenia G; Tennikova, Tatiana B

2017-11-01

The development of sorbents for selective binding of cholesterol, which is a risk factor for cardiovascular disease, has a great importance for analytical science and medicine. In this work, two series of macroporous cholesterol-imprinted monolithic sorbents differing in the composition of functional monomers (methacrylic acid, butyl methacrylate, 2-hydroxyethyl methacrylate and ethylene dimethacrylate), amount of a template (4, 6 and 8 mol%) used for molecular imprinting, as well as mean pore size were synthesized by in situ free-radical process in stainless steel housing of 50 mm × 4.6 mm i.d. All prepared materials were characterized regarding to their hydrodynamic permeability and porous properties, as well as examined by BET and SEM methods. Imprinting factors, apparent dynamic dissociation constants, the maximum binding capacity, the number of theoretical plates and the height equivalent to a theoretical palate of MIP monoliths at different mobile phase flow rates were determined. The separation of a mixture of structural analogues, namely, cholesterol and prednisolone, was demonstrated. Additionally, the possibility of using the developed monoliths for cholesterol solid-phase extraction from simulated biological solution was shown. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A review of tin oxide-based catalytic systems: Preparation, characterization and catalytic behavior

NASA Technical Reports Server (NTRS)

Hoflund, Gar B.

1987-01-01

This paper reviews the important aspects of the preparation, characterization and catalytic behavior of tin oxide-based catalytic systems including doped tin oxide, mixed oxides which contain tin oxide, Pt supported on tin oxide and Pt/Sn supported on alumina. These systems have a broad range of applications and are continually increasing in importance. However, due to their complex nature, much remains to be understood concerning how they function catalytically.

Duloxetine HCl lipid nanoparticles: preparation, characterization, and dosage form design.

PubMed

Patel, Ketan; Padhye, Sameer; Nagarsenker, Mangal

2012-03-01

Solid lipid nanoparticles (SLNs) of duloxetine hydrochloride (DLX) were prepared to circumvent the problems of DLX, which include acid labile nature, high first-pass metabolism, and high-dosing frequency. The DLX-SLNs were prepared by using two different techniques, viz. solvent diffusion method and ultrasound dispersion method, and evaluated for particle size, zeta potential, entrapment efficiency, physical characteristics, and chemical stability. Best results were obtained when SLNs were prepared by ultrasound dispersion method using glyceryl mono stearate as solid lipid and DLX in ratio of 1:20 and mixture of polysorbate 80 and poloxamer 188 as surfactant in concentration of 3%. The mean particle size of formulation and entrapment efficiency was 91.7 nm and 87%, respectively, and had excellent stability in acidic medium. Differential scanning calorimetry and X-ray diffraction data showed complete amorphization of DLX in lipid. In vitro drug release from SLNs was observed for 48 h and was in accordance with Higuchi kinetics. In vivo antidepressant activity was evaluated in mice by forced swim test. DLX-SLNs showed significant enhancement in antidepressant activity at 24 h when administered orally in comparison to drug solution. These results confirm the potential of SLNs in enhancing chemical stability and improving the efficacy of DLX via oral route. The SLN dispersion was converted into solid granules by adsorbing on colloidal silicon dioxide and characterized for particle size after redispersion, morphology, and flow properties. Results indicated that nanoparticles were successfully adsorbed on the carrier and released SLNs when dispersed in water.

Multiple-step preparation and physicochemical characterization of crystalline α-germanium hydrogenphosphate

NASA Astrophysics Data System (ADS)

Romano, Ricardo; Ruiz, Ana I.; Alves, Oswaldo L.

2004-04-01

The reaction between germanium oxide and phosphoric acid has previously been described and led to impure germanium hydrogenphosphate samples with low crystallinity. A new multiple-step route involving the same reaction under refluxing and soft hydrothermal conditions is described for the preparation of pure and crystalline α-GeP. The physicochemical characterization of the samples allows accompaniment of the reaction evolution as well as determining short- and long-range structural organization. The phase purity of the α-GeP sample was confirmed by applying Rietveld's profile analysis, which also determined the cell parameters of its crystals.

Effort versus reward: preparing samples for fungal community characterization in high-throughput sequencing surveys of soils

USDA-ARS?s Scientific Manuscript database

Next generation fungal amplicon sequencing is being used with increasing frequency to study fungal diversity in various ecosystems; however, the influence of sample preparation on the characterization of fungal community is poorly understood. We investigated the effects of four procedural modificati...

Preparation, characterization and dynamical mechanical properties of dextran-coated iron oxide nanoparticles (DIONPs).

PubMed

Can, Hatice Kaplan; Kavlak, Serap; ParviziKhosroshahi, Shahed; Güner, Ali

2018-03-01

Dextran-coated iron oxide nanoparticles (DIONPs) with appropriate surface chemistry exhibit many interesting properties that can be exploited in a variety of biomedical applications such as magnetic resonance imaging (MRI) contrast enhancement, tissue repair, hyperthermia, drug delivery and in cell separation. This paper reports the experimental detail for preparation, characterization and investigation of thermal and dynamical mechanical characteristics of the dextran-coated Fe 3 O 4 magnetic nanoparticles. In our work, DIONPs were prepared in a 1:2 ratio of Fe(II) and Fe(III) salt in the HCl solution with NaOH at given temperature. The obtained dextran-coated iron-oxide nanoparticles structure-property correlation was characterized by spectroscopic methods; attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and XRD. Coating dextran on the iron-oxide proof of important peaks can be seen from the ATR-FTIR. Dramatic crystallinity increment can be observed from the XRD pattern of the iron-oxide dextran nanoparticles. The thermal analysis was examined by differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA) and differential thermal analysis (DTA). Dynamical mechanical properties of dextran nanoparticles were analysed by dynamic mechanical analysis (DMA). Thermal stability of the iron oxide dextran nanoparticles is higher than that of the dextran.

Preparation and characterization of a thermoresponsive gigaporous medium for high-speed protein chromatography.

PubMed

Qu, Jian-Bo; Chen, Yan-Li; Huan, Guan-Sheng; Zhou, Wei-Qing; Liu, Jian-Guo; Zhu, Hu; Zhang, Xiao-Yun

2015-01-01

A high-speed thermoresponsive medium was developed by grafting poly(N-isopropylacrylamide-co-butyl methacrylate) (P(NIPAM-co-BMA)) brushes onto gigaporous polystyrene (PS) microspheres via surface-initiated atom transfer radical polymerization (ATRP) technique, which has strong mechanical strength, good chemical stability and high mass transfer rate for biomacromolecules. The gigaporous structure, surface chemical composition, static protein adsorption, and thermoresponsive chromatographic properties of prepared medium (PS-P(NIPAM-co-BMA)) were characterized in detail. Results showed that the PS microspheres were successfully grafted with P(NIPAM-co-BMA) brushes and that the gigaporous structure was robustly maintained. After grafting, the nonspecific adsorption of proteins on PS microspheres was greatly reduced. A column packed with PS-P(NIPAM-co-BMA) exhibited low backpressure and significant thermo-responsibility. By simply changing the column temperature, it was able to separate three model proteins at the mobile phase velocity up to 2167 cm h(-1). In conclusion, the thermoresponsive polymer brushes grafted gigaporous PS microspheres prepared by ATRP are very promising in 'green' high-speed preparative protein chromatography. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparative isolation and characterization of some minor impurities of astaxanthin by high-performance liquid chromatography.

PubMed

Rao, R Nageswara; Alvi, S Naseeruddin; Rao, B Nageswara

2005-05-27

A simple and rapid preparative high-performance liquid chromatography (HPLC) method has been developed to isolate and characterize some minor impurities of astaxanthin using a normal-phase Lichrosorb silica column with n-hexane-acetone-tetrahydrofuran (90:2:8, v/v/v) as mobile-phase and detection at 475 nm. The isolated impurities were characterized as astacene, dehydro astacene and apoastaxanthinal by UV-vis, ESI-MS, 1H and 13C NMR spectroscopy and the molecular structures were assigned. The impurities collected using the developed conditions were over 98% pure.

Crosslinked type II collagen matrices: preparation, characterization, and potential for cartilage engineering.

PubMed

Pieper, J S; van der Kraan, P M; Hafmans, T; Kamp, J; Buma, P; van Susante, J L C; van den Berg, W B; Veerkamp, J H; van Kuppevelt, T H

2002-08-01

The limited intrinsic repair capacity of articular cartilage has stimulated continuing efforts to develop tissue engineered analogues. Matrices composed of type II collagen and chondroitin sulfate (CS), the major constituents of hyaline cartilage, may create an appropriate environment for the generation of cartilage-like tissue. In this study, we prepared, characterized, and evaluated type 11 collagen matrices with and without CS. Type II collagen matrices were prepared using purified, pepsin-treated, type II collagen. Techniques applied to prepare type I collagen matrices were found unsuitable for type II collagen. Crosslinking of collagen and covalent attachment of CS was performed using 1-ethyl-3-(3-dimethyl aminopropyl)carbodiimide. Porous matrices were prepared by freezing and lyophilization, and their physico-chemical characteristics (degree of crosslinking, denaturing temperature, collagenase-resistance, amount of CS incorporated) established. Matrices were evaluated for their capacity to sustain chondrocyte proliferation and differentiation in vitro. After 7 d of culture, chondrocytes were mainly located at the periphery of the matrices. In contrast to type I collagen, type II collagen supported the distribution of cells throughout the matrix. After 14 d of culture, matrices were surfaced with a cartilagenous-like layer, and occasionally clusters of chondrocytes were present inside the matrix. Chondrocytes proliferated and differentiated as indicated by biochemical analyses, ultrastructural observations, and reverse transcriptase PCR for collagen types I, II and X. No major differences were observed with respect to the presence or absence of CS in the matrices.

Preparation, characterization and gas sensing performance of BaTiO3 nanostructured thin films

NASA Astrophysics Data System (ADS)

Suryawanshi, Dinesh N.; Pathan, Idris G.; Bari, Anil. R.; Patil, Lalchand A.

2018-05-01

Spray pyrolysis techniques was employed to prepare BaTiO3 thin films. AR grade solutions of Barium chloride (0.05 M) and Titanium chloride (0.05 M) were mixed in the proportion of 30:70, 50:50 and 70:30. The solutions were sprayed on quartz substrate heated at 350°C temperature to obtain the films. These thin films were annealed for a two hours at 600°C in air medium respectively. The prepared thin films were characterized using XRD, FESEM, EDAX, TEM. The electrical and gas sensing properties of these films were investigated. 50:50 film showed better response to Liquid Petroleum Gas (LPG) as compare 30:70 and 70:30 films.

PREPARATION AND CHARACTERIZATION OF ORALLY DISINTEGRATING LORATADINE TABLETS MANUFACTURED WITH CO-PROCESSED MIXTURES.

PubMed

Amelian, Aleksandra; Szekalska, Marta; Wilczewska, Agnieszka Zofia; Basa, Anna; Winnicka, Katarzyna

2016-01-01

The aim of this study was to develop orally disintegrated tablets (ODT) with loratadine using Parteck ODT and Ludiflash--new commercially available tableting excipients based on co-processed mannitol. ODT containing loratadine were prepared with 3% addition of various superdisintegrants (AcDiSol, Kollidon CL-F and Kollidon CL-SF) by direct compression method. Obtained tablets were characterized for friability, pore structure, and wetting and disintegration time measured by four independents methods. In order to identify possible interactions between loratadine and the excipients, differential scanning calorimetry was used. The results showed that all formulated ODT were characterized by appropriate mechanical properties (friability < 1%), the uniform content of the drug substance and pleasant mouth feeling. Disintegration time below 30 s was observed in formulations with crospovidones as disintegrant.

Design, Synthesis, and Characterization of Nanostructured Materials for Energy Storage Devices and Flexible Chemical Sensors

NASA Astrophysics Data System (ADS)

Kang, Ning

Nanomaterials have shown increasing applications in the design and fabrication of functional devices such as energy storage devices and sensor devices. A key challenge is the ability to harness the nanostructures in terms of size, shape, composition and structure so that the unique nanoscale functional properties can be exploited. This dissertation describes our findings in design, synthesis, and characterization of nanoparticles towards applications in two important fronts. The first involves the investigation of nanoalloy catalysts and functional nanoparticles for energy storage devices, including Li-air and Li-ion batteries, aiming at increasing the capacity and cycle performance. Part of this effort focuses on design of bifunctional nanocatalysts through alloying noble metal with non-noble transition metal to improve the ORR and OER activity of Li-air batteries. By manipulating the composition and alloying structure of the catalysts, synergetic effect has been demonstrated, which is substantiated by both experimental results and theoretical calculation for the charge/discharge process. The other part of the effort focuses on modification of Si nanoparticles towards high-capacity anode materials. The modification involved dopant elements, carbon coating, and graphene composite formation to manipulate the ability of the nanoparticles in accommodating the volume expansion. The second part focuses on the design, preparation and characterization of metal nanoparticles and nanocomposite materials for the application in flexible sensing devices. The investigation focuses on fabrication of a novel class of nanoparticle-nanofibrous membranes consisting of gold nanoparticles embedded in a multi-layered fibrous membrane as a tunable interfacial scaffold for flexible sweat sensors. Sensing responses to different ionic species in aqueous solutions and relative humidity changes in the environment were demonstrated, showing promising potential as flexible sensing devices for

Preparation and characterization of solid dispersion freeze-dried efavirenz - polyvinylpyrrolidone K-30.

PubMed

Fitriani, Lili; Haqi, Alianshar; Zaini, Erizal

2016-01-01

The aim of this research is to prepare and characterize solid dispersion of efavirenz - polyvinylpyrrolidone (PVP) K-30 by freeze drying to increase its solubility. Solid dispersion of efavirenz - PVP K-30 was prepared by solvent evaporation method with ratio 2:1, 1:1, and 1:2 and dried using a freeze dryer. Characterizations were done by scanning electron microscopy (SEM), powder X-ray diffraction analysis, differential thermal analysis (DTA), and Fourier transform infrared (FT-IR) spectroscopy. Solubility test was carried out in CO2-free distilled water, and efavirenz assay was conducted using high-performance liquid chromatography with acetonitrile:acetic acid (80:20) as the mobile phases. Powder X-ray diffractogram showed a decrease in the peak intensity, which indicated the crystalline altered to amorphous phase. DTA thermal analysis showed a decrease in the melting point of the solid dispersion compared to intact efavirenz. SEM results indicated the changes in the morphology of the crystal into an amorphous form compared to pure components. FT-IR spectroscopy analysis showed a shift wavenumber of the spectrum efavirenz and PVP K-30. The solubility of solid dispersion at ratio 2:1, 1:1, and 1:2 was 6.777 μg/mL, 6.936 μg/mL, and 14,672 μg/mL, respectively, whereas the solubility of intact efavirenz was 0.250 μg/mL. In conclusion, the solubility of solid dispersion increased significantly (P < 0.05).

Characterization of fermented seaweed sauce prepared from nori (Pyropia yezoensis).

PubMed

Uchida, Motoharu; Kurushima, Hirotaka; Ishihara, Kenji; Murata, Yuko; Touhata, Ken; Ishida, Noriko; Niwa, Kentaro; Araki, Toshiyoshi

2017-03-01

High-salt content seaweed sauces were prepared for the first time using nori (Pyropia yezoensis) by fermentation and characterized. Components and taste of the two nori sauces (NSs) prepared separately were compared with those of soy and fish sauces. The NSs were rich in total nitrogen compounds (1.5 g N/100 ml on average) and potassium (880 mg/100 g), and had a unique free amino acid composition (e.g., taurine 617 mg/100 g), explaining their unique taste as evaluated by a taste sensing system. As for their food function, inhibitory activity of angiotensin-converting enzyme was observed. As for their food safety, arsenic was detected at a 0.8 mg/100 g level in total, but inorganic arsenic was not detected (<0.05 mg/100 g) and not regarded as a problem. Allergy-causing substances contained in wheat, soy beans, and crustaceans were not detected (<0.1 mg/100 g) with NSs. These results suggest that the nori sauce has a high potential as a novel nutritional source for humans. Copyright © 2016 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Optical characterization of pure and Al-doped ZnO prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Belka, Radosław; Keczkowska, Justyna; Kasińska, Justyna

2016-09-01

In this paper the preparation process and optical characterization of pure and Al3+ doped zinc oxide (Al:ZnO) coatings will be presented. ZnO based materials have been studied extensively due to their potential applications in optoelectronic devices as conductive gas sensors, transparent conductive, electrodes, solar cell windows, varistors, UVfilters or photovoltaic cells. It is II-VI semiconductor with wide-band gap of 3.37 eV and large exciton binding energy of 60meV. It is possible to improve the conductivity of ZnO coating by intentionally doping ZnO with aluminium ions during preparation process. Such transparent and conducting thin films, known as AZO (Aluminium Zinc Oxide) films, are very good candidate for application as transparent conducting materials in many optoelectronic devices. The well-known sol-gel method is used for preparation of solution, coated on glass substrates by dip coating process. Prepared samples were investigated by Raman and UV-VIS spectroscopy. Transmittance as well as specular and diffuse reflectance spectroscopy methods were used for studies of optical parameters. We found that Al admixture influences on optical bandgap of ZnO.

Characterization of amylose nanoparticles prepared via nanoprecipitation: Influence of chain length distribution.

PubMed

Chang, Yanjiao; Yang, Jingde; Ren, Lili; Zhou, Jiang

2018-08-15

The influence of chain length distribution of amylose on size and structure of the amylose nanoparticles (ANPs) prepared through nanoprecipitation was investigated. Amylose with different chain length distributions was obtained by β-amylase treating amylose paste for different times and measured by size exclusion chromatography (SEC) and fluorophore-assisted carbohydrate electrophoresis (FACE). ANPs prepared via precipitation were characterized by using dynamic light scattering (DLS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Results showed that the β-amylase treatments led to decrease in chain length of amylose, and it was the most important factor affecting size of ANPs. When hydrolysis degree of amylose was 52.8%, mean size of ANPs decreased from 206.4 nm to 102.7 nm. All the ANPs displayed a V-type crystalline structure and the effect of amylose chain length on crystallinity of the precipitated ANPs was negligible in the investigated range. Copyright © 2018 Elsevier Ltd. All rights reserved.

[Preparation and spectral characterization of CdS(y)Te(1-y) thin films].

PubMed

Li, Wei; Feng, Liang-Huan; Wu, Li-Li; Zhang, Jing-Quan; Li, Bing; Lei, Zhi; Cai, Ya-Ping; Zheng, Jia-Gui; Cai, Wei; Zhang, Dong-Min

2008-03-01

CdS(y)Te(1-y) (0 < or = y < or = 1) polycrystalline thin films were prepared on glass substrates by co-evaporation of powders of CdTe and CdS. For the characterization of the structure and composition of the CdS(y)Te(1-y) thin films the X-ray diffraction (XRD) and energy-dispersive spectroscopy (EDS) were used. The results indicate that the values of sulfur content y detected and controlled by the quartz wafer detector show good agreement with the EDS results. The films were found to be cubic for x < 0. 3, and hexagonal for x > or = 0.3. The 20-50 nm of grain sizes for CdS(y)Te(1-y) thin films were calculated using a method of XRD analysis. Finally, the optical properties of CdS(y)Te(1-y) thin films were characterized by UV-Vis-NIR spectroscopy alone. According to a method from Swanepoel, together with the first-order Sellmeier model, the thickness, of d-535 nm, energy gap of E(g)-1.41 eV, absorption coefficient, alpha(lambda) and refractive index, n(lambda) of CdS(0.22) Te(0.78) thin films were determined from the transmittance at normal incidence of light in the wavelength range 300-2 500 nm. The results also indicate that the CdS(y)Te(1-y) thin films with any composition (0 < or = y < or = 1) can be prepared by co-evaporation, and the method to characterize the optical properties of CdS(y)Te(1-y) thin films can be implemented for other semiconductor thin films.

Niosomes encapsulating Ibuprofen-cyclodextrin complexes: preparation and characterization.

PubMed

Marianecci, Carlotta; Rinaldi, Federica; Esposito, Sara; Di Marzio, Luisa; Carafa, Maria

2013-08-01

A new delivery system based on ibuprofen-β-cyclodextrin (βCd) complexation and its loading into non-ionic surfactant vesicles (NSVs) was developed to improve ibuprofen therapeutic efficacy in topical formulations. The proposed strategy exploits the well known solubilizing and stabilizing properties of cyclodextrins together with the high tolerability and percutaneous absorption enhancing properties of NSVs. The complexing capacity of Cds in the presence of Ibuprofen in aqueous solution was evaluated by means of phase solubility studies. The technique used to obtain solid ibuprofen-βCd complexes was the co-lyophilization method. The influence of the preparation method on the physicochemical properties of the final product was evaluated by means of Fourier Transform Infrared Spectroscopy and Differential scanning calorimetry studies. Ibuprofen-βCd complexes were included in Tween 20/Cholesterol vesicles and characterized in terms of size, zeta (ζ)-potential, stability, drug entrapment efficiency and drug release. The best ibuprofen-βCd-NSV system exhibited in vitro drug permeation properties significantly improved with respect to those of the plain drug suspension.

Preparation and Characterization of Graphene Oxide Paper

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

Dikin,D.; Stankovich, S.; Zimney, E.

2007-01-01

Free-standing paper-like or foil-like materials are an integral part of our technological society. Their uses include protective layers, chemical filters, components of electrical batteries or supercapacitors, adhesive layers, electronic or optoelectronic components, and molecular storage. Inorganic 'paper-like' materials based on nanoscale components such as exfoliated vermiculite or mica platelets have been intensively studied and commercialized as protective coatings, high-temperature binders, dielectric barriers and gas-impermeable membranes. Carbon-based flexible graphite foils composed of stacked platelets of expanded graphite have long been used in packing and gasketing applications because of their chemical resistivity against most media, superior sealability over a wide temperature range,more » and impermeability to fluids. The discovery of carbon nanotubes brought about bucky paper, which displays excellent mechanical and electrical properties that make it potentially suitable for fuel cell and structural composite applications. Here we report the preparation and characterization of graphene oxide paper, a free-standing carbon-based membrane material made by flow-directed assembly of individual graphene oxide sheets. This new material outperforms many other paper-like materials in stiffness and strength. Its combination of macroscopic flexibility and stiffness is a result of a unique interlocking-tile arrangement of the nanoscale graphene oxide sheets.« less

Preparation and characterization of graphene oxide paper.

PubMed

Dikin, Dmitriy A; Stankovich, Sasha; Zimney, Eric J; Piner, Richard D; Dommett, Geoffrey H B; Evmenenko, Guennadi; Nguyen, SonBinh T; Ruoff, Rodney S

2007-07-26

Free-standing paper-like or foil-like materials are an integral part of our technological society. Their uses include protective layers, chemical filters, components of electrical batteries or supercapacitors, adhesive layers, electronic or optoelectronic components, and molecular storage. Inorganic 'paper-like' materials based on nanoscale components such as exfoliated vermiculite or mica platelets have been intensively studied and commercialized as protective coatings, high-temperature binders, dielectric barriers and gas-impermeable membranes. Carbon-based flexible graphite foils composed of stacked platelets of expanded graphite have long been used in packing and gasketing applications because of their chemical resistivity against most media, superior sealability over a wide temperature range, and impermeability to fluids. The discovery of carbon nanotubes brought about bucky paper, which displays excellent mechanical and electrical properties that make it potentially suitable for fuel cell and structural composite applications. Here we report the preparation and characterization of graphene oxide paper, a free-standing carbon-based membrane material made by flow-directed assembly of individual graphene oxide sheets. This new material outperforms many other paper-like materials in stiffness and strength. Its combination of macroscopic flexibility and stiffness is a result of a unique interlocking-tile arrangement of the nanoscale graphene oxide sheets.

A protocol for preparing, characterizing and using three RNA-specific, live cell imaging probes: E36, E144 and F22.

PubMed

Li, Qian; Chang, Young-Tae

2006-01-01

This protocol outlines a methodology for the preparation and characterization of three RNA-specific fluorescent probes (E36, E144 and F22) and their use in live cell imaging. It describes a detailed procedure for their chemical synthesis and purification; serial product characterization and quality control tests, including measurements of their fluorescence properties in solution, measurement of RNA specificity and analysis of cellular toxicity; and live cell staining and counterstaining with Hoechst or DAPI. Preparation and application of these RNA imaging probes takes 1 week.

Preparation, Characterization, and Catalytic Activity of MoCo/USY Catalyst on Hydrodeoxygenation Reaction of Anisole

NASA Astrophysics Data System (ADS)

Nugrahaningtyas, K. D.; Suharbiansah, R. S. R.; Rahmawati, F.

2018-03-01

This research aims to prepare, characterize, and study the catalytic activity of Molybdenum (Mo) and Cobalt (Co) metal with supporting material Ultra Stable Y-Zeolite (USY), to produce catalysts with activity in hydrotreatment reaction and in order to eliminate impurities compounds that containing unwanted groups heteroatoms. The bimetallic catalysts MoCo/USY were prepared by wet impregnation method with weight variation of Co metal 0%, 2%, 4%, 6%, 8%, and Mo metal 8% (w/w), respectively. Activation method of the catalyst included calcination, oxidation, reduction and the crystallinity was characterized using X-ray diffraction (XRD), the acidity of the catalyst was analyzed using Fourier Transform Infrared Spectroscopy (FT-IR) and gravimetry method, minerals present in the catalyst was analyzed using X-Ray Fluorescence (XRF), and surface of the catalyst was analyzed using Surface Area Analyzer (SAA). Catalytic activity test (benzene yield product) of MoCo/USY on hydrodeoxigenation reaction of anisole aimed to determine the effect of Mo-Co/USY for catalytic activity in the reaction hydrodeoxigenation (HDO) anisole. Based on characterization and test of catalytic activity, it is known that catalytic of MoCo/USY 2% (catalyst B) shows best activities with acidity of 10.209 mmol/g, specific area of catalyst of 426.295 m2/g, pore average of 14.135 Å, total pore volume 0.318 cc/g, and total yield of HDO products 6.06%.

[Preparation and performance characterization of gold nanoparticles modified chiral capillary electrochromatography stationary phase].

PubMed

Xiong, Lele; Li, Ruijun; Ji, Yibing

2017-07-08

Gold nanoparticles (GNPs, 15 nm) were prepared and introduced to amino groups derived silica monolithic column. Bovine serum albumin (BSA) was immobilized via covalent modification method onto the carboxylic functionalized GNPs to afford chiral stationary phase (CSP) for enantioseparation. GNPs were well dispersed and successfully incorporated onto the columns with the contents as high as 17.18% by characterization method such as transmission electron microscopy (TEM), ultraviolet (UV)-visible absorption spectra and scanning electron microscopy (SEM). The preparation conditions of the BSA modified CSP were optimized and 10% (v/v) 3-aminopropyltriethoxysilane (APTES) and 15 g/L BSA were selected as appropriate reaction conditions. The enantioseparation performance of the BSA modified CSP has been investigated by capillary electrochromatography (CEC). Enantiomers of tryptophan, ephedrine and atenolol were resolved, and the baseline separation of tryptophan was achieved. Meanwhile, the influences of pH value, buffer concentrations and applied voltages used on the chiral separation were studied, and the optimal separation conditions were 10 mmol/L phosphate buffer at pH 7.4 and 15 kV applied voltages. In comparison with the BSA modified CSP prepared by physical adsorption, the CSP prepared by covalent modification method had better separation results, and the analytes could be separated directly without pre-column derivatization. In addition, the prepared BSA modified CSP exhibited good run to run repeatability with relative standard deviations (RSDs) of the migration times and selectivity factors not more than 2.3% and 0.96%, respectively. This work offers a good thinking for modification with other proteins or other types of chiral selectors.

Magnetic hyaluronate hydrogels: preparation and characterization

NASA Astrophysics Data System (ADS)

Tóth, Ildikó Y.; Veress, Gábor; Szekeres, Márta; Illés, Erzsébet; Tombácz, Etelka

2015-04-01

A novel soft way of hyaluronate (HyA) based magnetic hydrogel preparation was revealed. Magnetite nanoparticles (MNPs) were prepared by co-precipitation. Since the naked MNPs cannot be dispersed homogenously in HyA-gel, their surface was modified with natural and biocompatible chondroitin-sulfate-A (CSA) to obtain CSA-coated MNPs (CSA@MNPs). The aggregation state of MNPs and that loaded with increasing amount of CSA up to 1 mmol/g was measured by dynamic light scattering at pH~6. Only CSA@MNP with ≥0.2 mmol/g CSA content was suitable for magnetic HyA-gel preparation. Rheological studies showed that the presence of CSA@MNP with up to 2 g/L did not affect the hydrogel's rheological behavior significantly. The results suggest that the HyA-based magnetic hydrogels may be promising formulations for future biomedical applications, e.g. as intra-articular injections in the treatment of osteoarthritis.

Preparation and characterization of glass hollow fiber membrane for water purification applications.

PubMed

Makhtar, Siti Nurfatin Nadhirah Mohd; Rahman, Mukhlis A; Ismail, Ahmad Fauzi; Othman, Mohd Hafiz Dzarfan; Jaafar, Juhana

2017-07-01

This work discusses the preparation and characterizations of glass hollow fiber membranes prepared using zeolite-5A as a starting material. Zeolite was formed into a hollow fiber configuration using the phase inversion technique. It was later sintered at high temperatures to burn off organic materials and change the zeolite into glass membrane. A preliminary study, that used thermogravimetric analysis (TGA), X-ray diffraction (XRD), and Fourier transform infrared (FTIR), confirmed that zeolite used in this study changed to glass at temperatures above 1000 °C. The glass hollow fiber membranes prepared using the phase inversion technique has three different microstructures, namely (i) sandwich-like structure that originates from inner layer, (ii) sandwich-like that originates from outer layer, and (iii) symmetric sponge like. These variations were influenced by zeolite weight loading and the flow rate of water used to form the lumen. The separation performances of the glass hollow fiber membrane were studied using the pure water permeability and the rejection test of bovine serum albumin (BSA). The glass hollow fiber membrane prepared from using 48 wt% zeolite loading and bore fluid with 9 mL min -1 flow rate has the highest BSA rejection of 85% with the water permeability of 0.7 L m -2  h -1  bar -1 . The results showed that the separation performance of glass hollow fiber membranes was in the ultrafiltration range, enabled the retention of solutes with molecular sizes larger than 67 kDa such as milk proteins, endotoxin pyrogen, virus, and colloidal silica.

Preparation for implementation of the mechanistic-empirical pavement design guide in Michigan : part 1 - HMA mixture characterization.

DOT National Transportation Integrated Search

2013-03-01

This is the final report of the Part 1 (HMA Mixture Characterization) of the Preparation for Implementation of the Mechanistic-Empirical Pavement Design Guide in Michigan project. The main objectives of the Part 1 were (i) to conduct a literatu...

Preparation, characterization and in vitro evaluation of solid dispersions containing docetaxel.

PubMed

Chen, Jie; Qiu, Liyan; Hu, Minxin; Jin, Yi; Han, Jieru

2008-06-01

Solid dispersions using water-soluble carriers were studied for improving the dissolution of docetaxel, a poorly soluble compound. In order to obtain the most optimized formulation, we prepared many solid dispersions with different carriers, different solvents, or at a series of drug-to-carrier ratios, and compared their dissolution. The accumulative dissolution of docetaxel from poloxamer 188 was more excellent than that from PVP(k30) and glyceryl monostearate, and the dissolution of docetaxel from solid dispersion was markedly higher than that of pure docetaxel; meanwhile the increased dissolution was partly dependent on the ratios of docetaxel and poloxamer 188. The ethanol used to prepare solid dispersion is of more significant effect on the dissolution of docetaxel than that of acetone. The docetaxel/poloxamer 188 system was characterized by differential scanning calorimetry (DSC), X-ray diffractometry (XRD), and environmental scanning electron microscope (ESEM). The results of DSC, XRD, and ESEM analyses of docetaxel/poloxamer 188 system showed that there are intermolecular interactions between docetaxel and poloxamer, and the crystallinity of docetaxel disappeared. These results show that solid dispersion is a promising approach of developing docetaxel drug formulates.

Preparation and characterization of chitosan-clay nanocomposites for the removal of Cu(II) from aqueous solution.

PubMed

Azzam, Eid M S; Eshaq, Gh; Rabie, A M; Bakr, A A; Abd-Elaal, Ali A; El Metwally, A E; Tawfik, Salah M

2016-08-01

In the present study, chitosan assembled on gold and silver nanoparticles were prepared and characterized by UV-vis, TEM, EDX and DLS techniques. The nanocomposites chitosan (Ch)/clay, chitosan (Ch)/AgNPs/clay and chitosan (Ch)/AuNPs/clay were prepared by solution mixing method and characterized by FTIR, XRD, and SEM techniques. The adsorption of copper(II) ions onto the prepared hybrid composites from an aqueous solution using batch adsorption was examined. The results showed that benefiting from the surface property of clay, the abundant amino and hydroxyl functional groups of chitosan, the adsorbent provides adequate and versatile adsorption for the Cu(II) ions under investigation. The batch adsorption experiments showed that the adsorption of the Cu(II) is considerably dependent on pH of milieu, the amount of adsorbent, and contact time. Batch adsorption studies revealed that the adsorption capacity of Cu(II) increased with increase in initial concentration and contact time with optimum pH in the range around neutral. The maximum uptake of Cu(II) ions by (Ch)/AgNPs/clay composite was found to be 181.5mg/g. The adsorption efficiency of Cu(II) ions by prepared (Ch)/AgNPs/clay and (Ch)/AuNPs/clay is bigger than that the individual chitosan (Ch)/clay composite which clarifies the role of metal nanoparticles in enhancement the adsorption characters. The study suggests that the (Ch)/AgNPs/clay hybrid composite is a promising nano-adsorbent for the removal of Cu(II) ions from aqueous solution. Copyright © 2016 Elsevier B.V. All rights reserved.

Spray Dried Chitosan Microparticles for Intravesical Delivery of Celecoxib: Preparation and Characterization.

PubMed

Lopedota, Angela; Cutrignelli, Annalisa; Laquintana, Valentino; Denora, Nunzio; Iacobazzi, Rosa Maria; Perrone, Mara; Fanizza, Elisabetta; Mastrodonato, Maria; Mentino, Donatella; Lopalco, Antonio; Depalo, Nicoletta; Franco, Massimo

2016-09-01

Chitosan microparticles containing celecoxib (CB), were developed as chemoprevention of bladder cancer. Furthermore two inclusion complexes of CB with methyl-β-cyclodextrin (C1 and C2) were prepared to improve the solubility of the drug. C1 and C2 were obtained by freeze-drying and characterized in the solid state and in solution. Microparticles loaded with CB or C1 or C2 were prepared by spray drying and fully characterized. The yield and encapsulation efficiencies of microparticles depended by both the viscosity and the presence of the inclusion complex in the feed medium nebulised. Generally, the microparticles exhibited a spherical shape with mean diameter of approximately 2 μm which was compatible with local intravesical administration using a catheter. The CB release studies from the microparticles allowed us to identify both immediate release systems (microparticles including the complexes) and prolonged release systems (microparticles including CB alone). The latter exhibited good adhesion to the bladder mucosa, as highlighted by a mucoadhesion study. Histological studies revealed a desquamation of the superficial cells when the bladder mucosa was treated with microparticles loaded with CB, while the morphology of the urothelium did not change when it was treated with microparticles loaded with the inclusion complex. A new CB intravesical formulation than can easily be administered with a catheter and is able to release the drug at the target site for several hours was realized. This new delivery system could be a good alternative to classic oral CB administration.

Preparation and characterization of fusion processed solid dispersions containing a viscous thermally labile polymeric carrier.

PubMed

Hughey, Justin R; Keen, Justin M; Miller, Dave A; Brough, Chris; McGinity, James W

2012-11-15

The primary aim of the present study was to investigate the ability of hydroxypropyl and methoxyl substituted cellulose ethers to stabilize supersaturated concentrations of itraconazole (ITZ), a poorly water-soluble weak base, after an acid-to-neutral pH transition. A secondary aim of the study was to evaluate the effect of fusion processes on polymer stability and molecular weight. Polymer screening studies showed that stabilization of ITZ supersaturation was related to the molecular weight of the polymer and levels of hydroxypropyl and methoxyl substitution. METHOCEL E50LV (E50LV), which is characterized as having a high melt viscosity, was selected for solid dispersion formulation studies. Hot-melt extrusion processing of E50LV based compositions resulted in high torque loads, low material throughput and polymer degradation. KinetiSol Dispersing, a novel fusion based processing technique, was evaluated as a method to prepare the solid dispersions with reduced levels of polymer degradation. An experimental design revealed that polymer molecular weight was sensitive to shearing forces and high temperatures. However, optimal processing conditions resulted in significantly reduced E50LV degradation relative to HME processing. The technique was effectively utilized to prepare homogenous solid solutions of E50LV and ITZ, characterized as having a single glass transition temperature over a wide range of drug loadings. All prepared compositions provided for a high degree of ITZ supersaturation stabilization. Copyright © 2012 Elsevier B.V. All rights reserved.

Preparation, characterization, physical properties, and photoconducting behaviour of anthracene derivative nanowires

NASA Astrophysics Data System (ADS)

Xiao, Jinchong; Yin, Zongyou; Yang, Bo; Liu, Yi; Ji, Li; Guo, Jun; Huang, Ling; Liu, Xuewei; Yan, Qingyu; Zhang, Hua; Zhang, Qichun

2011-11-01

Organic nanowires of 9,10-dibromoanthracene (DBA) and 9,10-dicyanoanthracene (DCNA) were obtained by adding the THF solution of DBA/DCNA into water containing P123 surfactants. The as-prepared nanowires were characterized by UV-vis, fluorescence spectra, Field Emission Scanning Electron Microscopy (FESEM), and Transmission Electron Microscopy (TEM). We found that DBA and DCNA nanowires emitted green light rather than blue light for molecules in THF solution. The red-shift UV and fluorescent spectra of DBA and DCNA nanowires implied that these nanowires were formed through J-aggregation. The photoconducting study of DBA/DCNA nanowire-based network on rGO/SiO2/Si shows different photocurrent behaviors upon irradiation, which displayed that electron transfer from DCNA nanowire to rGO was stronger than that of DBA nanowires to rGO.Organic nanowires of 9,10-dibromoanthracene (DBA) and 9,10-dicyanoanthracene (DCNA) were obtained by adding the THF solution of DBA/DCNA into water containing P123 surfactants. The as-prepared nanowires were characterized by UV-vis, fluorescence spectra, Field Emission Scanning Electron Microscopy (FESEM), and Transmission Electron Microscopy (TEM). We found that DBA and DCNA nanowires emitted green light rather than blue light for molecules in THF solution. The red-shift UV and fluorescent spectra of DBA and DCNA nanowires implied that these nanowires were formed through J-aggregation. The photoconducting study of DBA/DCNA nanowire-based network on rGO/SiO2/Si shows different photocurrent behaviors upon irradiation, which displayed that electron transfer from DCNA nanowire to rGO was stronger than that of DBA nanowires to rGO. Electronic supplementary information (ESI) available: XRD patterns and simulations, and FT-IR spectra. CCDC reference numbers 840471. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c1nr10655d

Spindly cobalt ferrite nanocrystals: preparation, characterization and magnetic properties.

PubMed

Cao, Xuebo; Gu, Li

2005-02-01

In this paper we describe the preparation of homogeneously needle-shaped cobalt ferrite (CoFe(2)O(4)) nanocrystals on a large scale through the smooth decomposition of urea and the resulting co-precipitation of Co(2+) and Fe(3+) in oleic acid micelles. Furthermore, we found that other ferrite nanocrystals with a needle-like shape, such as zinc ferrite (ZnFe(2)O(4)) and nickel ferrite (NiFe(2)O(4)), can be prepared by the same process. Needle-shaped CoFe(2)O(4) nanocrystals dispersed in an aqueous solution containing oleic acid exhibit excellent stability and the formed colloid does not produce any precipitations after two months, which is of prime importance if these materials are applied in magnetic fluids. X-ray diffraction (XRD) measurements were used to characterize the phase and component of the co-precipitation products, and demonstrate that they are spinel ferrite with a cubic symmetry. Transmission electron microscopy (TEM) observation showed that all the nanocrystals present a needle-like shape with a 22 nm short axis and an aspect ratio of around 6. Varying the concentration of oleic acid did not bring about any obvious influence on the size distribution and shapes of CoFe(2)O(4). The magnetic properties of the needle-shaped CoFe(2)O(4) nanocrystals were evaluated by using a vibrating sample magnetometer (VSM), electron paramagnetic resonance (EPR), and a Mössbauer spectrometer, and the results all demonstrated that CoFe(2)O(4) nanocrystals were superparamagnetic at room temperature.

Preparation and characterization of citral-loaded solid lipid nanoparticles.

PubMed

Tian, Huaixiang; Lu, Zhuoyan; Li, Danfeng; Hu, Jing

2018-05-15

Citral-loaded solid lipid nanoparticles (citral-SLNs) were prepared via a high-pressure homogenization method, using glyceryl monostearate (GMS) as the solid lipid and a mixture of Tween 80 (T-80) and Span 80 (S-80) at a weight ratio of 1:1 as the surfactant. The microstructure and properties of the citral-SLNs were characterized by dynamic light scattering (DLS), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermal gravimetric analysis (TGA). The chemical stability of citral in the citral-SLNs was analyzed by solid-phase microextraction gas chromatography (SPME-GC). The GC results showed that 67.0% of the citral remained in the citral-SLN suspensions after 12 days, while only 8.22% remained in the control. Therefore, the encapsulation of citral in the solid lipid can enhance its stability in acidic surroundings. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparation and characterization of clove essential oil-loaded liposomes.

PubMed

Sebaaly, Carine; Jraij, Alia; Fessi, Hatem; Charcosset, Catherine; Greige-Gerges, Hélène

2015-07-01

In this study, suitable formulations of natural soybean phospholipid vesicles were developed to improve the stability of clove essential oil and its main component, eugenol. Using an ethanol injection method, saturated (Phospholipon 80H, Phospholipon 90H) and unsaturated soybean (Lipoid S100) phospholipids, in combination with cholesterol, were used to prepare liposomes at various eugenol and clove essential oil concentrations. Liposomal batches were characterized and compared for their size, polydispersity index, Zeta potential, loading rate, encapsulation efficiency and morphology. The liposomes were tested for their stability after storing them for 2 months at 4°C by monitoring changes in their mean size, polydispersity index and encapsulation efficiency (EE) values. It was found that liposomes exhibited nanometric oligolamellar and spherical shaped vesicles and protected eugenol from degradation induced by UV exposure; they also maintained the DPPH-scavenging activity of free eugenol. Liposomes constitute a suitable system for encapsulation of volatile unstable essential oil constituents. Copyright © 2015 Elsevier Ltd. All rights reserved.

Preparation and characterization of isoniazid-loaded crude soybean lecithin liposomes.

PubMed

Nkanga, Christian Isalomboto; Krause, Rui Werner; Noundou, Xavier Siwe; Walker, Roderick Bryan

2017-06-30

Tuberculosis (TB) is a poverty related infectious disease that is rapidly giving rise to public health concerns. Lengthy drug administration and frequent adverse side-effects associated with TB treatment make anti-tubercular drugs (ATDs) good candidates for drug delivery studies. This work aimed to formulate and prepare liposomes as a cost-effective option for ATD delivery. Liposomes were prepared by film hydration using crude soybean lecithin (CL) and not pure phospholipids as in the normal practice. Cholesterol was also used (up to 25% mass ratio), and isoniazid (INH) was encapsulated as model drug using a freeze-thaw loading technique. Purified soybean lecithin (PL) was also used for comparative purposes, under the same conditions. INH-loaded liposomes were characterized for particle size, Zeta Potential (ZP), encapsulation efficiency (EE) and drug release. Physicochemical properties were investigated using thermogravimetric analysis, differential scanning calorimetry, X-ray diffraction and Fourier transform infrared. INH-loaded CL-based liposomes showed high EE (79±2.45%). The average particle size (813.00±9.21nm) and ZP (-42.80±4.31mV) of this formulation are promising for the treatment of TB by pulmonary delivery. These findings suggest the possibility of encapsulating ATDs in liposomes made of crude soybean lecithin that is cheap and readily available. Copyright © 2017 Elsevier B.V. All rights reserved.

Surface Structure Spread Single Crystals (S4C): Preparation and characterization

NASA Astrophysics Data System (ADS)

de Alwis, A.; Holsclaw, B.; Pushkarev, V. V.; Reinicker, A.; Lawton, T. J.; Blecher, M. E.; Sykes, E. C. H.; Gellman, A. J.

2013-02-01

A set of six spherically curved Cu single crystals referred to as Surface Structure Spread Single Crystals (S4Cs) has been prepared in such a way that their exposed surfaces collectively span all possible crystallographic surface orientations that can be cleaved from the face centered cubic Cu lattice. The method for preparing these S4Cs and for finding the high symmetry pole point is described. Optical profilometry has been used to determine the true shapes of the S4Cs and show that over the majority of the surface, the shape is extremely close to that of a perfect sphere. The local orientations of the surfaces lie within ± 1° of the orientation expected on the basis of the spherical shape; their orientation is as good as that of many commercially prepared single crystals. STM imaging has been used to characterize the atomic level structure of the Cu(111) ± 11°-S4C. This has shown that the average step densities and the average step orientations match those expected based on the spherical shape. In other words, although there is some distribution of step-step spacing and step orientations, there is no evidence of large scale reconstruction or faceting. The Cu S4Cs have local structures based on the ideal termination of the face centered cubic Cu lattice in the direction of termination. The set of Cu S4Cs will serve as the basis for high throughput investigations of structure sensitive surface chemistry on Cu.

RapTOR: Automated Sequencing Library Preparation and Suppression for Rapid Pathogen Characterization (7th Annual SFAF Meeting, 2012)

ScienceCinema

Lane, Todd

2018-05-18

Todd Lane on "RapTOR: Automated sequencing library preparation and suppression for rapid pathogen characterization" at the 2012 Sequencing, Finishing, Analysis in the Future Meeting held June 5-7, 2012 in Santa Fe, New Mexico.

RapTOR: Automated Sequencing Library Preparation and Suppression for Rapid Pathogen Characterization (7th Annual SFAF Meeting, 2012)

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

Lane, Todd

2012-06-01

Todd Lane on "RapTOR: Automated sequencing library preparation and suppression for rapid pathogen characterization" at the 2012 Sequencing, Finishing, Analysis in the Future Meeting held June 5-7, 2012 in Santa Fe, New Mexico.

Preparation using pectinase and characterization of nanofibers from orange peel waste in juice factories.

PubMed

Hideno, Akihiro; Abe, Kentaro; Yano, Hiroyuki

2014-06-01

This study reports the preparation and characterization of nanofibers consisting mainly of cellulose microfibrils from orange peel (OP), which is a significant byproduct of orange juice production. Three treatments (boiling, alkaline, and pectinase) were investigated with and without subsequent grinding treatment. It was possible to prepare the cellulose nanofibers (CNFs) using these methods, except for the boiling treatment with grinding. Interestingly, only pectinase and a mild-physical blender treatment without grinding produced nanofibers. The width of the nanofibers from OP was approximately 10 to 50 nm. The microfibril bundles of OP were considered to be thinner than those of commercial CNFs. Our data indicated that the removal of pectic polysaccharides and hemicelluloses covering the cellulose microfibrils was important for the preparation of nanofibers from OP. These nanofibers from OP using pectinase are proposed to be applicable as food materials, pharmaceuticals, and filters for the tractive characteristics of the sheet. This study demonstrates: (1) it was possible to prepare the nanofibers from orange peel using pectinase and (2) the width of the nanofibers from orange peel was approximately 10 to 50 nm. (3) Removal of polysaccharides such as pectin and hemicelluloses covering cellulose microfibrils was very important for preparation of nanofibers from OP. Considering the tractive characteristics of the sheets from nanofibers and the origin of orange peel, they are suitable for application of food materials, pharmaceuticals, and filters. © 2014 Institute of Food Technologists®

Preparation and characterization of Polyacrylonitrile/ Manganese Dioxides- based Carbon Nanofibers via electrospinning process

NASA Astrophysics Data System (ADS)

Che Othman, F. E.; Yusof, N.; Jaafar, J.; Ismail, A. F.; Hasbullah, H.; Abdullah, N.; Ismail, M. S.

2016-06-01

This research reports the production of precursor polyacrylonitrile (PAN)/ manganese dioxide (MnO2) nanofibers (NFs) via electrospinning method followed by stabilization and carbonization processes. Nowadays, electrospinning has become a suitable method in manufacturing continuous NFs, thus it is employed to fabricate NFs in this study. The microstructural properties and adsorption competencies of the produced NFs were also studied. The NFs were prepared by electrospinning the polymer solution of Polyacrylonitrile (PAN) and Manganese Dioxide (MnO2) in, N, N-Dimethylformamide (DMF) solvent. The factors considered in this study were various polymer PAN/MnO2 concentrations which will significantly affect the specific surface area, fiber morphology and the diameter of the NFs prepared. Subsequently, heat treatment is applied by setting up the stabilization temperature at 275 °C and carbonization temperature at 800 °C with constant dwelling time (30 min). Nitrogen gas at constant rate 0.2 L/min was used for stabilization and carbonization with the stabilization rate (2 °C/min) and carbonization rate (5 °C/min). The carbon nanofibers (CNFs) produced were characterized using Scanning Electron Microscopy (SEM), Brunauer Emmett and Teller (BET) surface area and Fourier Transmission Infrared Spectroscopy (FTIR). It was found that the PAN/MnO2 CNFs were successfully produced with the carbonization temperature of 800 °C. The prepared PAN/MnO2 CNFs prepared showed an enhanced in specific surface area about two times compared to it precursor NFs.

Binary Alkali-Metal Silicon Clathrates by Spark Plasma Sintering: Preparation and Characterization

PubMed Central

Veremchuk, Igor; Beekman, Matt; Antonyshyn, Iryna; Schnelle, Walter; Baitinger, Michael; Nolas, George S.; Grin, Yuri

2016-01-01

The binary intermetallic clathrates K8-xSi46 (x = 0.4; 1.2), Rb6.2Si46, Rb11.5Si136 and Cs7.8Si136 were prepared from M4Si4 (M = K, Rb, Cs) precursors by spark-plasma route (SPS) and structurally characterized by Rietveld refinement of PXRD data. The clathrate-II phase Rb11.5Si136 was synthesized for the first time. Partial crystallographic site occupancy of the alkali metals, particularly for the smaller Si20 dodecahedra, was found in all compounds. SPS preparation of Na24Si136 with different SPS current polarities and tooling were performed in order to investigate the role of the electric field on clathrate formation. The electrical and thermal transport properties of K7.6Si46 and K6.8Si46 in the temperature range 4–700 K were investigated. Our findings demonstrate that SPS is a novel tool for the synthesis of intermetallic clathrate phases that are not easily accessible by conventional synthesis techniques. PMID:28773710

Preparation and characterization of gamma irradiated Starch/PVA/ZnO nanocomposite films

NASA Astrophysics Data System (ADS)

Akhavan, Azam; Khoylou, Farah; Ataeivarjovi, Ebrahim

2017-09-01

In this study starch/PVA/ZnO nanocomposite films with antibacterial activity were prepared and modified using gamma irradiation for packaging applications. ZnO nanoparticles (NPs) were synthesized from Zn(OH)2 using hydrothermal process and characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The prepared ZnO NPs were incorporated into blend films of starch and poly (vinyl alcohol) (PVA) with different concentrations from 0.1 to 1 wt% using solution casting method. The results of SEM confirmed good dispersion of ZnO NPs into the films while FTIR spectroscopy showed interactions between ZnO particles and starch/PVA blend. The nanocomposite films were irradiated at the dose range of 1-5 kGy. It was found that gamma irradiation induces a significant reduction in water absorptions of the films at the dose of 3 kGy. Different trends were observed for the tensile and elongation properties of the irradiated films. Based on the results, the bacterial growth on the films was effectively inhibited when the dosage of ZnO NPs was only 0.5 wt%.

Protocols for the analytical characterization of therapeutic monoclonal antibodies. II - Enzymatic and chemical sample preparation.

PubMed

Bobaly, Balazs; D'Atri, Valentina; Goyon, Alexandre; Colas, Olivier; Beck, Alain; Fekete, Szabolcs; Guillarme, Davy

2017-08-15

The analytical characterization of therapeutic monoclonal antibodies and related proteins usually incorporates various sample preparation methodologies. Indeed, quantitative and qualitative information can be enhanced by simplifying the sample, thanks to the removal of sources of heterogeneity (e.g. N-glycans) and/or by decreasing the molecular size of the tested protein by enzymatic or chemical fragmentation. These approaches make the sample more suitable for chromatographic and mass spectrometric analysis. Structural elucidation and quality control (QC) analysis of biopharmaceutics are usually performed at intact, subunit and peptide levels. In this paper, general sample preparation approaches used to attain peptide, subunit and glycan level analysis are overviewed. Protocols are described to perform tryptic proteolysis, IdeS and papain digestion, reduction as well as deglycosylation by PNGase F and EndoS2 enzymes. Both historical and modern sample preparation methods were compared and evaluated using rituximab and trastuzumab, two reference therapeutic mAb products approved by Food and Drug Administration (FDA) and European Medicines Agency (EMA). The described protocols may help analysts to develop sample preparation methods in the field of therapeutic protein analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and characterization of shape memory polymer scaffolds via solvent casting/particulate leaching.

PubMed

De Nardo, Luigi; Bertoldi, Serena; Cigada, Alberto; Tanzi, Maria Cristina; Haugen, Håvard Jostein; Farè, Silvia

2012-09-27

Porous Shape Memory Polymers (SMPs) are ideal candidates for the fabrication of defect fillers, able to support tissue regeneration via minimally invasive approaches. In this regard, control of pore size, shape and interconnection is required to achieve adequate nutrient transport and cell ingrowth. Here, we assessed the feasibility of the preparation of SMP porous structures and characterized their chemico-physical properties and in vitro cell response. SMP scaffolds were obtained via solvent casting/particulate leaching of gelatin microspheres, prepared via oil/water emulsion. A solution of commercial polyether-urethane (MM-4520, Mitsubishi Heavy Industries) was cast on compacted microspheres and leached-off after polymer solvent evaporation. The obtained structures were characterized in terms of morphology (SEM and micro-CT), thermo-mechanical properties (DMTA), shape recovery behavior in compression mode, and in vitro cytocompatibility (MG63 Osteoblast-like cell line). The fabrication process enabled easy control of scaffold morphology, pore size, and pore shape by varying the gelatin microsphere morphology. Homogeneous spherical and interconnected pores have been achieved together with the preservation of shape memory ability, with recovery rate up to 90%. Regardless of pore dimensions, MG63 cells were observed adhering and spreading onto the inner surface of the scaffolds obtained for up to seven days of static in vitro tests. A new class of SMP porous structures has been obtained and tested in vitro: according to these preliminary results reported, SMP scaffolds can be further exploited in the design of a new class of implantable devices.

Preparation and characterization of adefovir dipivoxil-stearic acid cocrystal with enhanced physicochemical properties.

PubMed

Seo, Jeong-Woong; Hwang, Kyu-Min; Lee, Sung-Hoon; Kim, Dong-Wook; Park, Eun-Seok

2017-06-11

The objectives of this study were to prepare cocrystal composed of adefovir dipivoxil (AD) and stearic acid (SA) and to investigate the enhanced properties of the cocrystal. The cocrystal was prepared by antisolvent precipitation and characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray powder diffraction (XRPD), and differential scanning calorimetry (DSC). The enhanced properties were evaluated by dissolution testing, permeability studies, and powder rheology analysis. The AD raw material has a cuboid-like crystal and the cocrystal has a needle shape. In the FT-IR study, there were bathochromic shifts caused by the hydrogen bonding. The melting point of the cocrystal was 52.9 °C, which was lower than that of AD. The XRPD pattern also had distinct differences, supporting the formation of a new crystalline form. The cocrystal showed changes in the lattice energy and the solvation strength, which caused an enhanced dissolution. The permeability was increased due to the SA, which acts as a P-gp inhibitor. The tabletability was enhanced due to the altered crystal habit. In conclusion, cocrystal containing AD and SA was successfully prepared, presenting advantages such as enhanced solubility, tabletability, and permeability. The use of the cocrystal is a desirable approach for the improved physicochemical properties.

Preparation and characterization of dialdehyde starch by one-step acid hydrolysis and oxidation.

PubMed

Zuo, Yingfeng; Liu, Wenjie; Xiao, Junhua; Zhao, Xing; Zhu, Ying; Wu, Yiqiang

2017-10-01

Dialdehyde starch was prepared by one-step synthesis of acid hydrolysis and oxidation, using corn starch as the raw material, sodium periodate (NaIO 4 ) as the oxidant, and hydrochloric acid (HCl) as the acid solution. The prepared dialdehyde starch was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and gel permeation chromatography (GPC). The results confirmed that oxidation occurred between the starch and NaIO 4 . The acid hydrolysis reaction reduced the molecular weight of starch and effectively improved the aldehyde group contents (92.7%). Scanning electron microscope (SEM) analysis indicated that the average particle size decreased after acid hydrolysis and oxidation reaction. X-ray diffraction (XRD) and thermal gravimetric analyzer (TGA) analysis demonstrated that the crystallinity of the obtained dialdehyde starch showed a downward trend and a decelerated thermal decomposition rate. The starch after acid hydrolysis and oxidation exhibited lower hot paste viscosity and higher reactivity. Copyright © 2017. Published by Elsevier B.V.

Preparation and characterization of erythromycin molecularly imprinted polymers based on distillation-precipitation polymerization.

PubMed

Liu, Jiang; Li, Le; Tang, Hui; Zhao, Feilang; Ye, Bang-Ce; Li, Yingchun; Yao, Jun

2015-09-01

Erythromycin-imprinted polymers with excellent recognition properties were prepared by an innovative strategy called distillation-precipitation polymerization. The interaction between erythromycin and methacrylic acid was studied by ultraviolet absorption spectroscopy, and the as-prepared materials were characterized by Fourier-transform infrared spectroscopy and scanning electron microscopy. Moreover, their binding performances were evaluated in detail by static, kinetic and selective sorption tests. It was found that the molecularly imprinted polymers afforded good morphology, monodispersity, and high adsorption capacity when the fraction of the monomers was 7 vol% in the whole reaction system, and the adsorption data for imprinted polymers correlated well with the Langmuir model. The maximum capacity of the imprinted and the non-imprinted polymers for adsorbing erythromycin is 44.03 and 19.95 mg/g, respectively. The kinetic studies revealed that the adsorption process fitted a pseudo-second-order kinetic model. Furthermore, the imprinted polymers display higher affinity toward erythromycin, compared with its analogue roxithromycin. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hemostatic gauze based on chitosan and hydroquinone: preparation, characterization and blood coagulation evaluation.

PubMed

Cassano, Roberta; Di Gioia, Maria Luisa; Mellace, Silvia; Picci, Nevio; Trombino, Sonia

2017-11-07

This work concerns on the preparation and performance evaluation of a new chitosan hydroquinone based gauze for hemostatic use. Chitosan and hydroquinone were firstly connected by etherification and then linked to the pre-carboxylate gauze. The functionalized material and the chitosan-hydroquinone ether were characterized by Fourier Transform Infrared (FT-IR) Spectroscopy and Differential Scanning Calorimetry (DSC). FT-IR results showed that an esterification occurred on carboxylic group of the gauze. The gauze functionalization degree was also evaluated by volumetric analysis. The ether hydroquinone content was obtained by the Folin test. Moreover, the linkage between hydroquinone and chitosan was confirmed by nuclear magnetic resonance (NMR). The hemostatic activity of functionalized gauze was evaluated by dynamic blood clotting assays. The obtained results showed that the prepared material can shorten the blood clotting time and induce the adhesion and activation of platelets. Finally, swelling characteristic of the new gauze was evaluated to confirm its high capacity to absorb the blood.

Preparation and Characterization of Rivastigmine Transdermal Patch Based on Chitosan Microparticles.

PubMed

Sadeghi, Mohsen; Ganji, Fariba; Taghizadeh, Seyyed Mojtaba; Daraei, Bahram

2016-01-01

Here we report a novel approach for preparation of a 6-day transdermal drug delivery system (TDDS) as treatment for mild to moderate Alzheimer's disease. The spray drying method was used to prepare microparticles containing the anti-Alzheimer drug, Rivastigmine, in combination with the natural polymer, chitosan, for transdermal drug delivery applications. The content of the drug was determined by High Performance Liquid Chromatography (HPLC) method which was validated as per FDA guidelines. The morphology and size range of the microparticles were determined; and the effect of drug concentration in the solution injected into the spray dryer on the particles characterizations was studied. The stability of Rivastigmine at high temperature was confirmed using FTIR analysis as well as a validate HPLC assay. The obtained results show that the drug was stable at high temperatures with 7 to 42% loading in the microparticles, and the higher drug concentrations of the solution injected into the spray dryer resulted in increase of the drug loading, surface drug and microparticles distortion. The TDDS containing the microparticles was also prepared with microparticle to dry adhesive ratios of 5, 10 and 15% using acrylic adhesive. Based on adhesion properties of the patches, gained from the probe tack and the peel adhesion 180° tests, and the 15% patch by having more drug content per unit area of the patch, and still having similar adhesion properties was compared to the microparticles-free patch of 5.1% Rivastigmine salt (equivalent to the drug content of the 15% patch) from the permeation point of view by using Franz cell diffusion over 6 days. The drug permeation rate from the microparticle-free patch was slower than the 15% microparticles patch, which is the result of crystallization of Rivastigmine salt in the acrylic adhesive. The 6-day-prepared TDDS can be considered as an alternative for one-week application of 6 Exelon patches.

[Preparation and characterization of nanoemulsion].

PubMed

Sun, Yu-Jing; Wu, Dao-Cheng; Cao, Yun-Xin; Sui, Yan-Fang

2005-01-01

To prepare nanoemulsion-encapsulated BSA-FITC (NEBSA-FITC), study its characteristics, and measure its uptake by dendritic cells (DCs) and peritoneal macrophages. NEBSA-FITC was prepared by a method of interfacial polymerization.The encapsulation rate, drug-carrying capacity and stability of the nanoemulsion were determined by Sephadex-G100 chromatography. The shape and size of NEBSA-FITC were observed under electron microscope. The uptake of NEBSA-FITC by DCs and macrophage cells was detected by FACS and laser confocal microscopy. The mean size of NEBSA-FITC was (25+/-10) nm. The encapsulation rate was 91%, the drug-carrying capacity was 0.091 g/L and NEBSA-FITC had a good stability. The FACS analysis showed that DCs and macrophage cells could take in more NEBSA-FITC than free BSA. The observation under laser confocal microscope found that NEBSA-FITC was located in the cytoplasm of DCs. Nanoemulsion can be efficiently taken by DCs and macrophage cells, and therefore may be promising efficient carrier of APCs-targeted antitumor vaccine.

Vaginal inserts based on chitosan and carboxymethylcellulose complexes for local delivery of chlorhexidine: preparation, characterization and antimicrobial activity.

PubMed

Bigucci, Federica; Abruzzo, Angela; Vitali, Beatrice; Saladini, Bruno; Cerchiara, Teresa; Gallucci, Maria Caterina; Luppi, Barbara

2015-01-30

The aim of this work was to prepare vaginal inserts based on chitosan/carboxymethylcellulose polyelectrolyte complexes for local delivery of chlorhexidine digluconate. Complexes were prepared with different chitosan/carboxymethylcellulose molar ratios at a pH value close to pKa interval of the polymers and were characterized in terms of physico-chemical properties, complexation yield and drug loading. Then complexes were used to prepare inserts as vaginal dosage forms and their physical handling, morphology, water-uptake ability and drug release properties as well as antimicrobial activity toward Candida albicans and Escherichia coli were evaluated. Results confirmed the ionic interaction between chitosan and carboxymethylcellulose and the influence of the charge amount on the complexation yield. Complexes were characterized by high values of drug loading and showed increasing water-uptake ability with the increase of carboxymethylcellulose amount. The selection of appropriate chitosan/carboxymethylcellulose molar ratios allowed to obtain cone-like shaped solid inserts, easy to handle and able to hydrate releasing the drug over time. Finally, the formulated inserts showed antimicrobial activity against common pathogens responsible for vaginal infections. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of chitosan-ferulic acid conjugate: Structure characterization and in the application of pharmaceuticals.

PubMed

Li, Chen; Li, Jian-Bin

2017-12-01

A novel drug delivery system based on chitosan derivatives was prepared by introducting ferulic acid to chitosan adopting a free radical-induced grafting procedure. This paper used an ascorbic acid/hydrogen peroxide redox pair as radical initiator. The chitosan derivative was characterized by Fourier transformed infrared (FTIR), Ultraviolet-visible spectrum (UV), Differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Electron microscopic scanning (SEM). What is more, preparing microcapsules with the chitosan conjugate as wall material, the drug release propertie of chitosan conjugates were compared with that of a blank chitosan, which treated in the same conditions but in the absence of ferulic acid. The study clearly demonstrates that free radical-induced grafting procedure was an effective reaction methods and chitosan-ferulic acid is a potential functionalized carrier material for drug delivery. Copyright © 2017 Elsevier B.V. All rights reserved.

Sildenafil vaginal suppositories: preparation, characterization, in vitro and in vivo evaluation.

PubMed

Shanmugam, Srinivasan; Kim, Young-Hun; Park, Jeong-Hee; Im, Ho Taek; Sohn, Young Taek; Kim, Kyeong Soo; Kim, Yong-Il; Yong, Chul Soon; Kim, Jong Oh; Choi, Han-Gon; Woo, Jong Soo

2014-06-01

The main objective was to investigate the in vitro release profile/kinetics, and in vivo plasma pharmacokinetics (PK) and organ biodistribution (BD) of the prepared sildenafil vaginal suppositories (SVS). Suppositories containing 25 mg of sildenafil were prepared by the cream melting technique using Witepsol H-15 as a suppository base. The suppositories were characterized for weight variation, content uniformity, hardness, disintegration time and crystallinity change. The in vitro dissolution in pH 4.5, and in vivo plasma PK and organ BD of sildenafil from SVS in female Sprague Dawley rats, were also investigated. The mean weight variation, content uniformity, hardness and disintegration time of the prepared SVS were 1.127 ± 0.020 g, 98.25 ± 2.50%, 2.5 ± 0.08 kg and 9 ± 1.0 min, respectively. The release of sildenafil from the SVS was more than 90% at 30 min, with a release kinetic of Hixson--Crowell model and non-Fickian diffusion (n = 0.464). The plasma PK study demonstrated a significantly lower Cmax (∼10 times) and AUC0-24 h (∼13 times) of sildenafil in plasma following intravaginal (IVG) administration of suppositories compared to oral (PO) administration of sildenafil solution. Nevertheless, the organ BD study showed a phenomenally higher Cmax (∼40 times) and AUC0-24 h (∼20 times) of sildenafil in uterus following IVG administration of suppositories than PO administration of sildenafil solution. This study demonstrated enhanced sildenafil exposure in the uterus following IVG administration of SVS, which could be used to target the uterus for therapeutic benefits.

Preparation and characterization of mono-sheet bipolar membranes by pre-irradiation grafting method for fuel cell applications

NASA Astrophysics Data System (ADS)

Guan, Yingjie; Fang, Jun; Fu, Tao; Zhou, Huili; Wang, Xin; Deng, Zixiang; Zhao, Jinbao

2016-09-01

A new method for the preparation of the mono-sheet bipolar membrane applied to fuel cells was developed based on the pre-irradiation grafting technology. A series of bipolar membranes were successfully prepared by simultaneously grafting of styrene onto one side of the poly(ethylene-co-tetrafluoroethylene) base film and 1-vinylimidazole onto the opposite side, followed by the sulfonation and alkylation, respectively. The chemical structures and microstructures of the prepared membranes were investigated by ATR-FTIR and SEM-EDS. The TGA measurements demonstrated the prepared bipolar membranes have reasonable thermal stability. The ion exchange capacity, water uptake and ionic conductivity of the membranes were also characterized. The H2/O2 single fuel cells using these membranes were evaluated and revealed a maximum power density of 107 mW cm-2 at 35 °C with unhumidified hydrogen and oxygen. The preliminary performances suggested the great prospect of these membranes in application of bipolar membrane fuel cells.

Preparation and characterization of fluorophenylboronic acid-functionalized affinity monolithic columns for the selective enrichment of cis-diol-containing biomolecules.

PubMed

Li, Qianjin; Liu, Zhen

2015-01-01

Boronate affinity monolithic columns have been developed into an important means for the selective recognition and capture of cis-diol-containing biomolecules, such as glycoproteins, nucleosides and saccharides. The ligands of boronic acids are playing an important role in boronate affinity monolithic columns. Although several boronate affinity monoliths with high affinity toward cis-diol-containing biomolecules have been reported, only few publications are focused on their detailed procedures for preparation and characterization. This chapter describes in detail the preparation and characterization of a boronate affinity monolithic column applying 2,4-difluoro-3-formyl-phenylboronic acid (DFFPBA) as a ligand. The DFFPBA-functionalized monolithic column not only exhibited an ultrahigh boronate affinity toward cis-diol-containing biomolecules, but also showed great potential for the selective enrichment of cis-diol-containing biomolecules in real samples.

Preparation and Characterization of Guar-Montmorillonite Nanocomposites

PubMed Central

Mansa, Rola; Detellier, Christian

2013-01-01

Polymer-clay nanocomposites are highly sought-after materials, mainly due to their applicability in a variety of avenues. From the standpoint of the preparation of these nanocomposites, however, organic compatibility with clay and adherence to “green chemistry” concepts and principles can be limiting factors. As such, the objective was to prepare a biopolymer-modified clay nanocomposite using a simple and environmentally friendly method of preparation, whereby pre-treatment of the clay for organic compatibility was bypassed. Novel montmorillonite nanocomposites were prepared using neutral guar gum and cationic guar gum. X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the formation of intercalated structures. A monolayer configuration of cationic guar within the interlayer space was indicated by XRD results, while treatment with neutral guar gum resulted in the observance of both monolayer and bilayer configurations. Additionally, TEM results indicated partial exfoliation. Results attributed from 13C cross polarization/magic angle spinning nuclear magnetic resonance spectroscopy (CP/MAS NMR) of the nanocomposites indicated peaks corresponding to the guar constituent, confirming the adsorption of the biopolymer. Inductively coupled plasma emission spectrometry (ICP-ES) results indicated the exchange of cations present in neutral guar gum with the sodium cations of montmorillonite, in the case of the neutral guar nanocomposites. PMID:28788384

Preparation and Characterization of Activated Carbon from Palm Kernel Shell

NASA Astrophysics Data System (ADS)

Andas, J.; Rahman, M. L. A.; Yahya, M. S. M.

2017-08-01

In this study, a high quality of activated carbon (AC) was successfully synthesized from palm kernel shell (PKS) via single step KOH activation. Several optimal conditions such as impregnation ratio and activation temperature were investigated. The prepared activated carbon under the optimum condition of impregnation ratio (1:1.5 raw/KOH) and activation temperature (800 °C) was characterized using Na2S2O3 volumetric method, CHNS/O analysis and Scanning Electron Microscope (SEM). Na2S2O3 volumetric showed an iodine number of 994.83 mgg-1 with yield % of 8.931 %. CHNS/O analysis verified an increase in C content for KOH-AC (61.10 %) in comparison to the raw PKS (47.28 %). Well-formation of porous structure was evidenced through SEM for KOH-AC. From this study, it showed a successful conversion of agricultural waste into value added porous material under benign condition.

Structural characterization of pharmaceutical heparins prepared from different animal tissues.

PubMed

Fu, Li; Li, Guoyun; Yang, Bo; Onishi, Akihiro; Li, Lingyun; Sun, Peilong; Zhang, Fuming; Linhardt, Robert J

2013-05-01

Although most pharmaceutical heparin used today is obtained from porcine intestine, heparin has historically been prepared from bovine lung and ovine intestine. There is some regulatory concern about establishing the species origin of heparin. This concern began with the outbreak of mad cow disease in the 1990s and was exacerbated during the heparin shortage in the 2000s and the heparin contamination crisis of 2007-2008. Three heparins from porcine, ovine, and bovine were characterized through state-of-the-art carbohydrate analysis methods with a view profiling their physicochemical properties. Differences in molecular weight, monosaccharide and disaccharide composition, oligosaccharide sequence, and antithrombin III-binding affinity were observed. These data provide some insight into the variability of heparins obtained from these three species and suggest some analytical approaches that may be useful in confirming the species origin of a heparin active pharmaceutical ingredient. Copyright © 2013 Wiley Periodicals, Inc.

Preparation and Characterization of Cyclotrimethylenetrinitramine (RDX) with Reduced Sensitivity

PubMed Central

Wang, Yuqiao; Li, Xin; Chen, Shusen; Ma, Xiao; Yu, Ziyang; Jin, Shaohua; Li, Lijie; Chen, Yu

2017-01-01

The internal defects and shape of cyclotrimethylenetrinitramine (RDX) crystal are critical parameters for the preparation of reduced sensitivity RDX (RS-RDX). In the current study, RDX was re-crystallized and spheroidized to form the high-quality RDX that was further characterized by purity, apparent density, size distribution, specific surface area, impact sensitivity, and shock sensitivity. The effects of re-crystallization solvent on the growth morphology of RDX crystal were investigated by both theoretical simulation and experiment test, and consistent results were obtained. The high-quality RDX exhibited a high purity (≥99.90%), high apparent density (≥1.811 g/cm3), spherical shape, and relatively low impact sensitivity (6%). Its specific surface area was reduced more than 30%. Compared with conventional RDXs, the high-quality RDX reduced the shock sensitivities of PBXN-109 and PBXW-115 by more than 30%, indicating that it was a RS-RDX. The reduced sensitivity and good processability of the high-quality RDX would be significant in improving the performances of RDX-based PBXs. PMID:28825661

Preparation and characterization of bio-diesels from various bio-oils.

PubMed

Lang, X; Dalai, A K; Bakhshi, N N; Reaney, M J; Hertz, P B

2001-10-01

Methyl, ethyl, 2-propyl and butyl esters were prepared from canola and linseed oils through transesterification using KOH and/ or sodium alkoxides as catalysts. In addition, methyl and ethyl esters were prepared from rapeseed and sunflower oils using the same catalysts. Chemical composition of the esters was determined by HPLC for the class of lipids and by GC for fatty acid compositions. The bio-diesel esters were characterized for their physical and fuel properties including density, viscosity, iodine value, acid value, cloud point, pure point, gross heat of combustion and volatility. Methyl and ethyl esters prepared from a particular vegetable oil had similar viscosities, cloud points and pour points, whereas methyl, ethyl, 2-propyl and butyl esters derived from a particular vegetable oil had similar gross heating values. However, their densities, which were 2 7% higher than those of diesel fuels, statistically decreased in the order of methyl approximately 2-propyl > ethyl > butyl esters. Butyl esters showed reduced cloud points (-6 degrees C to -10 degrees C) and pour points (-13 degrees C to -16 degrees C) similar to those of summer diesel fuel having cloud and pour points of -8 degrees C and -15 degrees C, respectively. The viscosities of bio-diesels (3.3-7.6 x 10(-4) Pa s at 40 degrees C) were much less than those of pure oils (22.4-45.1 x 10(-4) Pa s at 40 degrees C) and were twice those of summer and winter diesel fuels (3.50 and 1.72 x 10(-4) Pa s at 40 degrees C), and their gross heat contents of approximately 40 MJ/kg were 11% less than those of diesel fuels (approximately 45 MJ/kg). For different esters from the same vegetable oil, methyl esters were the most volatile, and the volatility decreased as the alkyl group grew bulkier. However, the bio-diesels were considerably less volatile than the conventional diesel fuels.

Preparation and electrochemical characterization of polyaniline/activated carbon composites as an electrode material for supercapacitors.

PubMed

Oh, Misoon; Kim, Seok

2012-01-01

Polyaniline (PANI)/activated carbon (AC) composites were prepared by a chemical oxidation polymerization. To find an optimum ratio between PANI and AC which shows superior electrochemical properties, the preparation was carried out in changing the amount of added aniline monomers. The morphology of prepared composites was investigated by scanning electron microscopy (SEM) and transmission electron microscope (TEM). The structural and thermal properties were investigated by Fourier transform infrared spectra (FT-IR) and thermal gravimetric analysis (TGA), respectively. The electrochemical properties were characterized by cyclic voltammetry (CV). Composites showed a summation of capacitances that consisted of two origins. One is double-layer capacitance by ACs and the other is faradic capacitance by redox reaction of PANI. Fiber-like PANIs are coated on the surface of ACs and they contribute to the large surface for redox reaction. The vacancy among fibers provided the better diffusion and accessibility of ion. High capacitances of composites were originated from the network structure having vacancy made by PANI fibers. It was found that the composite prepared with 5 ml of aniline monomer and 0.25 g of AC showed the highest capacitance. Capacitance of 771 F/g was obtained at a scan rate of 5 mV/s.

Preparation, Characterization, and UV Irradiation of Mars Soil Analogues Under Simulated Martian Conditions to Support Detection of Molecular Biomarkers

NASA Astrophysics Data System (ADS)

Fornaro, T.; Brucato, J. R.; ten Kate, I. L.; Siljeström, S.; Steele, A.; Cody, G. D.; Hazen, R. M.

2018-04-01

We present laboratory activities of preparation, characterization, and UV irradiation processing of Mars soil analogues, which are key to support both in situ exploration and sample return missions devoted to detection of molecular biomarkers on Mars.

Preparation, Characterization, and Enhanced Thermal and Mechanical Properties of Epoxy-Titania Composites

PubMed Central

Rubab, Zakya; Siddiqi, Humaira M.; Saeed, Shaukat

2014-01-01

This paper presents the synthesis and thermal and mechanical properties of epoxy-titania composites. First, submicron titania particles are prepared via surfactant-free sol-gel method using TiCl4 as precursor. These particles are subsequently used as inorganic fillers (or reinforcement) for thermally cured epoxy polymers. Epoxy-titania composites are prepared via mechanical mixing of titania particles with liquid epoxy resin and subsequently curing the mixture with an aliphatic diamine. The amount of titania particles integrated into epoxy matrix is varied between 2.5 and 10.0 wt.% to investigate the effect of sub-micron titania particles on thermal and mechanical properties of epoxy-titania composites. These composites are characterized by X-ray photoelectron (XPS) spectroscopy, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermogravimetric (TG), and mechanical analyses. It is found that sub-micron titania particles significantly enhance the glass transition temperature (>6.7%), thermal oxidative stability (>12.0%), tensile strength (>21.8%), and Young's modulus (>16.8%) of epoxy polymers. Epoxy-titania composites with 5.0 wt.% sub-micron titania particles perform best at elevated temperatures as well as under high stress. PMID:24578638

Preparation and Characterization of Ato Nanoparticles by Coprecipitation with Modified Drying Method

NASA Astrophysics Data System (ADS)

Liu, Shimin; Liang, Dongdong; Liu, Jindong; Jiang, Weiwei; Liu, Chaoqian; Ding, Wanyu; Wang, Hualin; Wang, Nan

Antimony-doped tin oxide (ATO) nanoparticles were prepared by coprecipitation by packing drying and traditional direct drying (for comparison) methods. The as-prepared ATO nanoparticles were characterized by TG, XRD, EDS, TEM, HRTEM, BET, bulk density and electrical resistivity measurements. Results indicated that the ATO nanoparticles obtained by coprecipitation with direct drying method featured hard-agglomerated morphology, high bulk density, low surface area and low electrical resistivity, probably due to the direct liquid evaporation during drying, the fast shrinkage of the precipitate, the poor removal efficiency of liquid molecules and the hard agglomerate formation after calcination. Very differently, the ATO product obtained by the packing and drying method featured free-agglomerated morphology, low bulk density, high surface area and high electrical resistivity ascribed probably to the formed vapor cyclone environment and liquid evaporation-resistance, avoiding fast liquid removal and improving the removal efficiency of liquid molecules. The intrinsic formation mechanism of ATO nanoparticles from different drying methods was illustrated based on the dehydration process of ATO precipitates. Additionally, the packing and drying time played key roles in determining the bulk density, morphology and electrical conductivity of ATO nanoparticles.

The Preparation and Characterization of INTEC HAW Phase I Composition Variation Study Glasses

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

Musick, C. A.; Peeler, D. K.; Piepel, G. F.

1999-03-01

A glass composition variation study (CVS) is in progress to define formulations for the vitrification of high activity waste (HAW) proposed to be separated from dissolved calcine stored at the Idaho National Engineering and Environmental Laboratory (INEEL). Estimates of calcine and HAW compositions prepared in FY97 were used to define test matrix glasses. The HAW composition is of particular interest because high aluminum, zirconium, phosphorous and potassium, and low iron and sodium content places it outside the realm of vitrification experience in the Department of Energy (DOE) complex. Through application of statistical techniques, a test matrix was defined for Phasemore » 1 of the CVS. From this matrix, formulations were systematically selected for preparation and characterization with respect to homogeneity, viscosity, liquidus temperature (TL), and leaching response when subjected to the Product Consistency Test (PCT). Based on the properties determined, certain formulations appear suitable for further development including use in planning Phase 2 of the study. It is recommended that glasses to be investigated in Phase 2 be limited to 3-5 wt % phosphate. The results of characterizing the Phase 1 glasses are presented in this document. A full analysis of the composition-property relationships of glasses being developed for immobilizing HAWs will be performing at the completion of CVS phases. This analysis will be needed for the optimization of the glass formulations of vitrifying HAW. Contributions were made to this document by personnel working at the INEEL, Pacific Northwest National Laboratories (PNNL), and the Savannah River Technology Center (SRTC).« less

Preparation, characterization and relative bioavailability of oral elemene o/w microemulsion.

PubMed

Zeng, Zhaowu; Zhou, Guanglin; Wang, Xiaoli; Huang, Eric Zhijian; Zhan, Xiaori; Liu, Jun; Wang, Shuling; Wang, Anming; Li, Haifeng; Pei, Xiaolin; Xie, Tian

2010-09-07

The objective was to develop an elemene oil/water (o/w) microemulsion and evaluate its characteristics and oral relative bioavailability in rats. Elemene was used as the oil phase and drug, polysorbate 80 as a surfactant along with ethanol, propylene glycol, and glycerol as the cosurfactants. The microemulsion was prepared by mixing method, or ultrasonication method in an ultrasonic bath. Its three-dimensional response surface diagram was drawn by Mathcad software. The microemulsion was characterized by visual observation, cross-polarized microscopy, size, zeta potential, acidity, viscosity, and surface tension measurement. The drug content and entrapment efficiency were determined by ultra fast liquid chromatography (UFLC) and liquid surface method. Blood was drawn from rats at different time points after oral administration of an elemene microemulsion or a commercial elemene emulsion for measurement of the drug in plasma by UFLC to establish the pharmacokinetic parameters and relative bioavailability. The elemene microemulsion as a clarified and isotropic system containing 1% elemene (w/v), 5% ethanol (v/v), 15% propylene glycol (v/v), 15% glycerol (v/v), and 5% polysorbate 80 (w/v), was characterized as (57.7 ± 2.8) nm in size, 0.485 ± 0.032 in polydispersity index, (3.2 ± 0.4) mv in zeta potential, (5.19 ± 0.08) in pH, 6 mpa·s in viscosity, (31.8 ± 0.3) mN·m(-1) in surface tension, (8.273 ± 0.018) mg·mL(-1) in content of β-elemene, and (99.81 ± 0.24)% in average entrapment efficiency. The area under the concentration-time curves from 0 h to 24 h (AUC(0→24h)) of the elemene microemulsion and commercial elemene emulsion were integrated to be 3.092 mg·h·L(-1) and 1.896 mg·h·L(-1) respectively, yielding a relative bioavailability of 163.1%. The present study demonstrates the elemene microemulsion as a new formulation with ease of preparation, high entrapment efficiency, excellent clarity, good stability, and improved bioavailability.

Preparation, characterization and relative bioavailability of oral elemene o/w microemulsion

PubMed Central

Zeng, Zhaowu; Zhou, Guanglin; Wang, Xiaoli; Huang, Eric Zhijian; Zhan, Xiaori; Liu, Jun; Wang, Shuling; Wang, Anming; Li, Haifeng; Pei, Xiaolin; Xie, Tian

2010-01-01

The objective was to develop an elemene oil/water (o/w) microemulsion and evaluate its characteristics and oral relative bioavailability in rats. Elemene was used as the oil phase and drug, polysorbate 80 as a surfactant along with ethanol, propylene glycol, and glycerol as the cosurfactants. The microemulsion was prepared by mixing method, or ultrasonication method in an ultrasonic bath. Its three-dimensional response surface diagram was drawn by Mathcad software. The microemulsion was characterized by visual observation, cross-polarized microscopy, size, zeta potential, acidity, viscosity, and surface tension measurement. The drug content and entrapment efficiency were determined by ultra fast liquid chromatography (UFLC) and liquid surface method. Blood was drawn from rats at different time points after oral administration of an elemene microemulsion or a commercial elemene emulsion for measurement of the drug in plasma by UFLC to establish the pharmacokinetic parameters and relative bioavailability. The elemene microemulsion as a clarified and isotropic system containing 1% elemene (w/v), 5% ethanol (v/v), 15% propylene glycol (v/v), 15% glycerol (v/v), and 5% polysorbate 80 (w/v), was characterized as (57.7 ± 2.8) nm in size, 0.485 ± 0.032 in polydispersity index, (3.2 ± 0.4) mv in zeta potential, (5.19 ± 0.08) in pH, 6 mpa·s in viscosity, (31.8 ± 0.3) mN·m−1 in surface tension, (8.273 ± 0.018) mg·mL−1 in content of β-elemene, and (99.81 ± 0.24)% in average entrapment efficiency. The area under the concentration-time curves from 0 h to 24 h (AUC0→24h) of the elemene microemulsion and commercial elemene emulsion were integrated to be 3.092 mg·h·L−1 and 1.896 mg·h·L−1 respectively, yielding a relative bioavailability of 163.1%. The present study demonstrates the elemene microemulsion as a new formulation with ease of preparation, high entrapment efficiency, excellent clarity, good stability, and improved bioavailability. PMID:20856831

Ultrastructural characterization of tooth-biomaterial interfaces prepared with broad and focused ion beams.

PubMed

Coutinho, E; Jarmar, T; Svahn, F; Neves, A A; Verlinden, B; Van Meerbeek, B; Engqvist, H

2009-11-01

Current available techniques for transmission electron microscopy (TEM) of tooth-biomaterial interfaces are mostly ineffective for brittle phases and impair integrated chemical and morphological characterization. The aims of this study were (1) to determine the applicability of new focused ion beam (FIB) and broad ion beam (BIB) techniques for TEM preparation of tooth-biomaterial interfaces; (2) to characterize the interfacial interaction with enamel and dentin of a conventional glass-ionomer (Chemfil Superior, DeTrey Dentsply, Germany), a 2-step self-etch (Clearfil SE, Kuraray, Japan) and a 3-step etch-and-rinse (OptiBond FL, Kerr, USA) adhesives; and (3) to characterize clinically relevant interfaces obtained from actual Class-I cavities. After bonding to freshly extracted human third molars, non-demineralized and non-stained sections were obtained using the FIB/BIB techniques and examined under TEM. The main structures generally disclosed in conventional ultramicrotomy samples were recognized in FIB/BIB-based ones. There were not any major differences between FIB and BIB concerning the resulting ultrastructural morphology. FIB/BIB-sections enabled to clearly resolve sub-micron hydroxyapatite crystals on top of hard tissues and the interface between matrix and filler in all materials, even at nano-scale. Some investigated interfaces disclosed areas with a distinct "fog" or "melted look", which is probably an artifact due to surface damage caused by the high-energy beam. Interfaces with enamel clearly disclosed the distinct "keyhole" shape of enamel rods sectioned at 90 degrees , delimited by a thin electron-lucent layer of inter-rod enamel. At regions where enamel crystals ran parallel with the interface, we observed a lack of interaction and some de-bonding along with interfacial void formation. The FIB/BIB methods are viable and reliable alternatives to conventional ultramicrotomy for preparation of thin sections of brittle and thus difficult to cut biomaterial

Morphology controlled graphene-alloy nanoparticle hybrids with tunable carbon monoxide conversion to carbon dioxide.

PubMed

Devi, M Manolata; Dolai, N; Sreehala, S; Jaques, Y M; Mishra, R S Kumar; Galvao, Douglas S; Tiwary, C S; Sharma, Sudhanshu; Biswas, Krishanu

2018-05-10

Selective oxidation of CO to CO2 using metallic or alloy nanoparticles as catalysts can solve two major problems of energy requirements and environmental pollution. Achieving 100% conversion efficiency at a lower temperature is a very important goal. This requires sustained efforts to design and develop novel supported catalysts containing alloy nanoparticles. In this regard, the decoration of nanoalloys with graphene, as a support for the catalyst, can provide a novel structure due to the synergic effect of the nanoalloys and graphene. Here, we demonstrate the effect of nano-PdPt (Palladium-Platinum) alloys having different morphologies on the catalytic efficiency for the selective oxidation of CO. Efforts were made to prepare different morphologies of PdPt alloy nanoparticles with the advantage of tuning the capping agent (PVP - polyvinyl pyrollidone) and decorating them on graphene sheets via the wet-chemical route. The catalytic activity of the G-PdPt hybrids with an urchin-like morphology has been found to be superior (higher % conversion at 135 °C lower) to that with a nanoflower morphology. The above experimental observations are further supported by molecular dynamics (MD) simulations.

Preparation and characterization of cobalt-substituted anthrax lethal factor

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

Saebel, Crystal E.; Carbone, Ryan; Dabous, John R.

2011-12-09

Highlights: Black-Right-Pointing-Pointer Cobalt-substituted anthrax lethal factor (CoLF) is highly active. Black-Right-Pointing-Pointer CoLF can be prepared by bio-assimilation and direct exchange. Black-Right-Pointing-Pointer Lethal factor binds cobalt tightly. Black-Right-Pointing-Pointer The electronic spectrum of CoLF reveals penta-coordination. Black-Right-Pointing-Pointer Interaction of CoLF with thioglycolic acid follows a 2-step mechanism. -- Abstract: Anthrax lethal factor (LF) is a zinc-dependent endopeptidase involved in the cleavage of mitogen-activated protein kinase kinases near their N-termini. The current report concerns the preparation of cobalt-substituted LF (CoLF) and its characterization by electronic spectroscopy. Two strategies to produce CoLF were explored, including (i) a bio-assimilation approach involving the cultivation of LF-expressingmore » Bacillus megaterium cells in the presence of CoCl{sub 2}, and (ii) direct exchange by treatment of zinc-LF with CoCl{sub 2}. Independent of the method employed, the protein was found to contain one Co{sup 2+} per LF molecule, and was shown to be twice as active as its native zinc counterpart. The electronic spectrum of CoLF suggests the Co{sup 2+} ion to be five-coordinate, an observation similar to that reported for other Co{sup 2+}-substituted gluzincins, but distinct from that documented for the crystal structure of native LF. Furthermore, spectroscopic studies following the exposure of CoLF to thioglycolic acid (TGA) revealed a sequential mechanism of metal removal from LF, which likely involves the formation of an enzyme: Co{sup 2+}:TGA ternary complex prior to demetallation of the active site. CoLF reported herein constitutes the first spectroscopic probe of LF's active site, which may be utilized in future studies to gain further insight into the enzyme's mechanism and inhibitor interactions.« less

Preparation and Characterization of Mesoporous Zirconia Made by Using a Poly (methyl methacrylate) Template

NASA Astrophysics Data System (ADS)

Duan, Guorong; Zhang, Chunxiang; Li, Aimei; Yang, Xujie; Lu, Lude; Wang, Xin

2008-03-01

Superfine powders of poly (methyl methacrylate) (PMMA) have been prepared by means of an emulsion polymerization method. These have been used as templates in the synthesis of tetragonal phase mesoporous zirconia by the sol gel method, using zirconium oxychloride and oxalic acid as raw materials. The products have been characterized by infrared spectroscopy, X-ray diffraction analysis, transmission electron microscopy, N2 adsorption-desorption isotherms, and pore size distribution. The results indicate that the average pore size was found to be 3.7 nm.

Preparation and characterization of zinc sulphide nanocomposites based on acrylonitrile butadiene rubber

NASA Astrophysics Data System (ADS)

Ramesan, M. T.; Nihmath, A.; Francis, Joseph

2013-06-01

Rubber composite based on acrylonitrile butadiene rubber (NBR) reinforced with nano zinc sulphide (ZnS) have been prepared via vulcanization process and characterized by several techniques. Processing characteristics such as scorch time, optimum cure time decreases with increase in concentration of nano filler in acrylonitrile butadiene rubber. Mechanical properties such as tensile and tear strength increases with increase in concentration of nano filler up to 7 phr of loading thereafter the value decreases, whereas hardness, and flame resistance increases with the dosage of fillers. These enhanced properties are due to the homogenous dispersion of nano fillers in NBR matrix, which is evidenced from the structure that evaluated using X-ray diffraction (XRD) and scanning electron microscopy (SEM).

Preparation, characterization, and potential application of chitosan, chitosan derivatives, and chitosan metal nanoparticles in pharmaceutical drug delivery

PubMed Central

Ahmed, Tarek A; Aljaeid, Bader M

2016-01-01

Naturally occurring polymers, particularly of the polysaccharide type, have been used pharmaceutically for the delivery of a wide variety of therapeutic agents. Chitosan, the second abundant naturally occurring polysaccharide next to cellulose, is a biocompatible and biodegradable mucoadhesive polymer that has been extensively used in the preparation of micro-as well as nanoparticles. The prepared particles have been exploited as a potential carrier for different therapeutic agents such as peptides, proteins, vaccines, DNA, and drugs for parenteral and nonparenteral administration. Therapeutic agent-loaded chitosan micro- or nanoparticles were found to be more stable, permeable, and bioactive. In this review, we are highlighting the different methods of preparation and characterization of chitosan micro- and nanoparticles, while reviewing the pharmaceutical applications of these particles in drug delivery. Moreover, the roles of chitosan derivatives and chitosan metal nanoparticles in drug delivery have been illustrated. PMID:26869768

Tungstocobaltate-pillared layered double hydroxides: Preparation, characterization, magnetic and catalytic properties

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

Wei Xiaocui; Baicheng College of Higher Medicine, Baicheng 137000; Fu Youzhi

2008-06-15

A new polyoxometalate anion-pillared layered double hydroxide (LDH) was prepared by aqueous ion exchange of a Mg-Al LDH precursor in nitrate form with the tungstocobaltate anions [CoW{sub 12}O{sub 40}]{sup 5-}. The physicochemical properties of the product were characterized by the methods of powder X-ray diffraction, elemental analysis, infrared spectroscopy, thermogravimetric analysis and cyclic voltammetry. It was confirmed that [CoW{sub 12}O{sub 40}]{sup 5-} was intercalated between the brucite-type layers of the LDHs without a change in the structure. Magnetic measurement shows the occurrence of antiferromagnetic interactions between the magnetic centers. The investigation of catalytic performance for this sample exhibits high activitymore » for the oxidation of benzaldehyde by hydrogen peroxide. - Graphical abstract: A tungstocobaltate anion [CoW{sub 12}O{sub 40}]{sup 5-} pillared layered double hydroxide (LDH) was prepared by aqueous ion exchange with a Mg-Al LDH precursor in nitrate form, demonstrating that [CoW{sub 12}O{sub 40}]{sup 5-} was intercalated between the brucite-type layers of the LDHs without change in structure. Magnetic measurement shows the occurrence of antiferromagnetic interactions between the magnetic centers. The investigation of catalytic performance for this sample exhibits high activity for the oxidation of benzaldehyde by hydrogen peroxide.« less

Human primary mixed brain cultures: preparation, differentiation, characterization and application to neuroscience research.

PubMed

Ray, Balmiki; Chopra, Nipun; Long, Justin M; Lahiri, Debomoy K

2014-09-16

Culturing primary cortical neurons is an essential neuroscience technique. However, most cultures are derived from rodent brains and standard protocols for human brain cultures are sparse. Herein, we describe preparation, maintenance and major characteristics of a primary human mixed brain culture, including neurons, obtained from legally aborted fetal brain tissue. This approach employs standard materials and techniques used in the preparation of rodent neuron cultures, with critical modifications. This culture has distinct differences from rodent cultures. Specifically, a significant numbers of cells in the human culture are derived from progenitor cells, and the yield and survival of the cells grossly depend on the presence of bFGF. In the presence of bFGF, this culture can be maintained for an extended period. Abundant productions of amyloid-β, tau and proteins make this a powerful model for Alzheimer's research. The culture also produces glia and different sub-types of neurons. We provide a well-characterized methodology for human mixed brain cultures useful to test therapeutic agents under various conditions, and to carry forward mechanistic and translational studies for several brain disorders.

Preparation and characterization of collagen/hydroxypropyl methylcellulose (HPMC) blend film.

PubMed

Ding, Cuicui; Zhang, Min; Li, Guoying

2015-03-30

This study aimed to prepare and characterize the collagen/HPMC blend film (1/1). Thermogravimetric analysis and differential scanning calorimetry were used to investigate the thermal properties of the film. Both thermal decomposition temperature and denaturation temperature of the blend film were higher than those of the collagen film due to the intermolecular hydrogen bonding interaction between collagen and HPMC, which was demonstrated by Fourier transform infrared spectroscopy. Additionally, the morphologies, mechanical properties and hydrophilicity of films were examined. The blend film exhibited a more homogeneous and compact structure compared with that of the collagen film, as observed from scanning electron microscopy and atomic force microscopy. The tensile strength, ultimate elongation and hydrophilicity of the blend film were superior to those of the pure collagen film. Furthermore, the introduction of polyethylene glycol 1500 had almost no influence on the thermal properties of the blend film but obviously improved its stretch-ability and smoothness. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparation, characterization and catalytic application of CoFe2O4 nanoparticles in the synthesis of benzimidazoles

NASA Astrophysics Data System (ADS)

Borade, Ravikumar M.; Shinde, Pavan R.; Kale, Swati B.; Pawar, Rajendra P.

2018-05-01

A highly efficient magnetically recoverable cobalt ferrite nano-catalyst was prepared by sol-gel autocombustion method using glycine as green fuel. The prepared material has been characterized by X-ray powder diffraction and scanning. An investigation of its catalytic activity showed it to be a heterogeneous Lewis acid catalyst for the synthesis of substituted benzimidazoles. The aqueous ethanol used as green solvent for the reaction. The nm size range of these particles facilitates the catalysis process, as an increased surface area available for the reaction. The easy separation of the catalyst by an external magnet and their recovery and reuse in next cycle reaction are additional benefits.

Preparation, characterization and in vivo evaluation of formulation of repaglinide with hydroxypropyl-β-cyclodextrin.

PubMed

Liu, Meina; Cao, Wen; Sun, Yinghua; He, Zhonggui

2014-12-30

The therapeutic efficacy of repaglinide (RPG) is limited by the low and variable oral bioavailability owing to its limited aqueous solubility. In our present study, the development and evaluation of inclusion complex applying hydroxypropyl-β-cyclodextrin (HP-β-CD) for the improvement of oral bioavailability of repaglinide was investigated systematically. The inclusion complex of repaglinide was prepared by lyophilization technique using drug: hydroxypropyl-β-cyclodextrin (1:15 mole). The prepared complexation was characterized by differential scanning calorimetry (DSC), X-ray diffractometry (XRD), NMR spectroscopy and evaluated by dissolution studies. The (1)H NMR was used in the structure study of repaglinide-HP-β-CD (RPG-HP-β-CD) inclusion complex. The analysis proved the higher probability of the repaglinide A-ring into the narrow rim of the β-cyclodextrin molecule. All the characterization information confirmed the formation of RPG-HP-β-CD inclusion complex. The in vivo pharmacokinetics of RPG-HP-β-CD and their physical mixture were performed in beagle dogs. For the first time, a simple, rapid, and sensitive LC-MS/MS method for determination of RPG in beagle dog plasma was developed. The Cmax and AUC0-t of RPG-HP-β-CD were 2.5 and 2 times higher than that of the physical mixture. These results suggested that the interaction of repaglinide with HP-β-CD could notably improve the dissolution rate and bioavailability of repaglinide comparing with its physical mixture. Copyright © 2014 Elsevier B.V. All rights reserved.

Nanoparticles Prepared From N,N-Dimethyl-N-Octyl Chitosan as the Novel Approach for Oral Delivery of Insulin: Preparation, Statistical Optimization and In-vitro Characterization

PubMed Central

Shamsa, Elnaz Sadat; Mahjub, Reza; Mansoorpour, Maryam; Rafiee-Tehrani, Morteza; Abedin Dorkoosh, Farid

2018-01-01

In this study, N,N-Dimethyl-N-Octyl chitosan was synthesized. Nanoparticles containing insulin were prepared using PEC method and were statistically optimized using the Box-Behnken response surface methodology. The independent factors were considered to be the insulin concentration, concentration and pH of the polymer solution, while the dependent factors were characterized as the size, zeta potential, PdI and entrapment efficiency. The optimized nanoparticles were morphologically studied using SEM. The cytotoxicity of the nanoparticles on the Caco-2 cell culture was studied using the MTT cytotoxicity assay method, while the permeation of the insulin nanoparticles across the Caco-2 cell monolayer was also determined. The optimized nanoparticles posed appropriate physicochemical properties. The SEM morphological studies showed spherical to sub-spherical nanoparticles with no sign of aggregation. The in-vitro release study showed that 95.5 ± 1.40% of the loaded insulin was released in 400 min. The permeability studies revealed significant enhancement in the insulin permeability using nanoparticles prepared from octyl chitosan at 240 min (11.3 ± 0.78%). The obtained data revealed that insulin nanoparticles prepared from N,N-Dimethyl-N-Octyl chitosan can be considered as the good candidate for oral delivery of insulin compared to nanoparticles prepared from N,N,N-trimethyl chitosan.

Preparation, characterization, and anti-Helicobacter pylori activity of Bi3+-Hericium erinaceus polysaccharide complex.

PubMed

Zhu, Yang; Chen, Yao; Li, Qian; Zhao, Ting; Zhang, Ming; Feng, Weiwei; Takase, Mohammed; Wu, Xueshan; Zhou, Zhaoxiang; Yang, Liuqing; Wu, Xiangyang

2014-09-22

Two new Bi3+-Hericium erinaceus polysaccharide (BiHEP) complexes were prepared using Bi3+ and two purified polysaccharides from H. erinaceus (HEPs), respectively. The complexes were characterized by elemental analysis, FT-IR, CD, SEM, AFM, XRD, and TG. The anti-Helicobacter pylori (Hp) activities in vitro by agar dilution assay of the complexes were evaluated. The molecular weights of HEPs were 197 and 20 kDa, respectively. All the analyses confirmed the formation of new BiHEP complexes with lower content of Bi3+ compared with colloidal bismuth subcitrate (CBS), the most utilized bismuth preparation clinically. Furthermore, HEPs themselves have definite inhibition effects on Hp, and BiHEP complexes have lower content of Bi exhibited strong inhibition effects on Hp (MIC=20 μg/mL), similar to that of CBS with higher content of Bi. The study provides a basis for further development of multiple treatments of Hp infection or new medicines. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparation and characterization of antibacterial electrospun chitosan/poly (vinyl alcohol)/graphene oxide composite nanofibrous membrane

NASA Astrophysics Data System (ADS)

Yang, Shuai; Lei, Peng; Shan, Yujuan; Zhang, Dawei

2018-03-01

In this paper, chitosan (CS)/poly (vinyl alcohol) (PVA)/graphene oxide (GO) composite nanofibrous membranes were prepared via electrospinning. Such nanofibrous membranes have been characterized and investigated for their morphological, structural, thermal stability, hydrophilic and antibacterial properties. SEM images showed that the uniform and defect-free nanofibers were obtained and GO sheets, shaping spindle and spherical, were partially embedded into nanofibers. FTIR, XRD, DSC and TGA indicated the good compatibility between CS and PVA. There were strong intermolecular hydrogen bonds between the chitosan and PVA molecules. Contact angle measurement indicated that while increasing the content of GO, the distance between fibers increased and water drop showed wetting state on the surface of nanofibrous membranes. As a result, the contact angle decreased significantly. Meanwhile, good antibacterial activity of the prepared nanofibrous membranes were exhibited against Gram-negative Escherichia coli and Gram-positive Staphylococcus aureus.

Preparation and characterization of N-benzoyl-O-acetyl-chitosan.

PubMed

Cai, Jinping; Dang, Qifeng; Liu, Chengsheng; Fan, Bing; Yan, Jingquan; Xu, Yanyan; Li, Jingjing

2015-01-01

A novel amphipathic chitosan derivative, N-benzoyl-O-acetyl-chitosan (BACS), was prepared by using the selective partial acylation of chitosan (CS), benzoyl chloride, and acetic acid under high-intensity ultrasound. The chemical structure and physical properties of BACS were characterized by FTIR, (1)H NMR, TGA, and XRD techniques. The degrees of substitution of benzoyl and acetyl for the chitosan derivatives were 0.26 and 1.15, respectively, which were calculated from the peak areas in NMR spectra by using the combined integral methods. The foaming properties of CS and BACS were determined and the results suggested BACS had better foam capacity and stability than those of chitosan. In addition, the antimicrobial activities of CS and BACS were also investigated against two species of bacteria (Escherichia coli and Staphylococcus aureus) and a fungus (Aspergillus niger), the results indicated that the antibacterial and antifungal activities of BACS were much stronger than those of the parent chitosan. These findings suggested that BACS was preferable for use as a food additive with a dual role of both foaming agent and food preservative. Copyright © 2015 Elsevier B.V. All rights reserved.

Streptomycin-loaded PLGA-alginate nanoparticles: preparation, characterization, and assessment

NASA Astrophysics Data System (ADS)

Asadi, Asadollah

2014-04-01

The aim of this study was to formulate and characterize streptomycin-loaded PLGA-alginate nanoparticles for their potential therapeutic use in Salmonella subsp. enterica ATCC 14028 infections. The streptomycin nanoparticle was prepared by solvent diffusion method, and the other properties such as size, zeta potential, loading efficacy, release kinetics, and antimicrobial strength were evaluated. The survey shows that nanoparticles may serve as a carrier of streptomycin and may provide localized antibacterial activity in the treatment of Salmonellosis. Electron microscopy showed spherical particles with indentations. The average size of the nanoparticles was 90 nm. At pH 7.2, the release kinetics of streptomycin from the nanoparticles was successfully illustrated as an initial burst defined by a first order equation that after this stage, it has a drastic tendency to obtain steady state. Nevertheless, nanoparticles showed loading efficacy nearly about 70-75 %. In addition, the tendency of concentration of streptomycin released from nanoparticles to reach antibacterial activity was similar to that of free streptomycin against PLGA-alginate, but it had threefold more antimicrobial strength in comparison with free streptomycin. This work shows the potential use of streptomycin-loaded PLGA-alginate nanoparticles and its capability.

Preparation and characterization of MWCNT nanofiller incorporated polymer composite for lithium battery applications

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

Pradeepa, P.; Raj, S. Edwin; Selvakumar, K.

Poly (ethyl methacrylate) based polymer electrolyte films were prepared by solution casting technique incorporating multi-walled carbon nanotube (MWCNT) as filler and characterized using XRD and Ac impedance analysis. The electrical conductivity is increased with increasing filler concentration (upto 6wt %), which is attributed to the formation of charge transfer complexes. The maximum ionic conductivity value is found to be 1.171×10{sup −3} Scm{sup −1} at 303K for PEMA (19wt %) -LiClO{sub 4} (8wt %) -MWCNT (6wt %) -PC (67wt %) electrolyte system. The temperature dependent ionic conductivity plot seems to obey Vogel -Tamman-Fulcher relation.

Preparation, characterization, and catalytic activity of zirconocene bridged on surface of silica gel

NASA Astrophysics Data System (ADS)

El Majdoub, Lotfia; Shi, Yasai; Yuan, Yuan; Zhou, Annan; Abutartour, Abubaker; Xu, Qinghong

2015-10-01

Zirconocene catalyst supported on silica gel was prepared for olefin polymerization by surface modification of calcined silica with SiCl4, and the reaction between the modified silica and cyclopentadienyl sodium and ZrCl4. The catalyst was characterized by using Fourier-transform infrared (FT-IR) spectrometer, thermogravimetric (TG), and differential scanning calorimetric (DSC) analytic spectrometer. It was found that the metallocene structure could be formed and connected on silica surface by chemical bond. Initial catalytic tests showed that the supported metallocene was catalytically active (methylaluminoxane as a cocatalyst), producing polymer with higher molecular weight than the metallocene just immobilized on the surface of silica gel.

Preparation and characterization of specific and high-affinity monoclonal antibodies against morphine.

PubMed

Rahbarizadeh, F; Rasaee, M J; Madani, R; Rahbarizadeh, M H; Omidfar, K

2000-10-01

A C6-hemisuccinate derivative of morphine was prepared and conjugated to bovine serum albumin. High titer antibody producing spleen cells were removed and fused with myeloma cells of Sp2/0 origin. A C3-hemisuccinate derivative of morphine was prepared and conjugated to enzyme penicillinase used as a tracer molecule. A novel enzyme-linked immunoadsorbent assay was developed using this conjugate to screen and characterize the monoclonal antibody produced in these experiments. After two successive limiting dilutions, antibodies produced by 5 clones with good affinities ranging from 10(8) to 10(12) M(-1) and less cross-reaction (least for codeine and other structurally related molecules) were selected. These clones were found to be of IgG class with kappa light chain. Subclass determination showed that two of the clones produced IgG2b and three of them produced IgG1 type of antibody. Affinity purifications were performed for the selected clone (MOR-I). Purified antibody was coated onto the wells of microtiter plate. The standard curve was constructed with a sensitivity of 100 pg/mL covering up to 10 ng/mL in buffer and urine. The slope of the standard curve for selected clone in buffer and urine was calculated to be -0.7 and -0.64, respectively.

CHITOSAN-CELLULOSE COMPOSITE MATERIALS: PREPARATION, CHARACTERIZATION AND APPLICATION FOR REMOVAL OF MICROCYSTIN

PubMed Central

Tran, Chieu D.; Duri, Simon; Delneri, Ambra; Franko, Mladen

2013-01-01

We developed a simple and one-step method to prepare biocompatible composites from cellulose (CEL) and chitosan (CS). [BMIm+Cl−], an ionic liquid (IL), was used as a green solvent to dissolve and prepare the [CEL+CS] composites. Since majority (>88%) of IL used was recovered for reuse by distilling the aqueous washings of [CEL+CS], the method is recyclable. XRD, FTIR, NIR, 13C CP-MAS-NMR and SEM were used to monitor the dissolution and to characterize the composites. The composite was found to have combined advantages of their components: superior mechanical strength (from CEL) and excellent adsorption capability for microcystin-LR, a deadly toxin produced by cyanobacteria (from CS). Specifically, the mechanical strength of the composites increased with CEL loading; e.g., up to 5X increase in tensile strength was achieved by adding 80% of CEL into CS. Kinetic results of adsorption confirm that unique properties of CS remain intact in the composite, i.e., it is not only a very good adsorbent for microcystin but also is better than all other available adsorbents. For example, it can adsorb 4X times more microcystin than the best reported adsorbent. Importantly, the microcystin adsorbed can be quantitatively desorbed to enable the composite to be reused with similar adsorption efficiency. PMID:23542326

Preparation and characterization of green graphene using grape seed extract for bioapplications.

PubMed

Yaragalla, Srinivasarao; Rajendran, Rajakumari; Jose, Jiya; AlMaadeed, Mariam A; Kalarikkal, Nandakumar; Thomas, Sabu

2016-08-01

The development of functionalized graphene materials concerning health and environmental aspects via green approaches is currently the most recent topic in the field of nanoscience and nanotechnology. Herein, we report the green reduction of graphene oxide (GO) to reduced graphene oxide (RGO) using grape seed extract (GSE). Structural properties of the prepared RGO were investigated using Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, thermogravimetric analysis (TGA), UV-Visible spectroscopy and X-ray diffraction analysis. These all characterization techniques clearly revealed that the RGO has been successfully prepared. Moreover, the average thickness (4.2nm) of RGO layers was also confirmed by transmission electron microscopy (TEM). Optical properties such as band gap and photoluminescence of the synthesized RGO were evaluated. The band gap of RGO was found to be 3.84eV and it showed emission in the visible region. Efficient antimicrobial activity against Escherichia coli and Staphylococcus aureus was observed with 4μgml(-1) & 5μgml(-1) of RGO and also the cell wall damage of these strains has been proved by atomic force microscopy (AFM). The in vitro study of RGO (500μg) disclosed the effective anti-proliferative activity (88%) against HCT-116 cell lines. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation and Characterization of Extruded Composites Based on Polypropylene and Chitosan Compatibilized with Polypropylene-Graft-Maleic Anhydride.

PubMed

Carrasco-Guigón, Fernando Javier; Rodríguez-Félix, Dora Evelia; Castillo-Ortega, María Mónica; Santacruz-Ortega, Hisila C; Burruel-Ibarra, Silvia E; Encinas-Encinas, Jose Carmelo; Plascencia-Jatomea, Maribel; Herrera-Franco, Pedro Jesus; Madera-Santana, Tomas Jesus

2017-01-25

The preparation of composites of synthetic and natural polymers represent an interesting option to combine properties; in this manner, polypropylene and chitosan extruded films using a different proportion of components and polypropylene-graft-maleic anhydride (PPgMA) as compatibilizer were prepared. The effect of the content of the biopolymer in the polypropylene (PP) matrix, the addition of compatibilizer, and the particle size on the properties of the composites was analyzed using characterization by fourier transform-infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), tensile strength, and contact angle, finding that in general, the addition of the compatibilizer and reducing the particle size of the chitosan, favored the physicochemical and morphological properties of the films.

Preparation and characterization of hydroxyapatite-coated iron oxide particles by spray-drying technique.

PubMed

Donadel, Karina; Felisberto, Marcos D V; Laranjeira, Mauro C M

2009-06-01

Magnetic particles of iron oxide have been increasingly used in medical diagnosis by magnetic resonance imaging and in cancer therapies involving targeted drug delivery and magnetic hyperthermia. In this study we report the preparation and characterization of iron oxide particles coated with bioceramic hydroxyapatite by spray-drying. The iron oxide magnetic particles (IOMP) were coated with hydroxyapatite (HAp) by spray-drying using two IOMP/HAp ratios (0.7 and 3.2). The magnetic particles were characterized by way of scanning electronic microscopy, energy dispersive X-ray, X-ray diffraction, Fourier transformed infrared spectroscopy, flame atomic absorption spectrometry,vibrating sample magnetometry and particle size distribution (laser diffraction). The surface morphology of the coated samples is different from that of the iron oxide due to formation of hydroxyapatite coating. From an EDX analysis, it was verified that the surface of the coated magnetic particles is composed only of HAp, while the interior containsiron oxide and a few layers of HAp as expected. The results showed that spray-drying technique is an efficient and relatively inexpensive method for forming spherical particles with a core/shell structure.

Preparation and characterization of nanocomposite polymer electrolytes poly(vinylidone fluoride)/nanoclay

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

Rahmawati, Suci A.; Sulistyaningsih,; Putro, Alviansyah Z. A.

2016-02-08

Polymer electrolytes are defined as semi solid electrolytes used as separator in lithium ion battery. Separator used as medium for transfer ions and to prevent electrical short circuits in battery cells. To obtain the optimal battery performance, separator with high porosity and electrolyte uptake is required. This can reduce the resistance in the transfer of ions between cathode and anode. The main objective of this work is to investigate the impact of different solvent (Dimethyl acetamide (DMAc), N-methyl-2-pyrrolidone (NMP) and dimethyl formamide (DMF)), pore forming agent poly(vinylpyrolidone) (PVP) and nanoclay as filler in addition of membrane using phase inversion methodmore » on the morphology, porosity, electrolyte uptake and degree of crystallinity. The membrane was prepared by the phase inversion method by adding PVP and Nanoclay using different solvents. The phase inversion method was prepared by dissolving Nanoclay and PVP in solvent for 1-2 hours, and then add the PVDF with stirring for 4 hours at 60°C. The membranes were characterized by porosity test, electrolyte uptake test, scanning electron microscope (SEM), and X-ray diffraction (XRD). The results showed that DMAc as solvent gives the highest value of porosity and electrolyte uptake. The addition of nanoclay and PVP enlarge the size of the pores and reduce the degree of crystallinity. So, the usage of DMAc as solvent is better than NMP or DMF.« less

Ag-Cu nanoalloyed film as a high-performance cathode electrocatalytic material for zinc-air battery

NASA Astrophysics Data System (ADS)

Lei, Yimin; Chen, Fuyi; Jin, Yachao; Liu, Zongwen

2015-04-01

A novel Ag50Cu50 film electrocatalyst for oxygen reduction reaction (ORR) was prepared by pulsed laser deposition (PLD) method. The electrocatalyst actually is Ag-Cu alloyed nanoparticles embedded in amorphous Cu film, based on transmission electron microscopy (TEM) characterization. The rotating disk electrode (RDE) measurements provide evidence that the ORR proceed via a four-electron pathway on the electrocatalysts in alkaline solution. And it is much more efficient than pure Ag catalyst. The catalytic layer has maximum power density of 67 mW cm-2 and an acceptable cell voltage at 0.863 V when current densities increased up to 100 mA cm-2 in the Ag50Cu50-based primary zinc-air battery. The resulting rechargeable zinc-air battery exhibits low charge-discharge voltage polarization of 1.1 V at 20 mAcm-2 and high durability over 100 cycles in natural air.

Preparation and characterization of Chitosan/Konjac glucomannan/CdS nanocomposite film with low infrared emissivity

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

Zhang, Feng-Ying; Zhou, Yu-Ming, E-mail: fchem@seu.edu.cn; Sun, Yan-qing

Novel organic-inorganic nanocomposite films were prepared with Chitosan (CS), Konjac glucomannan (KGM) and CdS by one-step synthesis. As-prepared films were characterized by IR spectra, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and infrared emissometer (IR). The results indicated that grown CdS dendrites were formed with reaction time of 12 h for Cd{sup 2+} and CS/KGM, and were well dispersed in CS/KGM with an average diameter of 40 nm. The CS/KGM/CdS nanocomposite films had significantly low infrared emissivity. When the mole ratio of CdS to summation of CS and KGM construction units was 1.0 with CdS size of 10-20 nm,more » the film got the lowest infrared emissivity value of 0.011, which could be attributed to the strong synergism effect existing between CS/KGM and CdS dendrites.« less

Preparation and Characterization of Microencapsulated Phase Change Materials for Use in Building Applications.

PubMed

Giro-Paloma, Jessica; Al-Shannaq, Refat; Fernández, Ana Inés; Farid, Mohammed M

2015-12-26

A method for preparing and characterizing microencapsulated phase change materials (MPCM) was developed. A comparison with a commercial MPCM is also presented. Both MPCM contained paraffin wax as PCM with acrylic shell. The melting temperature of the PCM was around 21 °C, suitable for building applications. The M-2 (our laboratory made sample) and Micronal ® DS 5008 X (BASF) samples were characterized using SEM, DSC, nano-indentation technique, and Gas Chromatography/Mass spectrometry (GC-MS). Both samples presented a 6 μm average size and a spherical shape. Thermal energy storage (TES) capacities were 111.73 J·g -1 and 99.3 J·g -1 for M-2 and Micronal ® DS 5008 X, respectively. Mechanical characterization of the samples was performed by nano-indentation technique in order to determine the elastic modulus ( E ), load at maximum displacement ( P m ), and displacement at maximum load ( h m ), concluding that M-2 presented slightly better mechanical properties. Finally, an important parameter for considering use in buildings is the release of volatile organic compounds (VOC's). This characteristic was studied at 65 °C by CG-MS. Both samples showed VOC's emission after 10 min of heating, however peaks intensity of VOC's generated from M-2 microcapsules showed a lower concentration than Micronal ® DS 5008 X.

Preparation and Characterization of Microencapsulated Phase Change Materials for Use in Building Applications

PubMed Central

Giro-Paloma, Jessica; Al-Shannaq, Refat; Fernández, Ana Inés; Farid, Mohammed M.

2015-01-01

A method for preparing and characterizing microencapsulated phase change materials (MPCM) was developed. A comparison with a commercial MPCM is also presented. Both MPCM contained paraffin wax as PCM with acrylic shell. The melting temperature of the PCM was around 21 °C, suitable for building applications. The M-2 (our laboratory made sample) and Micronal® DS 5008 X (BASF) samples were characterized using SEM, DSC, nano-indentation technique, and Gas Chromatography/Mass spectrometry (GC-MS). Both samples presented a 6 μm average size and a spherical shape. Thermal energy storage (TES) capacities were 111.73 J·g−1 and 99.3 J·g−1 for M-2 and Micronal® DS 5008 X, respectively. Mechanical characterization of the samples was performed by nano-indentation technique in order to determine the elastic modulus (E), load at maximum displacement (Pm), and displacement at maximum load (hm), concluding that M-2 presented slightly better mechanical properties. Finally, an important parameter for considering use in buildings is the release of volatile organic compounds (VOC’s). This characteristic was studied at 65 °C by CG-MS. Both samples showed VOC’s emission after 10 min of heating, however peaks intensity of VOC’s generated from M-2 microcapsules showed a lower concentration than Micronal® DS 5008 X. PMID:28787812

Preparation and Characterization of Selenium Incorporated Guar Gum Nanoparticle and Its Interaction with H9c2 Cells

PubMed Central

Soumya, Rema Sreenivasan; Vineetha, Vadavanath Prabhakaran; Reshma, Premachandran Latha; Raghu, Kozhiparambil Gopalan

2013-01-01

This study deals with the preparation and characterization of selenium incorporated guar gum nanoparticle (SGG), and its effect on H9c2 cardiomyoblast. Herein, nanoprecipitation techniques had been employed for the preparation of SGG nanoparticle. The prepared nanoparticle had been subjected to various types of analytical techniques like transmission electron microscopy (TEM), X-ray diffraction (XRD) and particle size analysis to confirm the characteristics of nanoparticle as well as for selenium incorporation. Physical characterization of nanoparticle showed that the size of nanoparticles increase upto ∼69–173 nm upon selenium incorporation from ∼41–132 nm. Then the prepared nanoparticles were evaluated for its effect on H9c2 cells. In this regard, the effect of nanoparticle on various vital parameters of H9c2 cells was studied. Parameters like cell viability, uptake of selenium incorporated guar gum nanoparticle by the cells, effect of SGG on DNA integrity, apoptosis, reactive oxygen species generation, alteration in transmembrane potential of mitochondria and cytoskeletal integrity had been investigated. Viability results showed that up to 25 nM of SGG was safe (10.31%) but beyond that it induces cytotoxicity. Cellular uptake of selenium showed that cell permeability for SGG is significantly high compared to normal selenium (7.2 nM of selenium for 25 nM SGG compared with 5.2 nM selenium for 25 nM sodium selenite). There was no apoptosis with SGG and also it protects DNA from hydroxyl radical induced breakage. Likewise no adverse effect on mitochondria and cytoskeleton was observed for 25 nM of SGG. Overall results reveal that SGG is highly suitable for biomedical research application. PMID:24098647

Preparation and characterization of polymeric nanocomposite films for application as protective coatings

NASA Astrophysics Data System (ADS)

Gagliardi, S.; Rondino, F.; D'Erme, C.; Persia, F.; Menchini, F.; Santarelli, M. L.; Paulke, B.-R.; Enayati, A. L.; Falconieri, M.

2017-08-01

Addiction of ceramic nanoparticles to acrylic polymers provides a simple and effective means to produce paints with important properties, such as mechanical resistance and tailored wettability, even though for optimal performances, an engineered nanoparticle distribution would be desirable. In this paper we report on the realization and on the morphological and functional characterization of nanocomposites where the nanophase is distributed on the surface of acrylic polymer films, in order to enhance the expression of surface-related properties. To this aim, commercial titanium oxide and silicon oxide nanopowders were dispersed in water and the suspensions were air-sprayed on polymeric films prepared by paint brushing, thus producing a nanostructured ceramic surface coating. Control of the pH of suspensions and acrylic acid functionalization of the surface of titania were used together with high power ultrasonic treatments in order to control dimension of the aggregates in the sprayed suspensions. Optical microscopy, mechanical profilometry, and atomic force microscopy were used to characterize the nanocomposite surface morphology and correlate it to the coating functional properties, evaluated through mechanical abrasion tests and contact angle measurements; also, colorimetry on coated stones was performed in order to test the impact of the coatings on the aesthetical appearance and their photostability under UV irradiation. Results show that the nanostructured ceramic layer slightly improves the resistance of coatings to mechanical abrasion in case of polymer films prepared from latexes. The nanocomposite surface layer does not affect the wettability of the polymer, which remained slightly hydrophilic; this behavior is likely due to inadequate distribution of the nanophase. On the other hand UV-induced superhydrophilicity was observed when the concentration of surface titania nanoparticles is about 0.6 mg/cm2. Colorimetric analysis on historical and Carrara

Preparation, Characterization and Activity of a Peptide-Cellulosic Aerogel Protease Sensor from Cotton

PubMed Central

Edwards, J. Vincent; Fontenot, Krystal R.; Prevost, Nicolette T.; Pircher, Nicole; Liebner, Falk; Condon, Brian D.

2016-01-01

Nanocellulosic aerogels (NA) provide a lightweight biocompatible material with structural properties, like interconnected high porosity and specific surface area, suitable for biosensor design. We report here the preparation, characterization and activity of peptide-nanocellulose aerogels (PepNA) made from unprocessed cotton and designed with protease detection activity. Low-density cellulosic aerogels were prepared from greige cotton by employing calcium thiocyanate octahydrate/lithium chloride as a direct cellulose dissolving medium. Subsequent casting, coagulation, solvent exchange and supercritical carbon dioxide drying afforded homogeneous cellulose II aerogels of fibrous morphology. The cotton-based aerogel had a porosity of 99% largely dominated by mesopores (2–50 nm) and an internal surface of 163 m2·g−1. A fluorescent tripeptide-substrate (succinyl-alanine-proline-alanine-4-amino-7-methyl-coumarin) was tethered to NA by (1) esterification of cellulose C6 surface hydroxyl groups with glycidyl-fluorenylmethyloxycarbonyl (FMOC), (2) deprotection and (3) coupling of the immobilized glycine with the tripeptide. Characterization of the NA and PepNA included techniques, such as elemental analysis, mass spectral analysis, attenuated total reflectance infrared imaging, nitrogen adsorption, scanning electron microscopy and bioactivity studies. The degree of substitution of the peptide analog attached to the anhydroglucose units of PepNA was 0.015. The findings from mass spectral analysis and attenuated total reflectance infrared imaging indicated that the peptide substrate was immobilized on to the surface of the NA. Nitrogen adsorption revealed a high specific surface area and a highly porous system, which supports the open porous structure observed from scanning electron microscopy images. Bioactivity studies of PepNA revealed a detection sensitivity of 0.13 units/milliliter for human neutrophil elastase, a diagnostic biomarker for inflammatory diseases. The

Preparation, Characterization and Activity of a Peptide-Cellulosic Aerogel Protease Sensor from Cotton.

PubMed

Edwards, J Vincent; Fontenot, Krystal R; Prevost, Nicolette T; Pircher, Nicole; Liebner, Falk; Condon, Brian D

2016-10-26

Nanocellulosic aerogels (NA) provide a lightweight biocompatible material with structural properties, like interconnected high porosity and specific surface area, suitable for biosensor design. We report here the preparation, characterization and activity of peptide-nanocellulose aerogels (PepNA) made from unprocessed cotton and designed with protease detection activity. Low-density cellulosic aerogels were prepared from greige cotton by employing calcium thiocyanate octahydrate/lithium chloride as a direct cellulose dissolving medium. Subsequent casting, coagulation, solvent exchange and supercritical carbon dioxide drying afforded homogeneous cellulose II aerogels of fibrous morphology. The cotton-based aerogel had a porosity of 99% largely dominated by mesopores (2-50 nm) and an internal surface of 163 m²·g -1 . A fluorescent tripeptide-substrate (succinyl-alanine-proline-alanine-4-amino-7-methyl-coumarin) was tethered to NA by (1) esterification of cellulose C6 surface hydroxyl groups with glycidyl-fluorenylmethyloxycarbonyl (FMOC), (2) deprotection and (3) coupling of the immobilized glycine with the tripeptide. Characterization of the NA and PepNA included techniques, such as elemental analysis, mass spectral analysis, attenuated total reflectance infrared imaging, nitrogen adsorption, scanning electron microscopy and bioactivity studies. The degree of substitution of the peptide analog attached to the anhydroglucose units of PepNA was 0.015. The findings from mass spectral analysis and attenuated total reflectance infrared imaging indicated that the peptide substrate was immobilized on to the surface of the NA. Nitrogen adsorption revealed a high specific surface area and a highly porous system, which supports the open porous structure observed from scanning electron microscopy images. Bioactivity studies of PepNA revealed a detection sensitivity of 0.13 units/milliliter for human neutrophil elastase, a diagnostic biomarker for inflammatory diseases. The

Hydroxyapatite/MCM-41 and SBA-15 Nano-Composites: Preparation, Characterization and Applications

PubMed Central

Anunziata, Oscar A.; Martínez, Maria L.; Beltramone, Andrea R.

2009-01-01

Composites of hydroxyapatite (HaP) and highly ordered large pore mesoporous silica molecular sieves such as, Al-SBA-15 and Al-MCM-41 (denoted as SBA-15 and MCM-41, respectively) were developed, characterized by XRD, BET, FTIR, HRTEM and NMR-MAS, and applied to fluoride retention from contaminated water. The proposed procedure by a new route to prepare the HaP/SBA-15 and HaP/MCM-41, composites generates materials with aluminum only in tetrahedral coordination, according to the 27Al NMR-MAS results. Free OH- groups of HaP nanocrystals, within the hosts, allowed high capacity fluoride retention. The activity of fluoride retention using HaP/MCM-41 or HaP/SBA-15 was 1-2 orders of magnitude greater, respectively, than with pure HaP.

Desulfurization of Cysteine-Containing Peptides Resulting from Sample Preparation for Protein Characterization by MS

PubMed Central

Wang, Zhouxi; Rejtar, Tomas; Zhou, Zhaohui Sunny; Karger, Barry L.

2010-01-01

In this paper, we have examined two cysteine modifications resulting from sample preparation for protein characterization by MS: (1) a previously observed conversion of cysteine to dehydroalanine, now found in the case of disulfide mapping and (2) a novel modification corresponding to conversion of cysteine to alanine. Using model peptides, the conversion of cysteine to dehydroalanine via β-elimination of a disulfide bond was seen to result from the conditions of typical tryptic digestion (37 °C, pH 7.0– 9.0) without disulfide reduction and alkylation.. Furthermore, the surprising conversion of cysteine to alanine was shown to occur by heating cysteine containing peptides in the presence of a phosphine (TCEP). The formation of alanine from cysteine, investigated by performing experiments in H2O or D2O, suggested a radical-based desulfurization mechanism unrelated to β-elimination. Importantly, an understanding of the mechanism and conditions favorable for cysteine desulfurization provides insight for the establishment of improved sample preparation procedures of protein analysis. PMID:20049891

Preparation and Characterization of Extruded Composites Based on Polypropylene and Chitosan Compatibilized with Polypropylene-Graft-Maleic Anhydride

PubMed Central

Carrasco-Guigón, Fernando Javier; Rodríguez-Félix, Dora Evelia; Castillo-Ortega, María Mónica; Santacruz-Ortega, Hisila C.; Burruel-Ibarra, Silvia E.; Encinas-Encinas, Jose Carmelo; Plascencia-Jatomea, Maribel; Herrera-Franco, Pedro Jesus; Madera-Santana, Tomas Jesus

2017-01-01

The preparation of composites of synthetic and natural polymers represent an interesting option to combine properties; in this manner, polypropylene and chitosan extruded films using a different proportion of components and polypropylene-graft-maleic anhydride (PPgMA) as compatibilizer were prepared. The effect of the content of the biopolymer in the polypropylene (PP) matrix, the addition of compatibilizer, and the particle size on the properties of the composites was analyzed using characterization by fourier transform-infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), tensile strength, and contact angle, finding that in general, the addition of the compatibilizer and reducing the particle size of the chitosan, favored the physicochemical and morphological properties of the films. PMID:28772464

X-ray absorption and Mössbauer spectroscopies characterization of iron nanoclusters prepared by the gas aggregation technique.

PubMed

Sánchez-Marcos, J; Laguna-Marco, M A; Martínez-Morillas, R; Céspedes, E; Menéndez, N; Jiménez-Villacorta, F; Prieto, C

2012-11-01

Partially oxidized iron nanoclusters have been prepared by the gas-phase aggregation technique with typical sizes of 2-3 nm. This preparation technique has been reported to obtain clusters with interesting magnetic properties such as very large exchange bias. In this paper, a sample composition study carried out by Mössbauer and X-ray absorption spectroscopies is reported. The information reached by these techniques, which is based on the iron short range order, results to be an ideal way to have a characterization of the whole sample since the obtained data are an average over a very large amount of the clusters. In addition, our results indicate the presence of ferrihydrite, which is a compound typically ignored when studying this type of systems.

Preparation and characterization of the nanoporous ultrathin multilayer films based on molybdenum polyoxometalate (Mo 38) n

NASA Astrophysics Data System (ADS)

Wang, L.; Jiang, M.; Wang, E. B.; Duan, L. Y.; Hao, N.; Lan, Y.; Xu, L.; Li, Z.

2003-11-01

Ultrathin multilayer films of the wheel-shaped molybdenum polyoxometalate cluster (Mo 38) n and poly(allylamine hydrochloride)(PAH) have been prepared by the layer-by-layer (LbL) self-assembly method. The ((Mo 38) n/PAH) m multilayer films have been characterized by X-ray photoelectron spectra (XPS) and atomic force microscopy (AFM). UV-VIS measurements reveal regular film growth with each (Mo 38) n adsorption. The electrochemistry behavior of the film at room temperature was investigated.

Preparation, Characterization and Properties of Alginate/Poly(γ-glutamic acid) Composite Microparticles

PubMed Central

Tong, Zongrui; Chen, Yu; Liu, Yang; Tong, Li; Chu, Jiamian; Xiao, Kecen; Zhou, Zhiyu; Dong, Wenbo; Chu, Xingwu

2017-01-01

Alginate (Alg) is a renewable polymer with excellent hemostatic properties and biocapability and is widely used for hemostatic wound dressing. However, the swelling properties of alginate-based wound dressings need to be promoted to meet the requirements of wider application. Poly(γ-glutamic acid) (PGA) is a natural polymer with high hydrophility. In the current study, novel Alg/PGA composite microparticles with double network structure were prepared by the emulsification/internal gelation method. It was found from the structure characterization that a double network structure was formed in the composite microparticles due to the ion chelation interaction between Ca2+ and the carboxylate groups of Alg and PGA and the electrostatic interaction between the secondary amine group of PGA and the carboxylate groups of Alg and PGA. The swelling behavior of the composite microparticles was significantly improved due to the high hydrophility of PGA. Influences of the preparing conditions on the swelling behavior of the composites were investigated. The porous microparticles could be formed while compositing of PGA. Thermal stability was studied by thermogravimetric analysis method. Moreover, in vitro cytocompatibility test of microparticles exhibited good biocompatibility with L929 cells. All results indicated that such Alg/PGA composite microparticles are a promising candidate in the field of wound dressing for hemostasis or rapid removal of exudates. PMID:28398222

Preparation, Characterization and Properties of Alginate/Poly(γ-glutamic acid) Composite Microparticles.

PubMed

Tong, Zongrui; Chen, Yu; Liu, Yang; Tong, Li; Chu, Jiamian; Xiao, Kecen; Zhou, Zhiyu; Dong, Wenbo; Chu, Xingwu

2017-04-11

Alginate (Alg) is a renewable polymer with excellent hemostatic properties and biocapability and is widely used for hemostatic wound dressing. However, the swelling properties of alginate-based wound dressings need to be promoted to meet the requirements of wider application. Poly( γ -glutamic acid) (PGA) is a natural polymer with high hydrophility. In the current study, novel Alg/PGA composite microparticles with double network structure were prepared by the emulsification/internal gelation method. It was found from the structure characterization that a double network structure was formed in the composite microparticles due to the ion chelation interaction between Ca 2+ and the carboxylate groups of Alg and PGA and the electrostatic interaction between the secondary amine group of PGA and the carboxylate groups of Alg and PGA. The swelling behavior of the composite microparticles was significantly improved due to the high hydrophility of PGA. Influences of the preparing conditions on the swelling behavior of the composites were investigated. The porous microparticles could be formed while compositing of PGA. Thermal stability was studied by thermogravimetric analysis method. Moreover, in vitro cytocompatibility test of microparticles exhibited good biocompatibility with L929 cells. All results indicated that such Alg/PGA composite microparticles are a promising candidate in the field of wound dressing for hemostasis or rapid removal of exudates.

Preparation and characterization of carbon nanofibrous/hydroxyapatite sheets for bone tissue engineering.

PubMed

Abd El-Aziz, A M; El Backly, Rania M; Taha, Nahla A; El-Maghraby, Azza; Kandil, Sherif H

2017-07-01

Critical size bone defects are orthopedic defects that will not heal without intervention or that will not completely heal over the natural life time of the animal. Although bone generally has the ability to regenerate completely however, critical defects require some sort of scaffold to do so. In the current study we proposed a method to obtain a carbon nanofibrous/Hydroxyapatite (HA) bioactive scaffold. The carbon nanofibrous (CNF) nonwoven fabrics were obtained by the use of the electrospinning process of the polymeric solution of poly acrylonitrile "PAN" and subsequent stabilization and carbonization processes. The CNFs sheets were functionalized by both hydroxyapatite (HA) and bovine serum albumin (BSA). The HA was added to the electrospun solution, but in case of (BSA), it was adsorbed after the carbonization process. The changes in the properties taking place in the precursor sheets were investigated using the characterization methods (SEM, FT-IR, TGA and EDX). The prepared materials were tested for biocompatibility via subcutaneous implantation in New Zealand white rabbits. We successfully prepared biocompatible functionalized sheets, which have been modified with HA or HA and BSA. The sheets that were functionalized by both HA and BSA are more biocompatible with fewer inflammatory cells of (neutrophils and lymphocytes) than ones with only HA over the period of 3weeks. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation, characterization, and antibacterial activity studies of silver-loaded poly(styrene-co-acrylic acid) nanocomposites.

PubMed

Song, Cunfeng; Chang, Ying; Cheng, Ling; Xu, Yiting; Chen, Xiaoling; Zhang, Long; Zhong, Lina; Dai, Lizong

2014-03-01

A simple method for preparing a new type of stable antibacterial agent was presented. Monodisperse poly(styrene-co-acrylic acid) (PSA) nanospheres, serving as matrices, were synthesized via soap-free emulsion polymerization. Field-emission scanning electron microscopy micrographs indicated that PSA nanospheres have interesting surface microstructures and well-controlled particle size distributions. Silver-loaded poly(styrene-co-acrylic acid) (PSA/Ag-NPs) nanocomposites were prepared in situ through interfacial reduction of silver nitrate with sodium borohydride, and further characterized by transmission electron microscopy and X-ray diffraction. Their effects on antibacterial activity including inhibition zone, minimum inhibitory concentration (MIC), minimum bactericidal concentration (MBC), and bactericidal kinetics were evaluated. In the tests, PSA/Ag-NPs nanocomposites showed excellent antibacterial activity against both gram-positive Staphylococcus aureus and gram-negative Escherichia coli. These nanocomposites are considered to have potential application in antibacterial coatings on biomedical devices to reduce nosocomial infection rates. Copyright © 2013 Elsevier B.V. All rights reserved.

Liposomes Containing Gadodiamide: Preparation, Physicochemical Characterization, and In Vitro Cytotoxic Evaluation.

PubMed

Maia, Ana Luiza Chaves; Fernandes, Christian; de Oliveira, Cynthia Nara Pereira; Teixeira, Claudia Salviano; Oliveira, Mariana Silva; Soares, Daniel Cristian Ferreira; Ramaldes, Gilson Andrade

2017-01-01

The aim of this study was to develop, characterize and assess the cytotoxic activity of pHsensitive (pHL-Gd), stealth pH-sensitive (SpHL-Gd), and conventional (convL-Gd) liposomes containing gadodiamide (Gd-DTPA-BMA). Formulations were prepared by reverse-phase evaporation method and their physicochemical properties were evaluated by means of particle size, zeta potential, and Gd-DTPA-BMA entrapment. SpHL-Gd was considered being the most promising liposome, since it combines stealth and fusogenic characteristics that might contribute to achieve higher therapeutic efficiency. Their drug encapsulation percentages have been optimized satisfactorily. The addition of Gd-DTPA-BMA at 125 μmol/mL in the SpHL-Gd preparation allowed obtaining liposomes with appropriate encapsulation percentage (20.3 ± 0.1%) and entrapment (25.4 ± 0.1 μmol/mL). The cytotoxic studies on the 4T1 breast cancer cell line demonstrated that liposomes-loaded with Gd-DTPA-BMA inhibited cancer cell. pHL-Gd and SpHL-Gd liposomes showed higher activity than convL-Gd and free Gd-DTPA-BMA, indicating that the pH-sensitive characteristic was important to improve intracellular delivery. The presence of polyethylene glycol (PEG) in the SpHL-Gd formulation did not affect the pH-sensitivity and internalization. Therefore, the results of this study suggest the feasibility of liposomes containing Gd-DTPA-BMA as a new promising controlled delivery system. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Preparation and characterization of a novel adsorbent from Moringa oleifera leaf

NASA Astrophysics Data System (ADS)

Bello, Olugbenga Solomon; Adegoke, Kayode Adesina; Akinyunni, Opeyemi Omowumi

2017-06-01

A new and novel adsorbent was obtained by impregnation of Moringa oleifera leaf in H2SO4 and NaOH, respectively. Prepared adsorbents were characterized using elemental analysis, FT-IR, SEM, TGA and EDX analyses, respectively. The effects of operational parameters, such as pH, moisture content, ash content, porosity and iodine number on these adsorbents were investigated and compared with those of commercial activated carbon (CAC). EDX results of acid activated M. oleifera leaf have the highest percentage of carbon by weight (69.40 %) and (76.11 %) by atom, respectively. Proximate analysis showed that the fixed carbon content of acid activated M. oleifera leaf (69.14 ± 0.01) was the highest of all adsorbents studied. Conclusively, the present investigation shows that acid activated M. oleifera leaf is a good alternative adsorbent that could be used in lieu of CAC for recovery of dyes and heavy metal from aqueous solutions and other separation techniques.

Polymeric Nanoparticles of Brazilian Red Propolis Extract: Preparation, Characterization, Antioxidant and Leishmanicidal Activity

NASA Astrophysics Data System (ADS)

do Nascimento, Ticiano Gomes; da Silva, Priscilla Fonseca; Azevedo, Lais Farias; da Rocha, Louisianny Guerra; de Moraes Porto, Isabel Cristina Celerino; Lima e Moura, Túlio Flávio Accioly; Basílio-Júnior, Irinaldo Diniz; Grillo, Luciano Aparecido Meireles; Dornelas, Camila Braga; Fonseca, Eduardo Jorge da Silva; de Jesus Oliveira, Eduardo; Zhang, Alex Tong; Watson, David G.

2016-06-01

The ever-increasing demand for natural products and biotechnology derived from bees and ultra-modernization of various analytical devices has facilitated the rational and planned development of biotechnology products with a focus on human health to treat chronic and neglected diseases. The aim of the present study was to prepare and characterize polymeric nanoparticles loaded with Brazilian red propolis extract and evaluate the cytotoxic activity of "multiple-constituent extract in co-delivery system" for antileishmanial therapies. The polymeric nanoparticles loaded with red propolis extract were prepared with a combination of poly-ɛ-caprolactone and pluronic using nanoprecipitation method and characterized by different analytical techniques, antioxidant and leishmanicidal assay. The red propolis nanoparticles in aqueous medium presented particle size (200-280 nm) in nanometric scale and zeta analysis (-20 to -26 mV) revealed stability of the nanoparticles without aggregation phenomenon during 1 month. After freeze-drying method using cryoprotectant (sodium starch glycolate), it was possible to observe particles with smooth and spherical shape and apparent size of 200 to 400 nm. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) and thermal analysis revealed the encapsulation of the flavonoids from the red propolis extract into the polymeric matrix. Ultra performance liquid chromatography coupled with diode array detector (UPLC-DAD) identified the flavonoids liquiritigenin, pinobanksin, isoliquiritigenin, formononetin and biochanin A in ethanolic extract of propolis (EEP) and nanoparticles of red propolis extract (NRPE). The efficiency of encapsulation was determinate, and median values (75.0 %) were calculated using UPLC-DAD. 2,2-Diphenyl-1-picryhydrazyl method showed antioxidant activity to EEP and red propolis nanoparticles. Compared to negative control, EEP and NRPE exhibited leishmanicidal activity with an IC50 value of ≅38.0 �

Preparation and characterization of mucoadhesive nanoparticles of poly (methyl vinyl ether-co-maleic anhydride) containing glycyrrhizic acid intended for vaginal administration.

PubMed

Aguilar-Rosas, Irene; Alcalá-Alcalá, Sergio; Llera-Rojas, Viridiana; Ganem-Rondero, Adriana

2015-01-01

Traditional vaginal preparations reside in the vaginal cavity for relatively a short period of time, requiring multiple doses in order to attain the desired therapeutic effect. Therefore, mucoadhesive systems appear to be appropriate to prolong the residence time in the vaginal cavity. In the current study, mucoadhesive nanoparticles based on poly(methyl vinyl ether-co-maleic anhydride) (PVM/MA) intended for vaginal delivery of glycyrrhizic acid (GA) (a drug with well-known antiviral properties) were prepared and characterized. Nanoparticles were generated by a solvent displacement method. Incorporation of GA was performed during nanoprecipitation, followed by adsorption of drug once nanoparticles were formed. The prepared nanoparticles were characterized in terms of size, Z-potential, morphology, drug loading, interaction of GA with PVM/MA (by differential scanning calorimetry) and the in vitro interaction of nanoparticles with pig mucin (at two pH values, 3.6 and 5; with and without GA adsorbed). The preparation method led to nanoparticles of a mean diameter of 198.5 ± 24.3 nm, zeta potential of -44.8 ± 2.8 mV and drug loading of 15.07 ± 0.86 µg/mg polymer. The highest mucin interaction resulted at pH 3.6 for nanoparticles without GA adsorbed. The data obtained suggest the promise of using mucoadhesive nanoparticles of PVM/MA for intravaginal delivery of GA.

Preparation and characterization of natural bentonite in to nanoparticles by co-precipitation method

NASA Astrophysics Data System (ADS)

Sirait, Makmur; Bukit, Nurdin; Siregar, Nurdin

2017-01-01

The nanoparticle based on natural bentonite from Pahae village had been prepared using co-precipitation method. Bentonite was dried in the oven at 100°C during a week. Bentonite is crushed using a mortal and milled by planetary ball mill to obtain the powder form. Further, the bentonite powder is activated with chemical reaction by dissolves the 50 g bentonite to 100 ml of HCl at 10 M. The magnetic stirrer was employed to mix the solution at 300 rpm and temperature 70°C. After that, the bentonite solution is washed using distilled water until the pH is neutral. The bentonite powder is calcined at temperature of 600°C for 1 hour with fix increment 150°C. Finally, the powder is given High Energy Milling (HEM) treatment for 30 minutes to obtain the particle size. The X-ray Difractometer (XRD) and Scanning Electron Microscope (SEM) were used to characterize. From the characterization results it is reported that the average of bentonite nanoparticle size is 35.26 nm and the chemical constituents of natural bentonite Pahae are Al, Si, Ca, Fe and Ti.

Error baseline rates of five sample preparation methods used to characterize RNA virus populations.

PubMed

Kugelman, Jeffrey R; Wiley, Michael R; Nagle, Elyse R; Reyes, Daniel; Pfeffer, Brad P; Kuhn, Jens H; Sanchez-Lockhart, Mariano; Palacios, Gustavo F

2017-01-01

Individual RNA viruses typically occur as populations of genomes that differ slightly from each other due to mutations introduced by the error-prone viral polymerase. Understanding the variability of RNA virus genome populations is critical for understanding virus evolution because individual mutant genomes may gain evolutionary selective advantages and give rise to dominant subpopulations, possibly even leading to the emergence of viruses resistant to medical countermeasures. Reverse transcription of virus genome populations followed by next-generation sequencing is the only available method to characterize variation for RNA viruses. However, both steps may lead to the introduction of artificial mutations, thereby skewing the data. To better understand how such errors are introduced during sample preparation, we determined and compared error baseline rates of five different sample preparation methods by analyzing in vitro transcribed Ebola virus RNA from an artificial plasmid-based system. These methods included: shotgun sequencing from plasmid DNA or in vitro transcribed RNA as a basic "no amplification" method, amplicon sequencing from the plasmid DNA or in vitro transcribed RNA as a "targeted" amplification method, sequence-independent single-primer amplification (SISPA) as a "random" amplification method, rolling circle reverse transcription sequencing (CirSeq) as an advanced "no amplification" method, and Illumina TruSeq RNA Access as a "targeted" enrichment method. The measured error frequencies indicate that RNA Access offers the best tradeoff between sensitivity and sample preparation error (1.4-5) of all compared methods.

Error baseline rates of five sample preparation methods used to characterize RNA virus populations

PubMed Central

Kugelman, Jeffrey R.; Wiley, Michael R.; Nagle, Elyse R.; Reyes, Daniel; Pfeffer, Brad P.; Kuhn, Jens H.; Sanchez-Lockhart, Mariano; Palacios, Gustavo F.

2017-01-01

Individual RNA viruses typically occur as populations of genomes that differ slightly from each other due to mutations introduced by the error-prone viral polymerase. Understanding the variability of RNA virus genome populations is critical for understanding virus evolution because individual mutant genomes may gain evolutionary selective advantages and give rise to dominant subpopulations, possibly even leading to the emergence of viruses resistant to medical countermeasures. Reverse transcription of virus genome populations followed by next-generation sequencing is the only available method to characterize variation for RNA viruses. However, both steps may lead to the introduction of artificial mutations, thereby skewing the data. To better understand how such errors are introduced during sample preparation, we determined and compared error baseline rates of five different sample preparation methods by analyzing in vitro transcribed Ebola virus RNA from an artificial plasmid-based system. These methods included: shotgun sequencing from plasmid DNA or in vitro transcribed RNA as a basic “no amplification” method, amplicon sequencing from the plasmid DNA or in vitro transcribed RNA as a “targeted” amplification method, sequence-independent single-primer amplification (SISPA) as a “random” amplification method, rolling circle reverse transcription sequencing (CirSeq) as an advanced “no amplification” method, and Illumina TruSeq RNA Access as a “targeted” enrichment method. The measured error frequencies indicate that RNA Access offers the best tradeoff between sensitivity and sample preparation error (1.4−5) of all compared methods. PMID:28182717

Preparation and characterization of PANI@G/CWO nanocomposite for enhanced 2-nitrophenol sensing

NASA Astrophysics Data System (ADS)

Khan, Anish; Khan, Aftab Aslam Parwaz; Rahman, Mohammed M.; Asiri, Abdullah M.; Inamuddin; Alamry, Khalid A.; Hameed, Salem A.

2018-03-01

A new material by polymer insertion via graphene oxide into cerium tungstate was prepared by very simple oxidation-reduction method. Aniline polymerization was done on the surface of graphene oxide (GO) which was reduced to graphene (G) simultaneously mixed with separately prepared inorganic matrices of cerium tungstate (Ce2(WO4)3 (CWO)). PANI@G/CWO was characterized by various spectroscopic methods as SEM, FTIR, TGA, XRD and XPS to confirm its possibilities. Selective 2-nitrophenol sensor was fabricated on flat glassy carbon electrode (GCE) and PANI@G/CWO nanocomposites in the form of thin layer. It was found excellent sensitivity as well as long life spam with broad dynamic concentration range (LDR) that showed efficient electrochemical performance towards 2-nitrophenol on fabricated chemical sensor by PANI@G/CWO. The linear calibration curve (r2 = 0.9914) with wide range of 2-nitrophenol concentration (1.0 nM-1.0 mM) was found having the detection limit of 0.87 nM while the sensitivity of the sensor was around 1.229 μ A μM-1 cm-2. It was introduced a new route for the development of a versatile phenolic sensor based on PANI@G/CWO nanocomposites by I-V method that is proved more selective and sensitive for environmental toxic materials.

Preparation and characterization of polymer nanocomposites coated magnetic nanoparticles for drug delivery applications

NASA Astrophysics Data System (ADS)

Prabha, G.; Raj, V.

2016-06-01

In the present research work, the anticancer drug 'curcumin' is loaded with Chitosan (CS)-polyethylene glycol (PEG)-polyvinylpyrrolidone (PVP) (CS-PEG-PVP) polymer nanocomposites coated with superparamagnetic iron oxide (Fe3O4) nanoparticles. The system can be used for targeted and controlled drug delivery of anticancer drugs with reduced side effects and greater efficiency. The prepared nanoparticles were characterized by Fourier transmission infrared spectroscopy (FTIR), vibrating sample magnetometry (VSM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Curcumin drug loaded Fe3O4-CS, Fe3O4-CS-PEG and Fe3O4-CS-PEG-PVP nanoparticles exhibited the mean particle size in the range of 183-390 nm with a zeta potential value of 26-41 mV as measured using Malvern Zetasizer. The encapsulation efficiency, loading capacity and in-vitro drug release behavior of curcumin drug loaded Fe3O4-CS, Fe3O4-CS-PEG and Fe3O4-CS-PEG-PVP nanoparticles were studied using UV spectrophotometer. Besides, the cytotoxicity of the prepared nanoparticles using MTT assay was also studied. The curcumin drug release was examined at different pH medium and it was proved that the drug release depends upon the pH medium in addition to the nature of matrix.

Role of nanocrystallinity on the chemical ordering of Co xPt 100-x nanocrystals synthesized by wet chemistry

DOE PAGES

Cordeiro, Marco; Kameche, Farid; Ngo, Anh -Tu; ...

2015-03-17

Co xPt 100–x nanoalloys have been synthesized by two different chemical processes either at high or at low temperature. Their physical properties and the order/disorder phase transition induced by annealing have been investigated depending on the route of synthesis. It is demonstrated that the chemical synthesis at high temperature allows stabilization of the fcc structure of the native nanoalloys while the soft chemical approach yields mainly poly or non crystalline structure. As a result the approach of the order/disorder phase transition is strongly modified as observed by high-resolution transmission electron microscopy (HR-TEM) studies performed during in situ annealing of themore » different nanoalloys. The control of the nanocrystallinity leads to significant decrease in the chemical ordering temperature as the ordered structure is observed at temperatures as low as 420 °C. Furthermore, this in turn preserves the individual nanocrystals and prevents their coalescence usually observed during the annealing necessary for the transition to an ordered phase.« less

Role of the nanocrystallinity on the chemical ordering of Co(x)Pt(100-x) nanocrystals synthesized by wet chemistry.

PubMed

Kameche, Farid; Ngo, Anh-Tu; Salzemann, Caroline; Cordeiro, Marco; Sutter, Eli; Petit, Christophe

2015-11-14

Co(x)Pt(100-x) nanoalloys have been synthesized by two different chemical processes either at high or at low temperature. Their physical properties and the order/disorder phase transition induced by annealing have been investigated depending on the route of synthesis. It is demonstrated that the chemical synthesis at high temperature allows stabilization of the fcc structure of the native nanoalloys while the soft chemical approach yields mainly poly or non crystalline structure. As a result the approach of the order/disorder phase transition is strongly modified as observed by high-resolution transmission electron microscopy (HR-TEM) studies performed during in situ annealing of the different nanoalloys. The control of the nanocrystallinity leads to significant decrease in the chemical ordering temperature as the ordered structure is observed at temperatures as low as 420 °C. This in turn preserves the individual nanocrystals and prevents their coalescence usually observed during the annealing necessary for the transition to an ordered phase.

Preparation and characterization Al3+-bentonite Turen Malang for esterification fatty acid (palmitic acid, oleic acid and linoleic acid)

NASA Astrophysics Data System (ADS)

Abdulloh, Abdulloh; Aminah, Nanik Siti; Triyono, Mudasir, Trisunaryanti, Wega

2016-03-01

Catalyst preparation and characterization of Al3+-bentonite for esterification of palmitic acid, oleic acid and linoleic acid has been done. Al3+-bentonite catalyst was prepared from natural bentonite of Turen Malang through cation exchange reaction using AlCl3 solution. The catalysts obtained were characterized by XRD, XRF, pyridine-FTIR and surface area analyser using the BET method. Catalyst activity test of Al3+-bentonite for esterification reaction was done at 65°C using molar ratio of metanol-fatty acid of 30:1 and 0.25 g of Al3+-bentonite catalyst for the period of ½, 1, 2, 3, 4 and 5 hours. Based on the characterization results, the Al3+-bentonite Turen Malang catalyst has a d-spacing of 15.63 Ǻ, acid sites of Brönsted and Lewis respectively of 230.79 µmol/g and 99.39 µmol/g, surface area of 507.3 m2/g and the average of radius pore of 20.09 Å. GC-MS analysis results of the oil phase after esterification reaction showed the formation of biodiesel (FAME: Fatty acid methyl ester), namely methyl palmitate, methyl oleate and methyl linoleate. The number of conversions resulted in esterification reaction using Al3+-bentonite Turen Malang catalyst was 74.61%, 37.75%, and 20, 93% for the esterification of palmitic acid, oleic acid and linoleic acid respectively.

Structural characterization of nanocrystalline cadmium sulphide powder prepared by solvent evaporation technique

NASA Astrophysics Data System (ADS)

Pandya, Samir; Tandel, Digisha; Chodavadiya, Nisarg

2018-05-01

CdS is one of the most important compounds in the II-VI group of semiconductor. There are numerous applications of CdS in the form of nanoparticles and nanocrystalline. Semiconductors nanoparticles (also known as quantum dots), belong to state of matter in the transition region between molecules and solids, have attracted a great deal of attention because of their unique electrical and optical properties, compared to bulk materials. In the field of optoelectronic, nanocrystalline form utilizes mostly in the field of catalysis and fluid technology. Considering these observations, presented work had been carried out, i.e. based on the nanocrystalline material preparation. In the present work CdS nano-crystalline powder was synthesized by a simple and cost effective chemical technique to grow cadmium sulphide (CdS) nanoparticles at 200 °C with different concentrations of cadmium. The synthesis parameters were optimized. The synthesized powder was structurally characterized by X-ray diffraction and particle size analyzer. In the XRD analysis, Micro-structural parameters such as lattice strain, dislocation density and crystallite size were analysed. The broadened diffraction peaks indicated nanocrystalline particles of the film material. In addition to that the size of the prepared particles was analyzed by particle size analyzer. The results show the average size of CdS particles ranging from 80 to 100 nm. The overall conclusion of the work can be very useful in the synthesis of nanocrystalline CdS powder.

Preparation and characterization of nanosized Ag/SLN composite and its viability for improved occlusion

NASA Astrophysics Data System (ADS)

Cynthia Jemima Swarnavalli, G.; Dinakaran, S.; Divya, S.

2016-10-01

Nanocomposites consisting of silver and solid lipid nanoparticles (SLN) elicit interest for their synergistic effect based enhanced properties in skin hydration. The nanocomposite preparation aims at combining the antimicrobial activity of silver with skin hydration performance of SLN. The nanocomposites designated Ag/SAN (silver/stearic acid nanoparticles), Ag/PAN (silver/palmitic acid nanoparticles) were prepared by incorporating silver nanoparticles into the dispersion of SLN and sonicating for 10 min followed by heating for 1 h at 50 °C in a thermostat. The occlusive property of the two nanocomposites was evaluated in comparison with the pure SLN by adopting de Vringer-de Ronde in vitro occlusion test. The incorporation of silver nanoparticles has improved occlusion factor by 10 % in the case of both composites at SLN concentration of 0.14 mmol. Characterization studies include XRD, DSC, HRSEM, DLS and zeta potential measurement. High resolution scanning electron microscopy (HRSEM) images divulge that the nanoparticles of composite (Ag/SAN) shows halo effect where the hydrophobic stearic acid is oriented at the core and is surrounded by silver nanoparticles while Ag/PAN shows cashew shaped SLN dispersed in silver nanoparticles matrix.

Preparation, characterization and optimization of sildenafil citrate loaded PLGA nanoparticles by statistical factorial design

PubMed Central

2013-01-01

Background and the aim of the study The objective of the present study was to formulate and optimize nanoparticles (NPs) of sildenafil-loaded poly (lactic-co-glycolic acid) (PLGA) by double emulsion solvent evaporation (DESE) method. The relationship between design factors and experimental data was evaluated using response surface methodology. Method A Box-Behnken design was made considering the mass ratio of drug to polymer (D/P), the volumetric proportion of the water to oil phase (W/O) and the concentration of polyvinyl alcohol (PVA) as the independent agents. PLGA-NPs were successfully prepared and the size (nm), entrapment efficiency (EE), drug loading (DL) and cumulative release of drug from NPs post 1 and 8 hrs were assessed as the responses. Results The NPs were prepared in a spherical shape and the sizes range of 240 to 316 nm. The polydispersity index of size was lower than 0.5 and the EE (%) and DL (%) varied between 14-62% and 2-6%, respectively. The optimized formulation with a desirability factor of 0.9 was selected and characterized. This formulation demonstrated the particle size of 270 nm, EE of 55%, DL of 3.9% and cumulative drug release of 79% after 12 hrs. In vitro release studies showed a burst release at the initial stage followed by a sustained release of sildenafil from NPs up to 12 hrs. The release kinetic of the optimized formulation was fitted to Higuchi model. Conclusions Sildenafil citrate NPs with small particle size, lipophilic feature, high entrapment efficiency and good loading capacity is produced by this method. Characterization of optimum formulation, provided by an evaluation of experimental data, showed no significant difference between calculated and measured data. PMID:24355133

Preparation and characterization of V/TiO{sub 2} nanocatalyst with magnetic nucleus of iron

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

Feyzi, Mostafa; Rafiee, Hamid Reza, E-mail: rafieehr@yahoo.com; Ranjbar, Shahram

2013-11-15

Graphical abstract: - Highlights: • Fe-V/TiO{sub 2} nanocatalyst is prepared. • Combination of sol–gel and wetness impregnation methods. • Facile separation of catalyst from medium by magnet. - Abstract: A magnetic composite containing V/TiO{sub 2} was prepared by combination of sol–gel and wetness impregnation methods. The effects of synthesis temperature, different weight percents of Fe supported on TiO{sub 2}, vanadium loading and the heating rate of calcination on the structure and morphology of nanocatalyst were investigated. The optimum conditions for synthesized catalyst were 40 wt.% of Fe, 15 wt.% of V and synthesis temperature equal to 30 °C. Characterization ofmore » catalyst is carried out using XRD, TGA, DSC, SEM, FTIR and N{sub 2} physisorption measurements. The magnetic character of nanocatalyst was measured using VSM, which showed the typical paramagnetic behavior of sample at room temperature with a saturation magnetization value equal to 8.283 emu/g. The nanocatalyst has a particle size about 56 nm and can easily be separated from medium by a magnet.« less

Characterization of Lone Pine, California, tremolite asbestos and preparation of research material

USGS Publications Warehouse

Harper, Martin; Van Gosen, Bradley S.; Crankshaw, Owen S; Doorn, Stacy S; Ennis, J. Todd; Harrison, Sara E

2014-01-01

Well-characterized amphibole asbestos mineral samples are required for use as analytical standards and in future research projects. Currently, the National Institute for Standards and Technology Standard Reference Material samples of asbestos are listed as ‘Discontinued’. The National Institute for Occupational Safety and Health (NIOSH) has a goal under the Asbestos Roadmap of locating and characterizing research materials for future use. Where an initial characterization analysis determines that a collected material is appropriate for use as a research material in terms of composition and asbestiform habit, sufficient amounts of the material will be collected to make it publicly available. An abandoned mine near Lone Pine, California, contains a vein of tremolite asbestos, which was the probable source of a reference material that has been available for the past 17 years from the Health and Safety Laboratory (HSL) in the UK. Newly collected fibrous vein material from this mine was analyzed at Research Triangle Institute (RTI International) with some additional analysis by the US Geological Survey’s Denver Microbeam Laboratory. The analysis at RTI International included: (i) polarized light microscopy (PLM) with a determination of principal optical properties; (ii) X-ray diffraction; (iii) transmission electron microscopy, including energy dispersive X-ray spectroscopy and selected-area electron diffraction; and (iv) spindle stage analysis using PLM to determine whether individual fibers and bundles of the samples were polycrystalline or single-crystal cleavage fragments. The overall findings of the study indicated that the material is tremolite asbestos with characteristics substantially similar to the earlier distributed HSL reference material. A larger quantity of material was prepared by sorting, acid-washing and mixing for sub-division into vials of ~10g each. These vials have been transferred from NIOSH to RTI International, from where they can be

Characterization of Lone Pine, California, Tremolite Asbestos and Preparation of Research Material

PubMed Central

Harper, Martin; Van Gosen, Bradley; Crankshaw, Owen S.; Doorn, Stacy S.; Ennis, Todd J.; Harrison, Sara E.

2016-01-01

Well-characterized amphibole asbestos mineral samples are required for use as analytical standards and in future research projects. Currently, the National Institute for Standards and Technology Standard Reference Material samples of asbestos are listed as ‘Discontinued’. The National Institute for Occupational Safety and Health (NIOSH) has a goal under the Asbestos Roadmap of locating and characterizing research materials for future use. Where an initial characterization analysis determines that a collected material is appropriate for use as a research material in terms of composition and asbestiform habit, sufficient amounts of the material will be collected to make it publicly available. An abandoned mine near Lone Pine, California, contains a vein of tremolite asbestos, which was the probable source of a reference material that has been available for the past 17 years from the Health and Safety Laboratory (HSL) in the UK. Newly collected fibrous vein material from this mine was analyzed at Research Triangle Institute (RTI International) with some additional analysis by the US Geological Survey’s Denver Microbeam Laboratory. The analysis at RTI International included: (i) polarized light microscopy (PLM) with a determination of principal optical properties; (ii) X-ray diffraction; (iii) transmission electron microscopy, including energy dispersive X-ray spectroscopy and selected-area electron diffraction; and (iv) spindle stage analysis using PLM to determine whether individual fibers and bundles of the samples were polycrystalline or single-crystal cleavage fragments. The overall findings of the study indicated that the material is tremolite asbestos with characteristics substantially similar to the earlier distributed HSL reference material. A larger quantity of material was prepared by sorting, acid-washing and mixing for sub-division into vials of ~10 g each. These vials have been transferred from NIOSH to RTI International, from where they can be

Flavourzyme, an Enzyme Preparation with Industrial Relevance: Automated Nine-Step Purification and Partial Characterization of Eight Enzymes.

PubMed

Merz, Michael; Eisele, Thomas; Berends, Pieter; Appel, Daniel; Rabe, Swen; Blank, Imre; Stressler, Timo; Fischer, Lutz

2015-06-17

Flavourzyme is sold as a peptidase preparation from Aspergillus oryzae. The enzyme preparation is widely and diversely used for protein hydrolysis in industrial and research applications. However, detailed information about the composition of this mixture is still missing due to the complexity. The present study identified eight key enzymes by mass spectrometry and partially by activity staining on native polyacrylamide gels or gel zymography. The eight enzymes identified were two aminopeptidases, two dipeptidyl peptidases, three endopeptidases, and one α-amylase from the A. oryzae strain ATCC 42149/RIB 40 (yellow koji mold). Various specific marker substrates for these Flavourzyme enzymes were ascertained. An automated, time-saving nine-step protocol for the purification of all eight enzymes within 7 h was designed. Finally, the purified Flavourzyme enzymes were biochemically characterized with regard to pH and temperature profiles and molecular sizes.

Preparation and characterization of high purity β-chitin from squid pens (Loligo chenisis).

PubMed

Cuong, Hoang Ngoc; Minh, Nguyen Cong; Van Hoa, Nguyen; Trung, Trang Si

2016-12-01

Squid pens were extracted by a NaOH solution at 80°C for 10h to remove protein and minerals. The as-prepared β-chitin had a high molecular weight (8.5±0.1×10 3 kDa), a low protein content (0.63±0.02wt.%), and a negligible amount of minerals. This method avoids the conventional method for the removal of minerals from shrimp and crab shells by HCl. The purity of resulting products was measured by NMR and FTIR. Moreover, the morphology and crystallinity of β-chitin was characterized by SEM and XRD. The β-chitin with long chains and high purity is suitable for producing high quantity β-chitosan for various potential applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation, characterization and antibacterial properties against E. coli K88 of chitosan nanoparticle loaded copper ions

NASA Astrophysics Data System (ADS)

Du, Wen-Li; Xu, Ying-Lei; Xu, Zi-Rong; Fan, Cheng-Li

2008-02-01

The present study was conducted to prepare and characterize chitosan nanoparticle loaded copper ions, and evaluate their antibacterial activity. Chitosan nanoparticles were prepared based on ionotropic gelation, and then the copper ions were loaded. The particle size, zeta potential and morphology were determined. Antibacterial activity was evaluated against E. coli K88 by determination of the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) in vitro. Results showed that the antibacterial activity was significantly enhanced by the loading of copper ions compared to those of chitosan nanoparticles and copper ions. The MIC and MBC of chitosan nanoparticle loaded copper ions were 21 times and 42 times lower than those of copper ions, respectively. To confirm the antibacterial mechanism, morphological changes of E. coli K88 treated by chitosan nanoparticle loaded copper ions were dynamically observed with an atomic force microscope (AFM). It was found that chitosan nanoparticle loaded copper ions killed E. coli K88 through damage to the cell membrane.

Preparation of biocompatible magnetite-carboxymethyl cellulose nanocomposite: characterization of nanocomposite by FTIR, XRD, FESEM and TEM.

PubMed

Habibi, Neda

2014-10-15

The preparation and characterization of magnetite-carboxymethyl cellulose nano-composite (M-CMC) material is described. Magnetite nano-particles were synthesized by a modified co-precipitation method using ferrous chloride tetrahydrate and ferric chloride hexahydrate in ammonium hydroxide solution. The M-CMC nano-composite particles were synthesized by embedding the magnetite nanoparticles inside carboxymethyl cellulose (CMC) using a freshly prepared mixture of Fe3O4 with CMC precursor. Morphology, particle size, and structural properties of magnetite-carboxymethyl cellulose nano-composite was accomplished using X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. As a result, magnetite nano-particles with an average size of 35nm were obtained. The biocompatible Fe3O4-carboxymethyl cellulose nano-composite particles obtained from the natural CMC polymers have a potential range of application in biomedical field. Copyright © 2014 Elsevier B.V. All rights reserved.

Polymeric Nanoparticles of Brazilian Red Propolis Extract: Preparation, Characterization, Antioxidant and Leishmanicidal Activity.

PubMed

do Nascimento, Ticiano Gomes; da Silva, Priscilla Fonseca; Azevedo, Lais Farias; da Rocha, Louisianny Guerra; de Moraes Porto, Isabel Cristina Celerino; Lima E Moura, Túlio Flávio Accioly; Basílio-Júnior, Irinaldo Diniz; Grillo, Luciano Aparecido Meireles; Dornelas, Camila Braga; Fonseca, Eduardo Jorge da Silva; de Jesus Oliveira, Eduardo; Zhang, Alex Tong; Watson, David G

2016-12-01

The ever-increasing demand for natural products and biotechnology derived from bees and ultra-modernization of various analytical devices has facilitated the rational and planned development of biotechnology products with a focus on human health to treat chronic and neglected diseases. The aim of the present study was to prepare and characterize polymeric nanoparticles loaded with Brazilian red propolis extract and evaluate the cytotoxic activity of "multiple-constituent extract in co-delivery system" for antileishmanial therapies. The polymeric nanoparticles loaded with red propolis extract were prepared with a combination of poly-ε-caprolactone and pluronic using nanoprecipitation method and characterized by different analytical techniques, antioxidant and leishmanicidal assay. The red propolis nanoparticles in aqueous medium presented particle size (200-280 nm) in nanometric scale and zeta analysis (-20 to -26 mV) revealed stability of the nanoparticles without aggregation phenomenon during 1 month. After freeze-drying method using cryoprotectant (sodium starch glycolate), it was possible to observe particles with smooth and spherical shape and apparent size of 200 to 400 nm. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) and thermal analysis revealed the encapsulation of the flavonoids from the red propolis extract into the polymeric matrix. Ultra performance liquid chromatography coupled with diode array detector (UPLC-DAD) identified the flavonoids liquiritigenin, pinobanksin, isoliquiritigenin, formononetin and biochanin A in ethanolic extract of propolis (EEP) and nanoparticles of red propolis extract (NRPE). The efficiency of encapsulation was determinate, and median values (75.0 %) were calculated using UPLC-DAD. 2,2-Diphenyl-1-picryhydrazyl method showed antioxidant activity to EEP and red propolis nanoparticles. Compared to negative control, EEP and NRPE exhibited leishmanicidal activity with an IC50 value of ≅38

Preparation and characterization of nanocrystalline cellulose/Eucommia ulmoides gum nanocomposite film.

PubMed

Sun, Qianqian; Zhao, Xinkun; Wang, Dongmei; Dong, Juane; She, Diao; Peng, Pai

2018-02-01

The nanocomposite films were prepared using Eucommia ulmoides gum (EUG) matrix reinforced with nanocrystalline cellulose (NCC) at different concentrations. Subsequently, the obtained films were characterized by Raman spectra, AFM, XRD, TGA, and DSC. Meanwhile, the wettability, mechanical, and water vapor barrier properties of these films were analyzed. AFM noticed that the average sizes of NCC were 81.95×50.17×13.06nm, while the size of molecular chain for EUG was 2530×57.33×1.28nm. In comparison with control film, a certain amount of NCC obviously improved elongation at break and enhanced their crystallinity and ΔH m . More importantly, NCC/EUG nanocomposite films presented lower thermal stability, glass transition temperature (T g ), melting temperature (T m ), and water vapor permeability (WVP) values, especially the WVP values of 4% NCC film were the lowest as 0.28×10 -9 , 0.30×10 -9 , and 0.58×10 -9 g/m/h/Pa at RH 34%, 55%, and 76%, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparation and characterization of self-crosslinked organic/inorganic proton exchange membranes

NASA Astrophysics Data System (ADS)

Zhong, Shuangling; Cui, Xuejun; Dou, Sen; Liu, Wencong

A series of silicon-containing sulfonated polystyrene/acrylate (Si-sPS/A) nanoparticles are successfully synthesized via simple emulsion polymerization method. The Si-sPS/A latexes show good film-forming capability and the self-crosslinked organic/inorganic proton exchange membranes are prepared by pouring the Si-sPS/A nanoparticle latexes into glass plates and drying at 60 °C for 10 h and 120 °C for 2 h. The potential of the membranes in direct methanol fuel cells (DMFCs) is characterized preliminarily by studying their thermal stability, ion-exchange capacity, water uptake, methanol diffusion coefficient, proton conductivity and selectivity (proton conductivity/methanol diffusion coefficient). The results indicate that these membranes possess excellent thermal stability and methanol barrier due to the existence of self-crosslinked silica network. In addition, the proton conductivity of the membranes is in the range of 10 -3-10 -2 S cm -1 and all the membranes show much higher selectivity in comparison with Nafion ® 117. These results suggest that the self-crosslinked organic/inorganic proton exchange membranes are particularly promising in DMFC applications.

Preparation and physicochemical characterization of 5 niclosamide solvates and 1 hemisolvate.

PubMed

van Tonder, Elsa C; Mahlatji, Mabatane D; Malan, Sarel F; Liebenberg, Wilna; Caira, Mino R; Song, Mingna; de Villiers, Melgardt M

2004-02-23

The purpose of the study was to characterize the physicochemical, structural, and spectral properties of the 1:1 niclosamide and methanol, diethyl ether, dimethyl sulfoxide, N,N' dimethylformamide, and tetrahydrofuran solvates and the 2:1 niclosamide and tetraethylene glycol hemisolvate prepared by recrystallization from these organic solvents. Structural, spectral, and thermal analysis results confirmed the presence of the solvents and differences in the structural properties of these solvates. In addition, differences in the activation energy of desolvation, batch solution calorimetry, and the aqueous solubility at 25 degrees C, 24 hours, showed the stability of the solvates to be in the order: anhydrate > diethyl ether solvate > tetraethylene glycol hemisolvate > methanol solvate > dimethyl sulfoxide solvate > N,N' dimethylformamide solvate. The intrinsic and powder dissolution rates of the solvates were in the order: anhydrate > diethyl ether solvate > tetraethylene glycol hemisolvate > N,N' dimethylformamide solvate > methanol solvate > dimethyl sulfoxide solvate. Although these nonaqueous solvates had higher solubility and dissolution rates than the monohydrous forms, they were unstable in aqueous media and rapidly transformed to one of the monohydrous forms.

Formulation, Preparation, and Characterization of Polyurethane Foams

ERIC Educational Resources Information Center

Pinto, Moises L.

2010-01-01

Preparation of laboratory-scale polyurethane foams is described with formulations that are easy to implement in experiments for undergraduate students. Particular attention is given to formulation aspects that are based on the main chemical reactions occurring in polyurethane production. This allows students to develop alternative formulations to…

The preparation and characterization of a lithium borate glass prepared by the gel technique

NASA Technical Reports Server (NTRS)

Weinberg, M. C.; Neilson, G. F.; Smith, G. L.; Dunn, B.; Moore, G. S.; Mackenzie, J. D.

1985-01-01

The preparation of an amorphous lithium borate gel by the metal organic procedure is described. In addition, a preliminary evaluation of the behavior of the gel upon heating is given. In particular the crystallization tendency of the gel is studied with the aid of DTA and X-ray diffraction, and the structural changes in the gel are monitored with the aid of IR spectroscopy. The glass produced from the lithium borate gel is compared to both the gel precursor material and a glass of similar composition prepared by conventional techniques. Specifically, the relevant water contents, crystallization behavior, and structural features are contrasted.

Preparation and characterization of novel biocompatible cryogels of poly (vinyl alcohol) and egg-albumin and their water sorption study.

PubMed

Bajpai, A K; Saini, Rajesh

2006-01-01

Polyvinyl alcohol (PVA) and egg albumin are water-soluble, biocompatible and biodegradable polymers and have been widely employed in biomedical fields. In this paper, novel physically cross-linked hydrogels composed of poly (vinyl alcohol) and egg albumin were prepared by cyclic freezing/thawing processes of aqueous solutions containing PVA and egg albumin. The FTIR analysis of prepared cryogels indicated that egg albumin was successfully introduced into the formed hydrogel possibly via hydrogen bonds among hydroxyl groups, amide groups and amino groups present in PVA and egg albumin. The gels were also characterized thermally and morphologically by DSC and SEM-techniques, respectively. The prepared so called 'cryogels' were evaluated for their water uptake potential and influence of various factors such as chemical architecture of the spongy hydrogels, pH and temperature of the swelling bath were investigated on the degree of water sorption by the cryogels. The effect of salt solution and various simulated biological fluids on the swelling of cryogel was also studied. The in vitro biocompatibility of the prepared cryogel was also judged by methods such as protein (BSA) adsorption, blood clot formation and percentage hemolysis measurements.

Preparation and characterization of controlled-release fertilizers coated with marine polysaccharide derivatives

NASA Astrophysics Data System (ADS)

Wang, Jing; Liu, Song; Qin, Yukun; Chen, Xiaolin; Xing, Rong'e.; Yu, Huahua; Li, Kecheng; Li, Pengcheng

2017-09-01

Encapsulation of water-soluble nitrogen fertilizers by membranes can be used to control the release of nutrients to maximize the fertilization effect and reduce environmental pollution. In this research, we formulated a new double-coated controlled-release fertilizer (CRF) by using food-grade microcrystalline wax (MW) and marine polysaccharide derivatives (calcium alginate and chitosan-glutaraldehyde copolymer). The pellets of water-soluble nitrogen fertilizer were coated with the marine polysaccharide derivatives and MW. A convenient and eco-friendly method was used to prepare the CRF. Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the morphology and composition of the products. The nitrogen-release properties were determined in water using UV-Vis spectrophotometry. The controlled-release properties of the fertilizer were improved dramatically after coating with MW and the marine polysaccharide derivatives. The results show that the double-coated CRFs can release nitrogen in a controlled manner, have excellent controlled-release features, and meet the European Standard for CRFs.

Polyacrylamide-hydroxyapatite composite: Preparation, characterization and adsorptive features for uranium and thorium

NASA Astrophysics Data System (ADS)

Baybaş, Demet; Ulusoy, Ulvi

2012-10-01

The composite of synthetically produced hydroxyapatite (HAP) and polyacrylamide was prepared (PAAm-HAP) and characterized by BET, FT-IR, TGA, XRD, SEM and PZC analysis. The adsorptive features of HAP and PAAm-HAP were compared for UO22+ and Th4+. The entrapment of HAP into PAAm-HAP did not change the structure of HAP. Both structures had high affinity to the studied ions. The adsorption capacity of PAAm-HAP was than that of HAP. The adsorption dependence on pH and ionic intensity provided supportive evidences for the effect of complex formation on adsorption process. The adsorption kinetics was well compatible to pseudo second order model. The values of enthalpy and entropy changes were positive. Th4+ adsorption from the leachate obtained from a regional fluorite rock confirmed the selectivity of PAAm-HAP for this ion. In consequence, PAAm-HAP should be considered amongst favorite adsorbents for especially deposition of nuclear waste containing U and Th, and radionuclide at secular equilibrium with these elements.

Preparation and characterization of ZnO/graphene nanocomposite for improved photovoltaic performance

NASA Astrophysics Data System (ADS)

Jayabal, P.; Gayathri, S.; Sasirekha, V.; Mayandi, J.; Ramakrishnan, V.

2014-11-01

Zinc oxide (ZnO) nanoparticles and ZnO/graphene (ZG) nanocomposite were synthesized via simple chemical route and its application as a photoanode for dye-sensitized solar cell (DSSC) was demonstrated. The prepared ZnO and ZG were structurally characterized by X-ray diffraction and micro-Raman techniques. The scanning electron micrograph of ZG revealed the spherical-shaped ZnO nanoparticles of particle size 160 nm was anchored on the two-dimensional graphene sheets. UV-Vis absorption spectroscopy showed that the ZG nanocomposite has enriched visible light absorption. The DSSCs were fabricated using the synthesized ZnO and ZG nanocomposite as photoanode and the effect of low-cost organic dyes on the photovoltaic performances of the solar cells were investigated. Comprehensive performances of ZG are better than that of ZnO-based DSSCs. The ZG DSSCs show power conversion efficiency (PCE) of 1.5 and 0.98 % for RB and EY sensitized electrodes, respectively. Moreover, the ZG dominates in many aspects due to the presence of graphene.

Poly (γ-glutamic acid)/beta-TCP nanocomposites via in situ copolymerization: Preparation and characterization.

PubMed

Shu, Xiu-Lin; Shi, Qing-Shan; Feng, Jin; Yang, Yun-Hua; Zhou, Gang; Li, Wen-Ru

2016-07-01

A series biodegradable poly (γ-glutamic acid)/beta-tricalcium phosphate (γ-PGA/TCP) nanocomposites were prepared which were composed of poly-γ-glutamic acid polymerized in situ with β-tricalcium phosphate and physiochemically characterized as bone graft substitutes. The particle size via dynamic light scattering, the direct morphological characterization via transmission electron microscopy and field emission scanning electron microscope, which showed that γ-PGA and β-TCP were combined compactly at 80℃, and the γ-PGA/TCP nanocomposites had homogenous and nano-sized grains with narrow particle size distributions. The water uptake and retention abilities, in vitro degradation properties, cytotoxicity in the simulated medium, and protein release of these novel γ-PGA/TCP composites were investigated. Cell proliferation in composites was nearly twice than β-TCP when checked in vitro using MC3T3 cell line. We also envision the potential use of γ-PGA/TCP systems in bone growth factor or orthopedic drug delivery applications in future bone tissue engineering applications. These observations suggest that the γ-PGA/TCP are novel nanocomposites with great potential for application in the field of bone tissue engineering. © The Author(s) 2016.

[Preparation and characterization of a polyvinylpyrrolidone water-based magnetic fluid].

PubMed

Xie, Jian-feng; Zhang, Yang-de; Zeng, Zhao-wu; Wang, Xiao-li; Liu, Xing-yan; Zhou, Wei-hua

2008-03-01

To prepare a stable water-based magnetic fluid. A water-based magnetic fluid was prepared by addition of polyvinylpyrrolidone (PVP) as the coating agent for the magnetic particles. After preparation of Fe3O4 by co-precipitation method, PVP was added for its coating, followed by ultrasonic agitation and purification. The magnetic nanoparticles of homogeneously small size and water-based magnetic fluid were obtained, which had good dispersion in water with strong magnetism. PVP can be used as a surfactant to stabilize the magnetic fluid.

13C NMR and XPS characterization of anion adsorbent with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse

NASA Astrophysics Data System (ADS)

Cao, Wei; Wang, Zhenqian; Zeng, Qingling; Shen, Chunhua

2016-12-01

Despite amino groups modified crop straw has been intensively studied as new and low-cost adsorbent for removal of anionic species from water, there is still a lack of clear characterization for amino groups, especially quaternary ammonium groups in the surface of crop straw. In this study, we used 13C NMR and XPS technologies to characterize adsorbents with quaternary ammonium groups prepared from rice straw, corn stalk and sugarcane bagasse. 13C NMR spectra clearly showed the presence of quaternary ammonium groups in lignocelluloses structure of modified crop straw. The increase of nitrogen observed in XPS survey spectra also indicated the existence of quaternary ammonium group in the surface of the adsorbents. The curve fitting of high-resolution XPS N1s and C1s spectra were conducted to probe the composition of nitrogen and carbon contained groups, respectively. The results showed the proportion of quaternary ammonium group significantly increased in the prepared adsorbent's surface that was dominated by methyl/methylene, hydroxyl, quaternary ammonium, ether and carbonyl groups. This study proved that 13C NMR and XPS could be successfully utilized for characterization of quaternary ammonium modified crop straw adsorbents.

Preparation and characterization of TiO2 coated Fe nanofibers for electromagnetic wave absorber.

PubMed

Jang, Dae-Hwan; Song, Hanbok; Lee, Young-In; Lee, Kun-Jae; Kim, Ki Hyeon; Oh, Sung-Tag; Lee, Sang-Kwan; Choa, Yong-Ho

2011-01-01

Recently, electromagnetic interference (EMI) and electromagnetic compatibility (EMC) have become serious problems due to the growth of electronic device and next generation telecommunication. It is necessary to develop new electromagnetic wave absorbing material to overcome the limitation of electromagnetic wave shielding materials. The EMI attenuation is normally related to magnetic loss and dielectric loss. Therefore, magnetic material coating dielectric materials are required in this reason. In this study, TiO2 coated Fe nanofibers were prepared to improve their properties for electromagnetic wave absorption. Poly(vinylpyrrolidone) (PVP) and Iron (III) nitrate nonahydrate (Fe(NO3)3 x 9H2O) were used as starting materials for the synthesis of Fe oxide nanofibers. Fe oxide nanofibers were prepared by electrospinning in an electric field and heat treatment. TiO2 layer was coated on the surface of Fe oxide nanofibers using sol-gel process. After the reduction of TiO2 coated Fe oxide nanofibers, Fe nanofibers with a TiO2 coating layer of about 10 nm were successfully obtained. The morphology and structure of fibers were characterized by SEM, TEM, and XRD. In addition, the absorption properties of TiO2 coated Fe nanofibers were measured by network analyzer.

Preparation, Characterization and Photocatalytic Activity of Ag/TiO2 Nanoparticle Semiconductor Catalysts

NASA Astrophysics Data System (ADS)

Zhang, Yaoyao; Li, Mengyao; Guo, Yinli

2018-01-01

A series of Ag-doped TiO2 powder photocatalysts were prepared by the sol-gel method. The phase structure and morphology of the samples were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The persistent organic pollutant sodium pentachlorophenol ate (PCP-Na) was selected as the target pollutant, and the photocatalytic property of the material Ag/TiO2 was evaluated by PCP-Na degradation rate. It was found that the calcination at 450 °C was conducive to form the anatase structure with high catalytic activity, and the catalytic activity was higher when the silver mole fraction of Ag/TiO2 was 0.50%. The influence of Ag/TiO2 dosage, hydrogen peroxide volume, silver mole fraction and PCP-Na initial concentration was investigated by the single factor experiment.

Synthesis and spectroscopic characterization of gold nanobipyramids prepared by a chemical reduction method

NASA Astrophysics Data System (ADS)

Thanh Ngo, Vo Ke; Phat Huynh, Trong; Giang Nguyen, Dang; Phuong Uyen Nguyen, Hoang; Lam, Quang Vinh; Dat Huynh, Thanh

2015-12-01

Gold nanobipyramids (NBPs) have attracted much attention because they have potential for applications in smart sensing devices, such as medical diagnostic equippments. This is due to the fact that they show more advantageous plasmonic properties than other gold nanostructures. We describe a chemical reduction method for synthesizing NBPs using conventional heating with ascorbic acid reduction and cetyltrimethylamonium bromide (CTAB) + AgNO3 as capping agents. The product was characterized by ultraviolet-visible spectroscopy (UV-vis), Fourier transmission infrared spectroscopy (FTIR), transmission electron microscopy (TEM), x-ray powder diffraction (XRD). The results showed that gold nanoparticles were formed with bipyramid shape (tip-to-tip distance of 88.4 ± 9.4 nm and base length of 29.9 ± 3.2 nm) and face-centered-cubic crystalline structure. Optimum parameters for preparation of NBPs are also found.

Preparation of eugenol-based polyurethane

NASA Astrophysics Data System (ADS)

Li, Yupeng; Luo, Fang; Cheng, Chuanjie

2018-03-01

The regenerative eugenol was used as the starting material to prepare diol species by two steps, with a total yield of 28%. Furthermore, the prepared diol reacts with 1,6-hexadiisocyanate(HDI) to afford the corresponding polyurethane (PU). The structure of intermediates and PU are characterized by 1H-NMR or IR.

Preparation and Characterization of Ni-Doped TiO2 Materials for Photocurrent and Photocatalytic Applications

PubMed Central

Ganesh, Ibram; Gupta, A. K.; Kumar, P. P.; Sekhar, P. S. C.; Radha, K.; Padmanabham, G.; Sundararajan, G.

2012-01-01

Different amounts of Ni-doped TiO2 (Ni = 0.1 to 10%) powders and thin films were prepared by following a conventional coprecipitation and sol-gel dip coating techniques, respectively, at 400 to 800°C, and were thoroughly characterized by means of XRD, FT-IR, FT-Raman, DRS, UV-visible, BET surface area, zeta potential, flat band potential, and photocurrent measurement techniques. Photocatalytic abilities of Ni-doped TiO2 powders were evaluated by means of methylene blue (MB) degradation reaction under simulated solar light. Characterization results suggest that as a dopant, Ni stabilizes TiO2 in the form of anatase phase, reduces its bandgap energy, and adjusts its flat band potentials such that this material can be employed for photoelectrochemical (PEC) oxidation of water reaction. The photocatalytic activity and photocurrent ability of TiO2 have been enhanced by doping of Ni in TiO2. The kinetic studies revealed that the MB degradation reaction follows the Langmuir-Hinshelwood first-order reaction relationship. PMID:22619580

A novel smart injectable hydrogel prepared by microbial transglutaminase and human-like collagen: Its characterization and biocompatibility.

PubMed

Zhao, Leilei; Li, Xian; Zhao, Jiaqi; Ma, Saijian; Ma, Xiaoxuan; Fan, Daidi; Zhu, Chenhui; Liu, Yannan

2016-11-01

Various tissue scaffold materials are increasingly used to repair skin defects by cross-linking because of the ability to fill and implant in any form via operation. However, crosslinker residues cannot be easily removed from scaffold materials prepared by chemical crosslinking methods, limiting their use for skin tissue engineering. Here, microbial transglutaminase (MTGase), a nontoxic crosslinker with high specific activity and reaction rate under mild conditions, was employed crosslinks in human-like collagen (HLC) to yield novel smart MTGase crosslinked with human-like collagen (MTGH) hydrogels, which are sensitive to temperature and/or enzymes. Various ratios of MTGase/HLC were performed, and their physicochemical properties were characterized, including the swelling ratio, the elastic modulus, the morphology and the porosity. The degradation behavior and mechanism of MTGase in concentration-dependent manner involved in formation hydrogels were identifying in vitro. The cell attachment in vitro and biocompatibility in vivo were also investigated. The results demonstrated that the use of different concentrations of MTGase to crosslink HLC produced products with different degradation times and biocompatibilities. The 50U/g MTGase-prepared MTGH hydrogels had a higher density of crosslinks, which made them more resistant to degradation by collagenase I and collagenase II. However, 40U/g MTGase-prepared MTGH hydrogels were more suitable for cell attachment. In addition, compared with the Collagen Implant I® (SUM) used in animal experiments, the 40U/g MTGase-prepared MTGH hydrogels had a lower toxicity and better biocompatibility. Therefore, 40U/g MTGase crosslinked with HLC should be used to prepare MTGH hydrogels for potential application as soft materials for skin tissue engineering. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation, Processing, and Characterization of Oriented Polycrystalline Zeolite and Aluminophosphate Membranes

NASA Astrophysics Data System (ADS)

Stoeger, Jared Andrew

Since the advent of zeolite membranes, speculation on their industrial applicability has been closely monitored, although widespread commercialization has been hampered by limitations in fabrication and post-synthesis processing. Economical, energy-efficient technology breakthroughs require an evaluation of a range of material candidates which show robustness and reliability. Straightforward manufacturing techniques should be devised to generate thousands of square meters of membrane area; however, this demands control of structural characteristics on the scale of nanometers. As described in this dissertation, the path forward will be forged by exploiting the intrinsic crystalline properties of zeolites or aluminophosphates for the next advancement in membrane technology. A facile method is described for the preparation of silicalite-1 (MFI zeolite type) membranes using the secondary growth technique on symmetric porous stainless steel tubes. Activation through rapid thermal processing (RTP), a lamp-based heat-treatment process used as a critical fabrication step in silicon integrated circuit manufacturing, is proven to reduce the density of non-zeolitic transport pathways which are detrimental to high-resolution molecular sieving. RTP-treated membranes are shown to have enhanced performance in the binary separation of vapor-phase isomers (p-/o-xylene), gas-phase isomers (n-/i-butane), and alcohol/water when compared to membranes activated at a much slower heating rate but otherwise similarly-prepared. The performance is discussed in the context of the market potential for industrially-attractive separations: the recovery of p-xylene from an isomeric mixture or alcohol biofuels from aqueous post-fermentation streams. Hydrothermal growth techniques for the preparation and characterization of continuous aluminophosphate (AFI zeolite type) membranes with a preferential crystallographic alignment on porous alpha-Al2O3 disc supports are demonstrated. A mechanism is

Preparation and characterization of photoactive composite kaolinite/TiO(2).

PubMed

Mamulová Kutláková, K; Tokarský, J; Kovář, P; Vojtěšková, S; Kovářová, A; Smetana, B; Kukutschová, J; Čapková, P; Matějka, V

2011-04-15

Preparation of nanocomposite kaolinite/TiO(2), using hydrolysis of titanyl sulfate in the presence of kaolin was addressed. A variable (kaolin)/(titanyl sulfate) ratio has been used in order to achieve the desired TiO(2) content in prepared nanocomposites. Calcination of the composites at 600 °C led to the transformation of the kaolinite to metakaolinite and to origination of metakaolinite/TiO(2) composites. The prepared samples were investigated using X-ray fluorescence spectroscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetry and diffuse reflectance spectroscopy in the UV-VIS region. Structural ordering of TiO(2) on the kaolinite particle surface was modeled using empirical force field atomistic simulations in the Material Studio modeling environment. Photodegradation activity of the composites prepared was evaluated by the discoloration of Acid Orange 7 aqueous solution. Copyright © 2011 Elsevier B.V. All rights reserved.

Preparation, characterization and conductivity study of nitro-mercurated styrene butadiene rubber/silver doped zinc oxide nanocomposites

NASA Astrophysics Data System (ADS)

Anilkumar, T.; Naik, Adarsh Ajith; Ramesan, M. T.

2017-06-01

Here we report the preparation of nitromercurated styrene butadiene rubber (NMSBR)/silver doped zinc oxide nanocomposite by inexpensive and ecofriendly two roll mill mixing. The composites were characterized by UV, FTIR, XRD, SEM, TGA and conductivity measurements. UV and FTIR spectrum indicated the interfacial interaction between the polymer and nanoparticles.XRD and SEM images showed the uniform arrangement of nanoparticles within the macromolecular chain. TGA study indicated the better thermal resistance of the composite. The dielectric properties and AC conductivity ofnanocomposites were much greater than nitromercurated SBR and they may be used as multifunctional materials for nanoelectronic devices.

Structural Rearrangement of Au-Pd Nanoparticles under Reaction Conditions: An ab Initio Molecular Dynamics Study.

PubMed

Xu, Cong-Qiao; Lee, Mal-Soon; Wang, Yang-Gang; Cantu, David C; Li, Jun; Glezakou, Vassiliki-Alexandra; Rousseau, Roger

2017-02-28

The structure, composition, and atomic distribution of nanoalloys under operating conditions are of significant importance for their catalytic activity. In the present work, we use ab initio molecular dynamics simulations to understand the structural behavior of Au-Pd nanoalloys supported on rutile TiO 2 under different conditions. We find that the Au-Pd structure is strongly dependent on the redox properties of the support, originating from strong metal-support interactions. Under reducing conditions, Pd atoms are inclined to move toward the metal/oxide interface, as indicated by a significant increase of Pd-Ti bonds. This could be attributed to the charge localization at the interface that leads to Coulomb attractions to positively charged Pd atoms. In contrast, under oxidizing conditions, Pd atoms would rather stay inside or on the exterior of the nanoparticle. Moreover, Pd atoms on the alloy surface can be stabilized by hydrogen adsorption, forming Pd-H bonds, which are stronger than Au-H bonds. Our work offers critical insights into the structure and redox properties of Au-Pd nanoalloy catalysts under working conditions.

Synthesis and characterization of zeolites prepared from industrial fly ash.

PubMed

Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

2014-09-01

In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm(3) of 5 mol · dm(-3) NaOH + 0.4 dm(3) of 3 mol · dm(-3) NaCl, 95 °C). As synthesized materials were characterized to obtain mineral composition (X-ray diffractometry, Scanning electron microscopy-energy dispersive spectrometry), adsorption properties (Brunauer-Emmett-Teller surface area, N2 isotherm adsorption/desorption), and ion exchange capacity. The most effective reaction for zeolite preparation was when sodalite was formed and the quantitative content of zeolite from X-ray diffractometry was 90 wt%, compared with 70 wt% for the Na-X and 75 wt% for the Na-P1. Residues from each synthesis reaction were the following: mullite, quartz, and the remains of amorphous aluminosilicate glass. The best zeolitic material as characterized by highest specific surface area was Na-X at almost 166 m(2) · g(-1), while for the Na-P1 and sodalite it was 71 and 33 m(2) · g(-1), respectively. The ion exchange capacity decreased in the following order: Na-X at 1.8 meq · g(-1), Na-P1 at 0.72 meq · g(-1), and sodalite at 0.56 meq · g(-1). The resulting zeolites are competitive for commercially available materials and are used as ion exchangers in industrial wastewater and soil decontamination.

Preparation, physical characterization, and stability of Ferrous-Chitosan microcapsules using different iron sources

NASA Astrophysics Data System (ADS)

Handayani, Noer Abyor; Luthfansyah, M.; Krisanti, Elsa; Kartohardjono, Sutrasno; Mulia, Kamarza

2017-11-01

Dietary modification, supplementation and food fortification are common strategies to alleviate iron deficiencies. Fortification of food is an effective long-term approach to improve iron status of populations. Fortification by adding iron directly to food will cause sensory problems and decrease its bioavailability. The purpose of iron encapsulation is: (1) to improve iron bioavailability, by preventing oxidation and contact with inhibitors and competitors; and (2) to disguise the rancid aroma and flavor of iron. A microcapsule formulation of two suitable iron compounds (iron II fumarate and iron II gluconate) using chitosan as a biodegradable polymer will be very important. Freeze dryer was also used for completing the iron microencapsulation process. The main objective of the present study was to prepare and characterize the iron-chitosan microcapsules. Physical characterization, i.e. encapsulation efficiency, iron loading capacity, and SEM, were also discussed in this paper. The stability of microencapsulated iron under simulated gastrointestinal conditions was also investigated, as well. Both iron sources were highly encapsulated, ranging from 71.5% to 98.5%. Furthermore, the highest ferrous fumarate and ferrous gluconate loaded were 1.9% and 4.8%, respectively. About 1.04% to 9.17% and 45.17% to 75.19% of Fe II and total Fe, were released in simulated gastric fluid for two hours and in simulated intestinal fluid for six hours, respectively.

Preparation and Characterization of Myosin Proteins.

ERIC Educational Resources Information Center

Caldwell, Elizabeth; Eftink, Maurice R.

1985-01-01

Students complete five experimental projects at the end of a senior-level biochemistry course which involves the isolation and characterization of myosin and its water-soluble subfragments. Procedures used and results obtained are provided for such projects as viscosity and ATPase measurements and gel electrophoresis experiments. (JN)

Preparation and Preliminary Characterization of Crystallizing Fluorescent Derivatives of Chicken Egg White Lysozyme

NASA Technical Reports Server (NTRS)

Sumida, John; Forsythe, Elizabeth L.; Pusey, Marc L.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

Fluorescence is one of the most versatile and powerful tools for the study of macromolecules. While most proteins are intrinsically fluorescent, working at crystallization concentrations require the use of covalently prepared derivatives added as tracers. This approach requires derivatives that do not markedly affect the crystal packing. We have prepared fluorescent derivatives of chicken egg white lysozyme with probes bound to one of two different sites on the protein molecule. Lucifer yellow and 5-(2-aminoethyl)aminonapthalene-1-sulfonic acid (EDANS) have been attached to the side chain carboxyl of Asp(sup 101) using a carbodiimide coupling procedure. Asp(sup 101) lies within the active site cleft, and it is believed that the probes are "buried" within that cleft. Lucifer yellow and MANS probes with iodoacetamide reactive groups have been bound to His(sup 15), located on the "back side" of the molecule relative to the active site. All the derivatives fluoresce in the solution and the crystalline states. Fluorescence characterization has focused on determination of binding effects on the probe quantum yield, lifetime, absorption and emission spectra, and quenching by added solutes. Quenching studies show that, as postulated, the Asp(sup 101)-bound probes are partially sheltered from the bulk solution by their location within the active site cleft. Probes bound to His(sup 15) have quenching constants about equal to those for the free probes, indicating that this site is highly exposed to the bulk solution.

Preparation and Preliminary Characterization of Crystallizing Fluorescent Derivatives of Chicken Egg White Lysozyme

NASA Technical Reports Server (NTRS)

Sumida, John P.; Forsythe, Elizabeth L.; Pusey, Marc L.

2001-01-01

Fluorescence is one of the most versatile and powerful tools for the study of macromolecules. While most proteins are intrinsically fluorescent, working at crystallization concentrations require the use of covalently prepared derivatives added as tracers. This approach requires derivatives that do not markedly affect the crystal packing. We have prepared fluorescent derivatives of chicken egg white lysozyme with probes bound to one of two different sites on the protein molecule. Lucifer yellow and 5-(2-aminoethyl)aminonapthalene-i-sulfonic acid (EDANS) have been attached to the side chain carboxyl of Asp(sup 101) using a carbodiimide coupling procedure. Asp(sup 101) lies within the active site cleft, and it is believed that the probes are 'buried' within that cleft. Lucifer yellow and MANS probes with iodoacetamide reactive five groups have been bound to His(sup 15), located on the 'back side' of the molecule relative to the active site. All the derivatives fluoresce in the solution and the crystalline states. Fluorescence characterization has focused on determination of binding effects on the probe quantum yield, lifetime, absorption and emission spectra, and quenching by added solutes. Quenching studies show that, as postulated, the Asp(sup 101)-bound probes are partially sheltered from the bulk solution by their location within the active site cleft. Probes bound to His(sup 15) have quenching constants about equal to those for the free probes, indicating that this site is highly exposed to the bulk solution.

Preparation and preliminary characterization of crystallizing fluorescent derivatives of chicken egg white lysozyme

NASA Astrophysics Data System (ADS)

Sumida, John P.; Forsythe, Elizabeth L.; Pusey, Marc L.

2001-11-01

Fluorescence is one of the most versatile and powerful tools for the study of macromolecules. While most proteins are intrinsically fluorescent, working at crystallization concentrations require the use of covalently prepared derivatives added as tracers. This approach requires derivatives that do not markedly affect the crystal packing. We have prepared fluorescent derivatives of chicken egg white lysozyme with probes bound to one of two different sites on the protein molecule. Lucifer yellow and 5-(2-aminoethyl)aminonapthalene-1-sulfonic acid (EDANS) have been attached to the side chain carboxyl of Asp 101 using a carbodiimide coupling procedure. Asp 101 lies within the active site cleft, and it is believed that the probes are "buried" within that cleft. Lucifer yellow and EDANS probes with iodoacetamide reactive groups have been bound to His 15, located on the "back side" of the molecule relative to the active site. All the derivatives fluoresce in the solution and the crystalline states. Fluorescence characterization has focused on determination of binding effects on the probe quantum yield, lifetime, absorption and emission spectra, and quenching by added solutes. Quenching studies show that, as postulated, the Asp 101-bound probes are partially sheltered from the bulk solution by their location within the active site cleft. Probes bound to His 15 have quenching constants about equal to those for the free probes, indicating that this site is highly exposed to the bulk solution.

Efficient Pb(II) removal using sodium alginate-carboxymethyl cellulose gel beads: Preparation, characterization, and adsorption mechanism.

PubMed

Ren, Huixue; Gao, Zhimin; Wu, Daoji; Jiang, Jiahui; Sun, Youmin; Luo, Congwei

2016-02-10

Alginate-carboxymethyl cellulose (CMC) gel beads were prepared in this study using sodium alginate (SA) and sodium CMC through blending and cross-linking. The specific surface area and aperture of the prepared SA-CMC gel beads were tested. The SA-CMC structure was characterized and analyzed via infrared spectroscopy, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. Static adsorption experiment demonstrated that Pb(II) adsorption of SA-CMC exceeded 99% under the optimized conditions. In addition, experiments conducted under the same experimental conditions showed that the lead ion removal efficiency of SA-CMC was significantly higher than that of conventional adsorbents. The Pb(II) adsorption process of SA-CMC followed the Langmuir adsorption isotherm, and the dynamic adsorption model could be described through a pseudo-second-order rate equation. Pb(II) removal mechanisms of SA-CMC, including physical, chemical, and electrostatic adsorptions, were discussed based on microstructure analysis and adsorption kinetics. Chemical adsorption was the main adsorption method among these mechanisms. Copyright © 2015 Elsevier Ltd. All rights reserved.

Characterization and evaluation of 5-fluorouracil-loaded solid lipid nanoparticles prepared via a temperature-modulated solidification technique.

PubMed

Patel, Meghavi N; Lakkadwala, Sushant; Majrad, Mohamed S; Injeti, Elisha R; Gollmer, Steven M; Shah, Zahoor A; Boddu, Sai Hanuman Sagar; Nesamony, Jerry

2014-12-01

The aim of this research was to advance solid lipid nanoparticle (SLN) preparation methodology by preparing glyceryl monostearate (GMS) nanoparticles using a temperature-modulated solidification process. The technique was reproducible and prepared nanoparticles without the need of organic solvents. An anticancer agent, 5-fluorouracil (5-FU), was incorporated in the SLNs. The SLNs were characterized by particle size analysis, zeta potential analysis, differential scanning calorimetry (DSC), infrared spectroscopy, atomic force microscopy (AFM), transmission electron microscopy (TEM), drug encapsulation efficiency, in vitro drug release, and in vitro cell viability studies. Particle size of the SLN dispersion was below 100 nm, and that of redispersed lyophilizates was ~500 nm. DSC and infrared spectroscopy suggested that the degree of crystallinity did not decrease appreciably when compared to GMS. TEM and AFM images showed well-defined spherical to oval particles. The drug encapsulation efficiency was found to be approximately 46%. In vitro drug release studies showed that 80% of the encapsulated drug was released within 1 h. In vitro cell cultures were biocompatible with blank SLNs but demonstrated concentration-dependent changes in cell viability to 5-FU-loaded SLNs. The 5-FU-loaded SLNs can potentially be utilized in an anticancer drug delivery system.

Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes

DOE PAGES

Balasekaran, Samundeeswari Mariappan; Sattelberger, Alfred P.; Hagenbach, Adelheid; ...

2017-12-08

Quadruply bonded rhenium(III) dimers with the stoichiometry Re 2L 4F 2 (1, L = hexahydro-2H-pyrimido[1,2a]pyrimidinate (hpp –); 2, L = diphenyl formamidinate (dpf –)) were prepared from the solid-state melt reactions (SSMRs) between (NH 4) 2[Re 2F 8]·2H 2O and HL. Then those compounds were characterized in the solid state by single-crystal X-ray diffraction and in solution by UV–visible spectroscopy and cyclic voltammetry. The compound [Re 2(hpp) 4F 2]PF 6 (3) was prepared from the one-electron oxidation of Re 2(hpp) 4F 2 with [Cp 2Fe]PF 6. Compounds 1–3 are isostructural with the corresponding chloro derivatives. In summation, compound 1 undergoesmore » two one-electron oxidations. Comparison with its higher halogen homologues reveals that Re 2(hpp) 4F 2 (1) is more easily oxidized than its chloro and bromo analogues.« less

Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes

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

Balasekaran, Samundeeswari Mariappan; Sattelberger, Alfred P.; Hagenbach, Adelheid

Quadruply bonded rhenium(III) dimers with the stoichiometry Re 2L 4F 2 (1, L = hexahydro-2H-pyrimido[1,2a]pyrimidinate (hpp –); 2, L = diphenyl formamidinate (dpf –)) were prepared from the solid-state melt reactions (SSMRs) between (NH 4) 2[Re 2F 8]·2H 2O and HL. Then those compounds were characterized in the solid state by single-crystal X-ray diffraction and in solution by UV–visible spectroscopy and cyclic voltammetry. The compound [Re 2(hpp) 4F 2]PF 6 (3) was prepared from the one-electron oxidation of Re 2(hpp) 4F 2 with [Cp 2Fe]PF 6. Compounds 1–3 are isostructural with the corresponding chloro derivatives. In summation, compound 1 undergoesmore » two one-electron oxidations. Comparison with its higher halogen homologues reveals that Re 2(hpp) 4F 2 (1) is more easily oxidized than its chloro and bromo analogues.« less

21 CFR 184.1148 - Bacterially-derived carbohydrase enzyme preparation.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Bacterially-derived carbohydrase enzyme preparation... carbohydrase enzyme preparation. (a) Bacterially-derived carbohydrase enzyme preparation is obtained from the... Bacillus subtilis or B. amyloliquefaciens. The preparation is characterized by the presence of the enzymes...

Preparation and characterization of RuO2/polypyrrole electrodes for supercapacitors

NASA Astrophysics Data System (ADS)

Li, Xiang; Wu, Yujiao; Zheng, Feng; Ling, Min; Lu, Fanghai

2014-11-01

Polypyrrole (PPy) embedded RuO2 electrodes were prepared by the composite method. Precursor solution of RuO2 was coated on tantalum sheet and annealed at 260 °C for 2.5 h to develop a thin film. PPy particles were deposited on RuO2 films and dried at 80 °C for 12 h to form composite electrode. Microstructure and morphology of RuO2/PPy electrode were characterized using Fourier transform infrared spectrometer, X-ray diffraction and scanning electron microscopy, respectively. Our results confirmed that counter ions are incorporated into RuO2 matrix. Structure of the composite with amorphous phase was verified by X-ray diffraction. Analysis by scanning electron microscopy reveals that during grain growth of RuO2/PPy, PPy particle size sharply increases as deposition time is over 20 min. Electrochemical properties of RuO2/PPy electrode were calculated using cyclic voltammetry. As deposition times of PPy are 10, 20, 25 and 30 min, specific capacitances of composite electrodes reach 657, 553, 471 and 396 F g-1, respectively. Cyclic behaviors of RuO2/PPy composite electrodes are stable.

Preparation and characterization of biocompatible silver nanoparticles using pomegranate peel extract.

PubMed

Nasiriboroumand, Majid; Montazer, Majid; Barani, Hossein

2018-02-01

The potential application of any nanoparticles, including silver nanoparticles (AgNPs), strongly depends on their stability against aggregation. In the current study, an aqueous extract of pomegranate peel was used as a stabilizer during synthesis of AgNPs. Nanoparticles have been prepared by the chemical reduction method from an aqueous solution of silver nitrate in the presence of sodium borohydride as a reducing agent. The AgNPs were characterized by dynamic light scattering (DLS), zeta-potential measurements, UV-Vis spectroscopy and transmission electron microscopy (TEM). The antibacterial efficiency of AgNPs against Escherichia coli was investigated. The size, polydispersity index, FWHM, and colloidal stability of nanoparticles in dispersion depends on the extract concentrations. In the presence of pomegranate peel extract, the nanoparticles suspension shows colloidal stability at least for a week. Our studies show that synthesized AgNPs with the above described procedure were stable at pH = 3-12 and in the temperature range of 25-85 °C. Additionally, AgNPs exhibit antibacterial properties, especially at the lowest amount of extract to silver ratio (K Extract/Ag ). Copyright © 2018. Published by Elsevier B.V.

Bottom-up strategies for the assembling of magnetic systems using nanoclusters

NASA Astrophysics Data System (ADS)

Dupuis, V.; Hillion, A.; Robert, A.; Loiselet, O.; Khadra, G.; Capiod, P.; Albin, C.; Boisron, O.; Le Roy, D.; Bardotti, L.; Tournus, F.; Tamion, A.

2018-05-01

In the frame of the 20th Anniversary of the Journal of Nanoparticle Research (JNR), our aim is to start from the historical context 20 years ago and to give some recent results and perspectives concerning nanomagnets prepared from clusters preformed in the gas phase using the low-energy cluster beam deposition (LECBD) technique. In this paper, we focus our attention on the typical case of Co clusters embedded in various matrices to study interface magnetic anisotropy and magnetic interactions as a function of volume concentrations, and on still current and perspectives through two examples of binary metallic 3d-5d TM (namely CoPt and FeAu) cluster assemblies to illustrate size-related and nanoalloy phenomena on magnetic properties in well-defined mass-selected clusters. The structural and magnetic properties of these cluster assemblies were investigated using various experimental techniques that include high-resolution transmission electron microscopy (HRTEM), superconducting quantum interference device (SQUID) magnetometry, and synchrotron techniques such as extended X-ray absorption fine structure (EXAFS) and X-ray magnetic circular dichroism (XMCD). Depending on the chemical nature of both NPs and matrix, we observe different magnetic responses compared to their bulk counterparts. In particular, we show how finite size effects (size reduction) enhance their magnetic moment and how specific relaxation in nanoalloys can impact their magnetic anisotropy.

Structural Characterization of Melanin Pigments from Commercial Preparations of the Edible Mushroom Auricularia auricula

PubMed Central

Prados-Rosales, Rafael; Toriola, Stacy; Nakouzi, Antonio; Chatterjee, Subhasish; Stark, Ruth; Gerfen, Gary; Tumpowsky, Paul; Dadachova, Ekaterina; Casadevall, Arturo

2016-01-01

Many of the most widely consumed edible mushrooms are pigmented, and these have been associated with some beneficial health effects. Nevertheless, the majority of the reported compounds associated with these desirable properties are non-pigmented. We have previously reported that melanin pigment from the edible mushroom Auricularia auricula can protect mice against ionizing radiation, although no physicochemical characterization was reported. Consequently, in this study we have characterized commercial A. auricula mushroom preparations for melanin content and carried out structural characterization of isolated insoluble melanin materials using a panel of sophisticated spectroscopic and physical/imaging techniques. Our results show that approximately 10% of the dry mass of A. auricula is melanin and that the pigment has physicochemical properties consistent with those of eumelanins, including hosting a stable free radical population. Electron microscopy studies show that melanin is associated with the mushroom cell wall in a manner similar to that of melanin from the model fungus C. neoformans. Elemental analysis of melanin indicated C, H, and N ratios consistent with 5,6-dihydroxyindole-2-carboxylic acid/5,6-dihydroxyindole and 1,8-dihydroxynaphthalene eumelanin. Validation of the identity of the isolated product as melanin was achieved by EPR analysis. A. auricula melanin manifested structural differences, relative to the C. neoformans melanin, with regard to the variable proportions of alkyl chains or oxygenated carbons. Given the necessity for new oral and inexpensive radioprotective materials coupled with the commercial availability of A. auricula mushrooms, this product may represent an excellent source of edible melanin. PMID:26244793

Preparation and characterization of α-Al2O3 film by low temperature thermal oxidation of Al8Cr5 coating

NASA Astrophysics Data System (ADS)

Zhang, Min; Xu, Bajin; Ling, Guoping

2015-03-01

In this paper, α-Al2O3 film was prepared by low temperature thermal oxidation of Al8Cr5 coating. The Al8Cr5 alloy coating was prepared on SUS430 stainless steel through a two-step approach including electrodepositing Cr/Al composite coating and subsequent heat treatment at 740 °C for 16 h. After mechanical polishing removal of voids on the surface, the Al8Cr5 coating was thermal oxidized at 720 °C in argon for 100 h. The samples were characterized by SEM, EDX, XRD, XPS and TEM. XPS detection on the surface of oxidized Al8Cr5 coating showed that the oxide film mainly consisted of Al2O3. TEM characterization of the oxide film showed that it was α-Al2O3 films ca. 110 nm. The formation of α-Al2O3 films at low temperature can be attributed to the formation of Cr2O3 nuclei at the initial stage of oxidation which lowers the nucleation energy barrier of α-Al2O3.

Glycan characterization of the NIST RM monoclonal antibody using a total analytical solution: From sample preparation to data analysis.

PubMed

Hilliard, Mark; Alley, William R; McManus, Ciara A; Yu, Ying Qing; Hallinan, Sinead; Gebler, John; Rudd, Pauline M

Glycosylation is an important attribute of biopharmaceutical products to monitor from development through production. However, glycosylation analysis has traditionally been a time-consuming process with long sample preparation protocols and manual interpretation of the data. To address the challenges associated with glycan analysis, we developed a streamlined analytical solution that covers the entire process from sample preparation to data analysis. In this communication, we describe the complete analytical solution that begins with a simplified and fast N-linked glycan sample preparation protocol that can be completed in less than 1 hr. The sample preparation includes labelling with RapiFluor-MS tag to improve both fluorescence (FLR) and mass spectral (MS) sensitivities. Following HILIC-UPLC/FLR/MS analyses, the data are processed and a library search based on glucose units has been included to expedite the task of structural assignment. We then applied this total analytical solution to characterize the glycosylation of the NIST Reference Material mAb 8761. For this glycoprotein, we confidently identified 35 N-linked glycans and all three major classes, high mannose, complex, and hybrid, were present. The majority of the glycans were neutral and fucosylated; glycans featuring N-glycolylneuraminic acid and those with two galactoses connected via an α1,3-linkage were also identified.

Structural and Spectral Characterization of Co2+- and Ni2+-DOPED CdO Powder Prepared From Solution at Room Temperature

NASA Astrophysics Data System (ADS)

Reddy, C. V.; Rao, L. V. Krishna; Satish, D. V.; Shim, J.; Ravikumar, R. V. S. S. N.

2015-11-01

The mild and simple solution method was used for the synthesis of Co2+- and Ni2+-doped CdO powders at room temperature. The prepared powders were characterized using powder X-ray diffraction, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), optical absorption, and Fourier transform infrared spectroscopy (FTIR). From the powder X-ray diffraction patterns, it has been observed that the prepared Co2+ and Ni2+ ion-doped CdO powders belong to the cubic phase, and the evaluated average crystalline sizes of the powders are 20 and 14 nm, respectively. The SEM images and the EDS spectra show that the prepared powders are distributed over different sizes in the grain boundaries. Optical absorption studies allow determination of site symmetry of the metal ion with its ligands. The crystal field (Dq) and inter-electronic repulsion (B and C) parameters have been evaluated from the optical absorption spectra. The FTIR spectra show the characteristic fundamental vibrations of the metal oxide and CdO.

[Preparation of panax notoginseng saponins-tanshinone H(A) composite method for pulmonary delivery with spray-drying method and its characterization].

PubMed

Wang, Hua-Mei; Fu, Ting-Ming; Guo, Li-Wei

2013-02-01

To prepare panax notoginseng saponins-tanshinone II(A) composite particles for pulmonary delivery, in order to explore a dry powder particle preparation method ensuring synchronized arrival of multiple components of traditional Chinese medicine compounds at absorption sites. Panax notoginseng saponins-tanshinone II(A) composite particles were prepared with spray-drying method, and characterized by scanning electron microscopy (SEM), confocal laser scanning microscope (CLSM), X-ray diffraction (XRD), infrared analysis (IR), dry laser particle size analysis, high performance liquid chromatography (HPLC) and the aerodynamic behavior was evaluated by a Next Generation Impactor (NGI). The dry powder particles produced had narrow particle size distribution range and good aerodynamic behavior, and could realize synchronized administration of multiple components. The spray-drying method is used to combine traditional Chinese medicine components with different physical and chemical properties in the same particle, and product into traditional Chinese medicine compound particles in line with the requirements for pulmonary delivery.

Preparation, characterization and application of novel proton conducting ceramics

NASA Astrophysics Data System (ADS)

Wang, Siwei

Due to the immediate energy shortage and the requirement of environment protection nowadays, the efficient, effective and environmental friendly use of current energy sources is urgent. Energy conversion and storage is thus an important focus both for industry and academia. As one of the hydrogen energy related materials, proton conducting ceramics can be applied in solid oxide fuel cells and steam electrolysers, as well as high temperature hydrogen separation membranes and hydrogen sensors. For most of the practical applications, both high proton conductivity and chemical stability are desirable. However, the state-of-the-art proton conducting ceramics are facing great challenges in simultaneously fulfilling conductivity and stability requirements for practical applications. Consequently, understanding the properties for the proton conducting ceramics and developing novel materials that possess both high proton conductivity and enhanced chemical stability have both scientific and practical significances. The objective of this study is to develop novel proton conducting ceramics, either by evaluating the doping effects on the state-of-the-art simple perovskite structured barium cerates, or by investigating novel complex perovskite structured Ba3Ca1.18Nb1.82O 9-delta based proton conductors as potential proton conducting ceramics with improved proton conductivity and enhanced chemical stability. Different preparation methods were compared, and their influence on the structure, including the bulk and grain boundary environment has been investigated. In addition, the effects of microstructure on the electrical properties of the proton conducting ceramics have also been characterized. The solid oxide fuel cell application for the proton conducting ceramics performed as electrolyte membranes has been demonstrated.

Preparation, characterization and toxicology properties of α- and β-chitosan Maillard reaction products nanoparticles.

PubMed

Zhang, Hongcai; Zhang, Yiwen; Bao, Erjaing; Zhao, Yanyun

2016-08-01

In this study, β-chitosan (CS) Maillard reaction (MR) NPs was prepared to improve the water solubility of CS NPs. The α- and β-CS MR was firstly induced by high intensity ultrasound-assisted (UA) water-bath heating at 80°C for 8h. The α- and β-CS Maillard reaction products (MRPs NPs were then prepared by ionic gelation method between the positively charged primary amino groups of CS and the negatively charged groups of sodium tripolyphosphate (TPP). The α- and β-CS MRPs NPs had particle size of 42.49 and 61.74nm, and Zeta-potential of 27.43 and 35.13mV, respectively. The prepared α- and β-CS MRPs NPs was characterized by transmission electron microscope (TEM), Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and thermogravimetric analysis (TGA)-differential scanning calorimetry (DSC) to verify whether α- and β-CS MRPs has been incorporated into the CS NPs. The α- and β-CS MRPs NPs exhibited no significant difference (p>0.05) in antioxidant activity compared with α- and β-CS MRPs at the same concentration based on reducing power, DPPH radical scavenging activity, and ORAC values. The cytotoxicity test of α- and β-CS MRPs NPs showed good cell viability (70.86-99.16%) of human pulmonary microvascular endothelial cells (HLMVEC) at the concentration range from 0.12 to 1mg/mL, and fluorescein-5-isothiocyanate (FITC)-α- and β-CS MRPs NPs maintained the morphological characteristics of living cells. These results showed that α- and β-CS MRPs NPs can be used as water-soluble antioxidant substances for applications in food and other fields. Copyright © 2016. Published by Elsevier B.V.

Preparation and characterization of cellulose-based foams via microwave curing

PubMed Central

Demitri, Christian; Giuri, Antonella; Raucci, Maria Grazia; Giugliano, Daniela; Madaghiele, Marta; Sannino, Alessandro; Ambrosio, Luigi

2014-01-01

In this work, a mixture of a sodium salt of carboxymethylcellulose (CMCNa) and polyethylene glycol diacrylate (PEGDA700) was used for the preparation of a microporous structure by using the combination of two different procedures. First, physical foaming was induced using Pluronic as a blowing agent, followed by a chemical stabilization. This second step was carried out by means of an azobis(2-methylpropionamidine)dihydrochloride as the thermoinitiator (TI). This reaction was activated by heating the sample homogeneously using a microwave generator. Finally, the influence of different CMCNa and PEGDA700 ratios on the final properties of the foams was investigated. The viscosity, water absorption capacity, elastic modulus and porous structure were evaluated for each sample. In addition, preliminary biological characterization was carried out with the aim to prove the biocompatibility of the resulting material. The foam, including 20% of PEGDA700 in the mixture, demonstrated higher viscosity and stability before thermo-polymerization. In addition, increased water absorption capacity, mechanical resistance and a more uniform microporous structure were obtained for this sample. In particular, foam with 3% of CMCNa shows a hierarchical structure with open pores of different sizes. This morphology increased the properties of the foams. The full set of samples demonstrated an excellent biocompatibility profile with a good cell proliferation rate of more than 7 days. PMID:24501679

Differential processing of the two subunits of human choriogonadotropin (hCG) by granulosa cells. I. Preparation and characterization of selectively labeled hCG

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

Landefeld, T.D.; Byrne, M.D.; Campbell, K.L.

1981-12-01

The alpha- and beta-subunits of hCG were radioiodinated and recombined with unlabeled complementary subunits. The resultant recombined hormones, selectively labeled in either the alpha- or beta-subunit, were separated from unrecombined subunit by sodium dodecyl sulfate-polyacrylamide gel electrophoresis, extracted with Triton X-100, and characterized by binding analysis. The estimates of maximum binding (active fraction) of the two resultant selectively labeled, recombined hCG preparations, determined with excess receptor were 0.41 and 0.59. These values are similar to those obtained when hCG is labeled as an intact molecule. The specific activities of the recombined preparations were estimated by four different methods, and themore » resulting values were used in combination with the active fraction estimates to determine the concentrations of active free and bound hormone. Binding analyses were run using varying concentrations of both labeled and unlabeled hormone. Estimates of the equilibrium dissociation binding constant (Kd) and receptor capacity were calculated in three different ways. The mean estimates of capacity (52.6 and 52.7 fmol/mg tissue) and Kd (66.6 and 65.7 pM) for the two preparations were indistinguishable. Additionally, these values were similar to values reported previously for hCG radioiodinated as an intact molecule. The availability of well characterized, selectively labeled hCG preparations provides new tools for studying the mechanism of action and the target cell processing of the subunits of this hormone.« less

Preparation and characterization of injectable fibrillar type I collagen and evaluation for pseudoaneurysm treatment in a pig model.

PubMed

Geutjes, Paul J; van der Vliet, J Adam; Faraj, Kaeuis A; de Vries, Noes; van Moerkerk, Herman T B; Wismans, Ronnie G; Hendriks, Thijs; Daamen, Willeke F; van Kuppevelt, Toin H

2010-11-01

Despite the efficacy of collagen in femoral artery pseudoaneurysm treatment, as reported in one patient study, its use has not yet gained wide acceptance in clinical practice. In this particular study, the collagen was not described in detail. To further investigate the potential of collagen preparations, we prepared and characterized highly purified injectable fibrillar type I collagen and evaluated its use for femoral artery pseudoaneurysm (PSA) treatment in vivo using a pig model. Purified fibrillar type I collagen was characterized using electron microscopy. The effect of three different sterilization procedures, ie, hydrogen peroxide gas plasma (H2O2), ethylene oxide gas (EtO), and gamma irradiation, was studied on both SDS-PAGE and platelet aggregation. Different collagen injectables were prepared (3%, 4%, and 5%) and tested using an injection force test applying a 21-gauge needle. To evaluate the network characteristics of the injectable collagen, the collagen was suspended in phosphate buffered saline (PBS) at 37°C and studied both macroscopically and electron microscopically. To determine whether the collagen induced hemostasis in vivo, a pig PSA model was used applying a 4% EtO sterilized collagen injectable, and evaluation by angiography and routine histology. Electron microscopy of the purified type I collagen revealed intact fibrils with a distinct striated pattern and a length<300 μm. Both SDS-PAGE and platelet aggregation analysis of the sterilized collagen indicated no major differences between EtO and H2O2 sterilization, although gamma-irradiated collagen showed degradation products. Both 3% and 4% (w/v) collagen suspensions were acceptable with respect to the force used (<50 N). The 4% suspension was selected as the preferred injectable collagen, which formed a dense network under physiologic conditions. Testing the collagen in vivo (n=5), the angiograms revealed that the PSA partly or completely coagulated. Histology confirmed the network

Millable polyurethane/organoclay nanocomposites: preparation, characterization, and properties.

PubMed

Siliani, M; López-Manchado, M A; Valentín, J L; Arroyo, M; Marcos, A; Khayet, M; Villaluenga, J P G

2007-02-01

Novel millable polyurethane (PU)/organoclay nanocomposites have been successfully prepared by conventional transformation techniques. One natural (C6A) and two organically modified (C15A and C30B) montmorillonites have been used as clays for preparing PU nanocomposites. The optimum dispersion of nanofiller at a nanometer scale in PU matrix was confirmed by X-ray diffraction patterns and transmission electron microscopy. A substantial improvement of the PU properties by addition of only a small amount of organoclay was observed. It is worthy to note that the organoclays show a different interfacial interaction with the PU matrix, which was reflected in different macroscopic properties. Thus, C30B organoclay seems to react with PU chains to form covalent bonds, while C15A only interacts physically with PU chains. Mechanical and barrier properties are analyzed.

Preparation and characterization of free films of high amylose/pectin mixtures cross-linked with sodium trimetaphosphate.

PubMed

Prezotti, Fabíola Garavello; Meneguin, Andréia Bagliotti; Evangelista, Raul Cesar; Cury, Beatriz Stringhetti Ferreira

2012-11-01

High amylose and pectin were mixed at 1:1 mass ratio and cross-linked with sodium trimetaphosphate (STMP) in alkaline medium. Films were prepared from aqueous dispersions of these cross-linked polymer blend at three different concentrations (3, 4 and 5%), by solvent casting method. Characterization of the films included thickness, surface morphology, water uptake, water vapor permeability (WVP), tensile strength measurements and enzymatic digestion. The cross-linking allowed to obtain films with improved mechanical properties and reduced WVP. The high resistance to enzymatic digestion exhibited by these films represents a promising approach to their application in the development of colon drug delivery systems.

Preparation, characterization, and infrared emissivity property of optically active polyurethane/TiO{sub 2}/SiO{sub 2} multilayered microspheres

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

Yang Yong; Zhou Yuming, E-mail: ymzhou@seu.edu.cn; Ge Jianhua

Optically active polyurethane/titania/silica (LPU/TiO{sub 2}/SiO{sub 2}) multilayered core-shell composite microspheres were prepared by the combination of titania deposition on the surface of silica spheres and subsequent polymer grafting. LPU/TiO{sub 2}/SiO{sub 2} was characterized by FT-IR, UV-vis spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), SEM and TEM, and the infrared emissivity value (8-14 {mu}m) was investigated in addition. The results indicated that titania and polyurethane had been successfully coated onto the surfaces of silica microspheres. LPU/TiO{sub 2}/SiO{sub 2} exhibited clearly multilayered core-shell construction. The infrared emissivity values reduced along with the increase of covering layers thus provedmore » that the interfacial interactions had direct influence on the infrared emissivity. Besides, LPU/TiO{sub 2}/SiO{sub 2} multilayered microspheres based on the optically active polyurethane took advantages of the orderly secondary structure and strengthened interfacial synergistic actions. Consequently, it possessed the lowest infrared emissivity value. - Graphical Abstract: Optically active polyurethane/titania/silica (LPU/TiO{sub 2}/SiO{sub 2}) multilayered core-shell composite microspheres were prepared by the combination of titania deposition on the surface of silica spheres and subsequent polymer grafting. Highlights: > Optically active polyurethane based on tyrosine was used for the modification of nanoparticles. > LPU/TiO{sub 2}/SiO{sub 2} multilayered core-shell microspheres were prepared and characterized. > Interfacial interactions and secondary structure affected the infrared emissivity of composite.« less

Characterization and Electrochromic Properties of Vanadium Oxide Thin Films Prepared via Spray Pyrolysis

NASA Astrophysics Data System (ADS)

Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M.-M.

2013-08-01

Vanadium oxide thin films were grown on glass substrates using spray pyrolysis technique. The effects of substrate temperature, vanadium concentration in the initial solution and the solution spray rate on the nanostructural and the electrochromic properties of deposited films are investigated. Characterization and the electrochromic measurements were carried out using X-ray diffraction, scanning electron microscopy and cyclic voltammogram. XRD patterns showed that the prepared films have polycrystalline structure and are mostly mixed phases of orthorhombic α-V2O5 along with minor β-V2O5 and V4O9 tetragonal structures. The preferred orientation of the deposited films was found to be along [101] plane. The cyclic voltammogram results obtained for different samples showed that only the films with 0.2 M solution concentration, 5 ml/min solution spray rate and 450°C substrate temperature exhibit two-step electrochromic properties. The results show a correlation between cycle voltammogram, morphology and resistance of the films.

Nanocelluloses from jute fibers and their nanocomposites with natural rubber: Preparation and characterization.

PubMed

Thomas, Martin George; Abraham, Eldho; Jyotishkumar, P; Maria, Hanna J; Pothen, Laly A; Thomas, Sabu

2015-11-01

Nanocellulose fibers having an average diameter of 50nm were isolated from raw jute fibers by steam explosion process. The isolation of nanocellulose from jute fibers by this extraction process is proved by SEM, XRD, FTIR, birefringence and TEM characterizations. This nanocellulose was used as the reinforcing agent in natural rubber (NR) latex along with crosslinking agents to prepare crosslinked nanocomposite films. The effects of nanocellulose loading on the morphology and mechanics of the nanocomposites have been carefully analyzed. Significant improvements in the Young's modulus and tensile strength of the nanocomposite were observed because of the reinforcing ability of the nanocellulose in the rubber matrix. A mechanism is suggested for the formation of the Zn-cellulose complex. The three-dimensional network of cellulose nanofibers (cellulose/cellulose network and Zn/cellulose network) in the NR matrix plays a major role in improving the properties of the crosslinked nanocomposites. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and characterization of 304 stainless steel/Q235 carbon steel composite material

NASA Astrophysics Data System (ADS)

Shen, Wenning; Feng, Lajun; Feng, Hui; Cao, Ying; Liu, Lei; Cao, Mo; Ge, Yanfeng

The composite material of 304 stainless steel reinforced Q235 carbon steel has been prepared by modified hot-rolling process. The resulted material was characterized by scanning electron microscope, three-electrode method, fault current impact method, electrochemical potentiodynamic polarization curve measurement and electrochemical impedance spectroscopy. The results showed that metallurgical bond between the stainless steel layer and carbon steel substrate has been formed. The composite material exhibited good electrical conductivity and thermal stability. The average grounding resistance of the composite material was about 13/20 of dip galvanized steel. There has no surface crack and bubbling formed after fault current impact. The composite material led to a significant decrease in the corrosion current density in soil solution, compared with that of hot dip galvanized steel and bare carbon steel. On the basis polarization curve and EIS analyses, it can be concluded that the composite material showed improved anti-corrosion property than hot-dip galvanized steel.

Classification of solid dispersions: correlation to (i) stability and solubility (ii) preparation and characterization techniques.

PubMed

Meng, Fan; Gala, Urvi; Chauhan, Harsh

2015-01-01

Solid dispersion has been a topic of interest in recent years for its potential in improving oral bioavailability, especially for poorly water soluble drugs where dissolution could be the rate-limiting step of oral absorption. Understanding the physical state of the drug and polymers in solid dispersions is essential as it influences both the stability and solubility of these systems. This review emphasizes on the classification of solid dispersions based on the physical states of drug and polymer. Based on this classification, stability aspects such as crystallization tendency, glass transition temperature (Tg), drug polymer miscibility, molecular mobility, etc. and solubility aspects have been discussed. In addition, preparation and characterization methods for binary solid dispersions based on the classification have also been discussed.

Preparation and Characterization of Injectable Brushite Filled-Poly (Methyl Methacrylate) Bone Cement

PubMed Central

Rodriguez, Lucas C.; Chari, Jonathan; Aghyarian, Shant; Gindri, Izabelle M.; Kosmopoulos, Victor; Rodrigues, Danieli C.

2014-01-01

Powder-liquid poly (methyl methacrylate) (PMMA) bone cements are widely utilized for augmentation of bone fractures and fixation of orthopedic implants. These cements typically have an abundance of beneficial qualities, however their lack of bioactivity allows for continued development. To enhance osseointegration and bioactivity, calcium phosphate cements prepared with hydroxyapatite, brushite or tricalcium phosphates have been introduced with rather unsuccessful results due to increased cement viscosity, poor handling and reduced mechanical performance. This has limited the use of such cements in applications requiring delivery through small cannulas and in load bearing. The goal of this study is to design an alternative cement system that can better accommodate calcium-phosphate additives while preserving cement rheological properties and performance. In the present work, a number of brushite-filled two-solution bone cements were prepared and characterized by studying their complex viscosity-versus-test frequency, extrusion stress, clumping tendency during injection through a syringe, extent of fill of a machined void in cortical bone analog specimens, and compressive strength. The addition of brushite into the two-solution cement formulations investigated did not affect the pseudoplastic behavior and handling properties of the materials as demonstrated by rheological experiments. Extrusion stress was observed to vary with brushite concentration with values lower or in the range of control PMMA-based cements. The materials were observed to completely fill pre-formed voids in bone analog specimens. Cement compressive strength was observed to decrease with increasing concentration of fillers; however, the materials exhibited high enough strength for consideration in load bearing applications. The results indicated that partially substituting the PMMA phase of the two-solution cement with brushite at a 40% by mass concentration provided the best combination of the

Characterization of doped hydrogenated nanocrystalline silicon films prepared by plasma enhanced chemical vapour deposition

NASA Astrophysics Data System (ADS)

Wang, Jin-Liang; Wu, Er-Xing

2007-03-01

The B- and P-doped hydrogenated nanocrystalline silicon films (nc-Si:H) are prepared by plasma-enhanced chemical vapour deposition (PECVD). The microstructures of doped nc-Si:H films are carefully and systematically characterized by using high resolution electron microscopy (HREM), Raman scattering, x-ray diffraction (XRD), Auger electron spectroscopy (AES), and resonant nucleus reaction (RNR). The results show that as the doping concentration of PH3 increases, the average grain size (d) tends to decrease and the crystalline volume percentage (Xc) increases simultaneously. For the B-doped samples, as the doping concentration of B2H6 increases, no obvious change in the value of d is observed, but the value of Xc is found to decrease. This is especially apparent in the case of heavy B2H6 doped samples, where the films change from nanocrystalline to amorphous.

Preparation and characterization of six calixarene bonded stationary phases for high performance liquid chromatography.

PubMed

Ding, Chenghua; Qu, Kang; Li, Yongbo; Hu, Kai; Liu, Hongxia; Ye, Baoxian; Wu, Yangjie; Zhang, Shusheng

2007-11-02

Six calixarene bonded silica gel stationary phases were prepared and characterized by elemental analysis, infrared spectroscopy and thermal analysis. Their chromatographic performance was investigated by using PAHs, aromatic positional isomers and E- and Z-ethyl 3-(4-acetylphenyl) acrylate isomers as probes. Separation mechanism based on the different interactions between calixarenes and analytes were discussed. The chromatographic behaviors of those analytes on the calixarene columns were influenced by the supramolecular interaction including pi-pi interaction, space steric hindrance and hydrogen bonding interaction between calixarenes and analytes. Notably, the presence of polar groups (-OH, -NO(2) and -NH(2)) in the aromatic isomers could improve their separation selectivity on calixarene phase columns. The results from quantum chemistry calculation using DFT-B3LYP/STO-3G* base group were consistent with the retention behaviors of PHAs on calix[4]arene column.

Nano-liposomal dry powder inhaler of tacrolimus: preparation, characterization, and pulmonary pharmacokinetics.

PubMed

Chougule, Mahavir; Padhi, Bijay; Misra, Ambikanandan

2007-01-01

The studies were undertaken to evaluate feasibility of pulmonary delivery of liposomaly encapsulated tacrolimus dry powder inhaler for prolonged drug retention in lungs as rescue therapy to prevent refractory rejection of lungs after transplantation. Tacrolimus encapsulated liposomes were prepared by thin film evaporation technique and liposomal dispersion was passed through high pressure homogenizer. Tacrolimus nano-liposomes (NLs) were separated by centrifugation and characterized. NLs were dispersed in phosphate buffer saline (PBS) pH 7.4 containing different additives like lactose, sucrose, and trehalose, and L-leucine as antiadherent. The dispersion was spray dried and spray dried powders were characterized. In vitro and in vivo pulmonary deposition was performed using Andersen Cascade Impactor and intratracheal instillation in rats respectively. NLs were found to have average size of 140 nm, 96% +/- 1.5% drug entrapment, and zeta potential of 1.107 mV. Trehalose based formulation was found to have low density, good flowability, particle size of 9.46 +/- 0.8 microm, maximum fine particle fraction (FPF) of 71.1 +/- 2.5%, mean mass aerodynamic diameter (MMAD) 2.2 +/- 0.1 microm, and geometric standard deviation (GSD) 1.7 +/- 0.2. Developed formulations were found to have in vitro prolonged drug release up to 18 hours, following Higuchi's Controlled Release model. In vivo studies revealed maximal residence of tacrolimus within lungs of 24 hours, suggesting slow clearance from the lungs. The investigation provides a practical approach for direct delivery of tacrolimus encapsulated in NLs for controlled and prolonged retention at the site of action. It may play a promising role as rescue therapy in reducing the risk of acute rejection and chronic rejection.

Preparation and characterization of carbon-supported sub-monolayer palladium decorated gold nanoparticles for the electro-oxidation of ethanol in alkaline media

NASA Astrophysics Data System (ADS)

Zhu, L. D.; Zhao, T. S.; Xu, J. B.; Liang, Z. X.

Carbon-supported gold nanoparticles (Au/C) are successfully decorated with mono- or sub-monolayer palladium atoms with different Pd/Au atomic ratios by a chemically epitaxial seeded growth method. TEM, UV-vis spectrometry and XRD techniques are used to characterize the particle size, dispersion, palladium coverage on gold seeds and crystal structures of the prepared catalysts. Cyclic voltammetric tests show that the Pd-decorated Au/C (denoted by Pd@Au/C) have higher specific activities than that of Pd/C for the oxidation of ethanol in alkaline media. This suggests that the Pd utilization is improved with such a surface-alloyed nanostructure. In addition, stable chronoamperometric responses are achieved with the so-prepared electrocatalysts during ethanol oxidation.

Characterizations of maghemite thin films prepared by a sol-gel method

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

Lau, L. N., E-mail: lau7798@gmail.com; Ibrahim, N. B., E-mail: baayah@ukm.edu.my

2015-09-25

Iron is one of the abundant elements of Mother Nature and its compound, iron oxide is an interesting material to study since its discovery in the form of magnetite. It can exist in many phases such as hematite and maghemite, this unique nature has put it as a potential candidate in various applications. The aim of this work is to study the influence of different precursor concentrations on the microstructural and magnetic properties of iron oxide thin film. All samples were prepared via the sol-gel method followed by a spin coating technique on quartz substrates. Iron oxide films were confirmedmore » as maghemite phase from X-ray diffraction patterns. The film morphology was examined by a field emission scanning electron microscope and it showed non-systematic value of average grain size and film thickness throughout the study. Hysteresis loop further confirmed that maghemite is a magnetic material when it was characterized by a vibrating sample magnetometer. The coercivity did not show any correlation with molarity. Nevertheless, it increased as the precursor concentration of the film increased due to the domain behaviour. In conclusion, maghemite thin films were successfully synthesized by the sol-gel method with different precursor concentrations in this work.« less

Azo biphenyl polyurethane: Preparation, characterization and application for optical waveguide switch

NASA Astrophysics Data System (ADS)

Jiang, Yan; Da, Zulin; Qiu, Fengxian; Yang, Dongya; Guan, Yijun; Cao, Guorong

2018-01-01

Azo waveguide polymers are of particular interest in the design of materials for applications in optical switch. The aim of this contribution was the synthesis and thermo-optic waveguide switch properties of azo biphenyl polyurethanes. A series of monomers and azo biphenyl polyurethanes (Azo BPU1 and Azo BPU2) were synthesized and characterized by FT-IR, UV-Vis spectroscopy and 1H NMR. The physical and mechanical properties of thin polymer films were measured. The refractive index and thermo-optic coefficient (dn/dT) of polymer films were investigated for TE (transversal electric) polarizations by ATR technique. The transmission loss of film was measured using the Charge Coupled Device digital imaging devices. The results showed the Azo BPU2 containing chiral azobenzene chromophore had higher dn/dT and lower transmission loss. Subsequently, a 1 × 2 Y-branch and 2 × 2 Mach-Zehnder optical switches based on the prepared polymers were designed and simulated. The results showed that the power consumption of all switches was less than 1.0 mW. Compared with 1 × 2 Y-branch optical switch, the 2 × 2 Mach-Zehnder optical switches based on the same polymer have the faster response time, which were about only 1.2 and 2.0 ms, respectively.

Preparation and characterization of aminoethyl hydroxypropyl starch modified with collagen peptide.

PubMed

Wen, Huigao; Hu, Jin; Ge, Hongyu; Zou, Shengqiong; Xiao, Yao; Li, Ya; Feng, Han; Fan, Lihong

2017-08-01

The preparation of aminoethyl hydroxypropyl starch collagen peptide (AEHPS-COP) was via an enzyme-catalyzed reaction between amino groups in aminoethyl hydroxypropyl starch (AEHPS) and γ-carboxamide groups in collagen peptide (COP) by using microbial transglutaminase (MTGase) as biocatalyst. As an intermediate reactant, AEHPS was synthesized from hydroxypropyl starch (HPS) and 2-chloroethylamine hydrochloride (CEH). The chemical structures of HPS, AEHPS and AEHPS-COP were characterized by Fourier transform infrared spectroscopy (FT-IR) and 13 C nuclear magnetic resonance ( 13 C NMR). The reaction conditions that influenced the degree of substitution (DS) of AEHPS-COP were optimized, which included the reaction temperature, the reaction time, the mass ratio of collagen peptide to aminoethyl hydroxypropyl starch and the pH value. In addition, in vitro antioxidant activities of AEHPS-COP were evaluated through the scavenging activity of hydroxyl and 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical. Furthermore, the methylthiazol tetrazolium (MTT) assay was applied to investigate the cell viability of AEHPS-COP. The results indicated that the AEHPS-COP exhibited better cell viability to L929 mouse fibroblast cells. Therefore, the AEHPS-COP showed a promising potential application in cosmetic, biomedical and pharmaceutical fields. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and Characterization of Ion-Irradiated Nanodiamonds as Photoacoustic Contrast Agents.

PubMed

Fang, Chia-Yi; Chang, Cheng-Chun; Mou, Chung-Yuan; Chang, Huan-Cheng

2015-02-01

Highly radiation-damaged or irradiated nanodiamonds (INDs) are a new type of nanomaterial developed recently as a potential photoacoustic (PA) contrast agent for deep-tissue imaging. This work characterized in detail the photophysical properties of these materials prepared by ion irradiation of natural diamond powders using various spectroscopic methods. For 40-nm NDs irradiated with 40-keV He+ at a dose of 3 x 10(15) ions/cm2, an average molar extinction coefficient of 4.2 M-1 cm-1 per carbon atom was measured at 1064 nm. Compared with gold nanorods of similar dimensions (10 nm x 67 nm), the INDs have a substantially smaller (by > 4 orders of magnitude) molar extinction coefficient per particle. However, the deficit is readily compensated by the much higher thermal stability, stronger hydrophilic interaction with water, and a lower nanobubble formation threshold (~30 mJ/cm2) of the sp3-carbon-based nanomaterial. No sign of photodamage was detected after high-energy (>100 mJ/cm2) illumination of the INDs for hours. Cell viability assays at the IND concentration of up to 100 µg/mL showed that the nanomaterial is non-cytotoxic and potentially useful for long-term PA bioimaging applications.

Preparation and characterization of Pd doped ceria-ZnO nanocomposite catalyst for methyl tert-butyl ether (MTBE) photodegradation.

PubMed

Seddigi, Zaki S; Bumajdad, Ali; Ansari, Shahid P; Ahmed, Saleh A; Danish, Ekram Y; Yarkandi, Naeema H; Ahmed, Shakeel

2014-01-15

A series of binary oxide catalysts (ceria-ZnO) were prepared and doped with different amounts of palladium in the range of 0.5%-1.5%. The prepared catalysts were characterized by SEM, TEM, XRD and XPS, as well as by N2 sorptiometry study. The XPS results confirmed the structure of the Pd CeO2-x-ZnO. The photocatalytic activity of these catalysts was evaluated for degradation of MTBE in water. These photocatalyst efficiently degrade a 100ppm aqueous solution of MTBE upon UV irradiation for 5h in the presence of 100mg of each of these photocatalysts. The removal of 99.6% of the MTBE was achieved with the ceria-ZnO catalyst doped with 1% Pd. In addition to the Pd loading, the N2 sorptiometry study introduced other factors that might affect the catalytic efficiency is the catalyst average pore sizes. The photoreaction was determined to be a first order reaction. Copyright © 2013 Elsevier B.V. All rights reserved.

Irradiation of industrial enzyme preparations. II. Characterization of fungal pectinase by thin-layer isoelectric focusing and gel filtration

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

Delincee, H.

1978-01-01

Industrial dry fungal pectinase from A. niger was irradiated with doses (up to 1 Mrad) of /sup 60/Co-..gamma..rays effective in reducing microbial contamination. The pectinase was characterized by thin-layer isoelectric focusing and gel filtration in order to detect possible radiation-induced structural alterations. Thin-layer isoelectric focusing revealed at least fifteen multiple forms with pectin-depolymerizing activity, with isoelectric points in the range pH 4.5 to 7. Heterogeneity of pectinesterase was also demonstrated, the main band occurring around pH 4. By thin-layer gel filtration the molecular weight of the pectin-depolymerase was estimated as being about 36,000, and that of pectinesterase as about 33,000.more » Radiation-induced changes of the charge properties or molecular size of the irradiated pectinase preparation were not observed. The feasibility of using ionizing radiation for the reduction of microbial contamination of industrial enzyme preparations looks promising.« less

Preparation and Characterization of Various Poly(ether ether ketone) Containing Imidazolium Moiety for Anion Exchange Membrane Fuel Cell Application.

PubMed

Lee, Byeol-Nim; Son, Tae Yang; Park, Chi Hoon; Kim, Tae Hyun; Nam, Sang Yong

2018-09-01

In this study, various poly(ether ether ketone) were synthesized using three different monomers and the imidazolium group was introduced into synthesized poly(ether ether ketone)s by using substitution reaction. Synthesized polymers were used to prepare anion exchange membranes and to evaluate its properties. Thermal, chemical and structural properties were carried out using thermogravimetric analysis, nuclear magnetic resonance. The anion exchange membranes with different imidazolium moieties were characterized by several different analytical techniques such as water up take, ion exchange capacity, hydroxide conductivity for checking the possibility to apply the anion exchange membrane fuel cell. Consequently, results of characterization were studied to understand the correlation between stabilities of the membrane and functional group and polymer backbone structures. And we confirm membrane performance was improved by increasing imidazolium cation groups.

Preparation and characterization of activated carbon from acorn shell by physical activation with H2O-CO2 in two-step pretreatment.

PubMed

Şahin, Ömer; Saka, Cafer

2013-05-01

Activated carbons have been prepared by physical activation with H2O-CO2 in two-step pre-treatment including ZnCl2-HCl from acorn shell at 850 °C. The active carbons were characterized by N2 adsorption at 77 K. Adsorption capacity was demonstrated by the iodine numbers. The surface chemical characteristics of activated carbons were determined by FTIR spectroscopic method. The microstructure of the activated carbons prepared was examined by scanning electron microscopy. The maximum BET surface area of the obtained activated carbon was found to be around 1779 m(2)/g. Copyright © 2013 Elsevier Ltd. All rights reserved.

Preparation and Characterization of Polyhydroxybutyrate/Polycaprolactone Nanocomposites

PubMed Central

Liau, Cha Ping; Bin Ahmad, Mansor; Shameli, Kamyar; Yunus, Wan Md Zin Wan

2014-01-01

Polyhydroxybutyrate (PHB)/polycaprolactone (PCL)/stearate Mg-Al layered double hydroxide (LDH) nanocomposites were prepared via solution casting intercalation method. Coprecipitation method was used to prepare the anionic clay Mg-Al LDH from nitrate salt solution. Modification of nitrate anions by stearate anions between the LDH layers via ion exchange reaction. FTIR spectra showed the presence of carboxylic acid (COOH) group which indicates that stearate anions were successfully intercalated into the Mg-Al LDH. The formation of nanocomposites only involves physical interaction as there are no new functional groups or new bonding formed. X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated that the mixtures of nanocomposites are intercalated and exfoliated types. XRD results showed increasing of basal spacing from 8.66 to 32.97 Å in modified stearate Mg-Al LDH, and TEM results revealed that the stearate Mg-Al LDH layers are homogeneously distributed in the PHB/PCL polymer blends matrix. Enhancement in 300% elongation at break and 66% tensile strength in the presence of 1.0 wt % of the stearate Mg-Al LDH as compare with PHB/PCL blends. Scanning electron microscopy (SEM) proved that clay improves compatibility between polymer matrix and the best ratio 80PHB/20PCL/1stearate Mg-Al LDH surface is well dispersed and stretched before it breaks. PMID:24600329

21 CFR 184.1148 - Bacterially-derived carbohydrase enzyme preparation.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Bacterially-derived carbohydrase enzyme... carbohydrase enzyme preparation. (a) Bacterially-derived carbohydrase enzyme preparation is obtained from the... Bacillus subtilis or B. amyloliquefaciens. The preparation is characterized by the presence of the enzymes...

21 CFR 184.1148 - Bacterially-derived carbohydrase enzyme preparation.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Bacterially-derived carbohydrase enzyme... carbohydrase enzyme preparation. (a) Bacterially-derived carbohydrase enzyme preparation is obtained from the... Bacillus subtilis or B. amyloliquefaciens. The preparation is characterized by the presence of the enzymes...

21 CFR 184.1148 - Bacterially-derived carbohydrase enzyme preparation.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Bacterially-derived carbohydrase enzyme... carbohydrase enzyme preparation. (a) Bacterially-derived carbohydrase enzyme preparation is obtained from the... Bacillus subtilis or B. amyloliquefaciens. The preparation is characterized by the presence of the enzymes...

Methods to Prepare Aluminum Salt-Adjuvanted Vaccines.

PubMed

Thakkar, Sachin G; Cui, Zhengrong

2017-01-01

Many human vaccines contain certain insoluble aluminum salts such as aluminum oxyhydroxide and aluminum hydroxyphosphate as vaccine adjuvants to boost the immunogenicity of the vaccines. Aluminum salts have been used as vaccine adjuvants for decades and have an established, favorable safety profile. However, preparing aluminum salts and aluminum salt-adjuvanted vaccines in a consistent manner remains challenging. This chapter discusses methods to prepare aluminum salts and aluminum salt-adjuvanted vaccines, factors to consider during preparation, and methods to characterize the vaccines after preparation.

Surface characterization of acidic ceria-zirconia prepared by direct sulfation

NASA Astrophysics Data System (ADS)

Azambre, B.; Zenboury, L.; Weber, J. V.; Burg, P.

2010-05-01

Acidic ceria-zirconia (SCZ) solid acid catalysts with a nominal surface density of ca 2 SO 42-/nm 2 were prepared by a simple route consisting in soaking high specific surface area Ce xZr 1- xO 2 (with x = 0.21 and 0.69) mixed oxides solutions in 0.5 M sulphuric acid. Characterizations by TPD-MS, TP-DRIFTS and FT-Raman revealed that most of surface structures generated by sulfation are stable at least up to 700 °C under inert atmosphere and consist mainly as isolated sulfates located on defects or crystal planes and to a lesser extent as polysulfates. Investigations by pyridine adsorption/desorption have stated that: SCZ possess both strong Brønsted (B) and Lewis (L) acid sites, some of them being presumably superacidic; the B/L site ratio was found to be more dependent on the temperature and hydration degree than on the composition of the ceria-zirconia. By contrast, the reactivity of the parent Ce xZr 1- xO 2 materials towards pyridine is mostly driven by redox properties resulting in the formation of Py-oxide with the participation of Lewis acid sites of moderate strength ( cus Ce x+ and Zr x+ cations). Basicity studies by CO 2 adsorption/desorption reveal that SCZ surfaces are solely acidic whereas the number and strength of Lewis basic sites increases with the Ce content for the parent Ce xZr 1- xO 2 materials.

Highly monodisperse multiple twinned AuCu-Pt trimetallic nanoparticles with high index surfaces.

PubMed

Khanal, Subarna; Bhattarai, Nabraj; McMaster, David; Bahena, Daniel; Velazquez-Salazar, J Jesus; Jose-Yacaman, Miguel

2014-08-14

Trimetallic nanoparticles possess different properties than their mono- and bi-metallic counterparts, opening a wide range of possibilities for diverse potential applications with the notion to study possible morphology, atomic ordering, reduce precious metal consumption and many others. In this paper, we present a comprehensive experimental study on AuCu-Pt trimetallic nanoparticles with an average diameter of 15 ± 1.0 nm, synthesized in a one-pot synthesis method and characterized by the Cs-corrected scanning transmission electron microscopy technique that allowed us to probe the structure at the atomic level resolution. A new way to control the nanoparticle morphology by the presence of third metal (Pt) is also discussed by the overgrowth of Pt on the as prepared AuCu core by Frank-van der Merwe (FM) layer-by-layer and Stranski-Krastanov (SK) island-on-wetting-layer growth modes. With the application of this research, we are now a step closer to produce optimum catalysts in which the active phase forms only surface monolayers. In addition, the nanoalloy exhibits high index facet surfaces with {211} and {321} families that are highly open-structure surfaces and are interesting for the catalytic applications.

Highly Monodisperse Multiple Twinned AuCu/Pt Trimetallic Nanoparticles with High Index Surfaces

PubMed Central

Khanal, Subarna; Bhattarai, Nabraj; McMaster, David; Bahena, Daniel; Velazquez-Salazar, J. Jesus

2014-01-01

Trimetallic nanoparticles present different properties than their mono- and bi-metallic counterparts, opening a wide range of possibilities for diverse potential applications with the notion to study possible morphology, atomic ordering, reduce precious metal consumption and many others. In this paper, we are presenting a comprehensive experimental study on AuCu/Pt trimetallic nanoparticles with an average diameter 15 ± 1.0 nm, synthesized in one-pot synthesis method and characterized by Cs-corrected scanning transmission electron microscopy technique that allowed us to probe the structure at the atomic level resolution. A new way to control the nanoparticle morphology by the presence of third metal (Pt) is also discussed by the overgrowth of Pt on as prepared AuCu core by Frank–van der Merwe (FM) layer-by-layer and Stranski–Krastanov (SK) island-on-wetting-layer growth modes. With the application of this research, we are now a step closer to produce optimum catalysts in which the active phase forms only surface monolayers. In addition, the nanoalloy presents high index facet surfaces with {211} and {321} families, that are highly open-structure surfaces and are interesting for the catalytic applications. PMID:24975090

Preparation and characterization of siloxane-containing thermoplastic polyimides

NASA Technical Reports Server (NTRS)

Maudgal, S.; St Clair, T. L.

1984-01-01

Copolyimides and homopolyimides of bis(gamma-aminopropyl)tetramethyldisiloxane and 3,3'-diaminobenzophenone have been prepared with benzophenonetetracarboxylic dianhydride. The properties of the copolyimides were compared with those of the homopolyimides to assess the effect of incorporation of siloxane groups in the backbone. Applications of the polymers as adhesives and mouldings are discussed.

Combinatorial preparation and characterization of thin-film multilayer electro-optical devices.

PubMed

Neuber, Christian; Bäte, Markus; Thelakkat, Mukundan; Schmidt, Hans-Werner; Hänsel, Helmut; Zettl, Heiko; Krausch, Georg

2007-07-01

In this article we present a setup for the combinatorial vapor deposition of thin-film multilayer devices as well as methods for the fast and efficient analytic screening of the libraries obtained. The preparation setup is based on a commercially available evaporation chamber equipped with various evaporation sources for both organic and metallic materials. The combinatorial approach is realized by the combination of a rotation stage for the substrate, a five-mask sampler, and an additional mask whose position can be deliberately varied along one axis during the evaporation process. The latter is used to evaporate linear as well as step gradients by continuous or stepwise movement of a shutter mask. The mask sampler allows to define the sectors of the library and to evaporate more complex structures, e.g., an electrode layout. Finally, the simultaneous evaporation of two or more materials enables us to produce layers of varying composition ratio in general and doped materials, in particular. For the control of the evaporation process we have developed an automation software, which is particularly helpful for complex library designs and which grants excellent repeatability of experiments. Efficient and fast characterization of the obtained libraries is realized by (i) a purely optical setup and (ii) an electro-optical setup. (i) The UV/vis reader FLASHScan 530 permits to map out the UV/vis absorbance or fluorescence of the whole library. The UV/vis absorbance is primarily used to determine layer thicknesses and to confirm thickness uniformity across larger regions. The fluorescence measurements are used to determine the composition of layers containing fluorescent dyes. (ii) For a detailed short- and long-term electro-optical analysis we have developed an automated measurement system, which allows the characterization of 8x8 optoelectronic devices and to study their degradation behavior. Both solar cells and organic light-emitting diodes can be tested. Finally, we

Preparation and characterization of novel carbon dioxide adsorbents based on polyethylenimine-modified Halloysite nanotubes.

PubMed

Cai, Haohao; Bao, Feng; Gao, Jie; Chen, Tao; Wang, Si; Ma, Rui

2015-01-01

New nano-sized carbon dioxide (CO2) adsorbents based on Halloysite nanotubes impregnated with polyethylenimine (PEI) were designed and synthesized, which were excellent adsorbents for the capture of CO2 at room temperature and had relatively high CO2 adsorption capacity. The prepared adsorbents were characterized by various techniques such as Fourier transform infrared spectrometry, gel permeation chromatography, dynamic light scattering, thermogravimetry, thermogravimetry-Fourier transform-infrared spectrometry, scanning electron microscopy and transmission electron microscopy. The adsorption characteristics and capacity were studied at room temperature, the highest CO2 adsorption capacity of 156.6 mg/g-PEI was obtained and the optimal adsorption capacity can reach a maximum value of 54.8 mg/g-adsorbent. The experiment indicated that this kind of adsorbent has a high stability at 80°C and PEI-impregnated adsorbents showed good reversibility and stability during cyclic adsorption-regeneration tests.

Bhasmas: unique ayurvedic metallic-herbal preparations, chemical characterization.

PubMed

Kumar, A; Nair, A G C; Reddy, A V R; Garg, A N

2006-03-01

Bhasmas are unique Ayurvedic metallic preparations with herbal juices/fruits, known in the Indian subcontinent since the seventh century BC and widely recommended for treatment of a variety of chronic ailments. Twenty bhasmas based on calcium, iron, zinc, mercury, silver, potassium, arsenic, copper, tin, and gemstones were analyzed for up to 18 elements by instrumental neutron activation analysis, including their C, H, N, and S contents. In addition to the major constituent element found at % level, several other essential elements such as Na, K, Ca, Mg, V, Mn, Fe, Cu, and Zn have also been found in microg/g amounts and ultratrace (ng/g) amounts of Au and Co. These seem to remain chelated with organic ligands derived from medicinal herbs. The bhasmas are biologically produced nanoparticles and are taken along with milk, butter, honey, or ghee (a preparation from milk); thus, this makes these elements easily assimilable, eliminating their harmful effects and enhancing their biocompatibility. Siddha Makaradhwaja, a mercury preparation is found to be stoichiometrically HgS without any traces of any other element. Similarly, Swet Parpati is stoichiometrically KNO3 but is found to have Mn, Cu, Zn, Na, P, and Cl as well. An attempt has been made to correlate the metallic contents with their medicinal importance. Na and K, the two electrolytic elements, seem to be well correlated, although K/Na varies in a wide range from 0.06 to 95, with specifically low values for Ca-, Fe-, and Zn-based bhasmas. K/P also varies in a wide range from 0.23 to 12, although for most bhasmas (n = 12), it is 2.3 +/- 1.2. Further, Fe/Mn is linearly correlated (r = 0.96) with Fe in nine noniron bhasmas.

Preparation, characterization, and antibacterial activity of silver nanoparticle-decorated graphene oxide nanocomposite.

PubMed

Shao, Wei; Liu, Xiufeng; Min, Huihua; Dong, Guanghui; Feng, Qingyuan; Zuo, Songlin

2015-04-01

In this work, we report a facile and green approach to prepare a uniform silver nanoparticles (AgNPs) decorated graphene oxide (GO) nanocomposite (GO-Ag). The nanocomposite was fully characterized by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectra, ultraviolet-visible (UV-vis) absorption spectra, and X-ray photoelectron spectroscopy (XPS), which demonstrated that AgNPs with a diameter of approximately 22 nm were uniformly and compactly deposited on GO. To investigate the silver ion release behaviors, HEPES buffers with different pH (5.5, 7, and 8.5) were selected and the mechanism of release actions was discussed in detail. The cytotoxicity of GO-Ag nanocomposite was also studied using HEK 293 cells. GO-Ag nanocomposite displayed good cytocompatibility. Furthermore, the antibacterial properties of GO-Ag nanocomposite were studied using Gram-negative E. coli ATCC 25922 and Gram-positive S. aureus ATCC 6538 by both the plate count method and disk diffusion method. The nanocomposite showed excellent antibacterial activity. These results demonstrated that GO-Ag nanocomposite, as a kind of antibacterial material, had a great promise for application in a wide range of biomedical applications.

Synthesis and characterization of cadmium sulphide thin films prepared by spin coating

NASA Astrophysics Data System (ADS)

Chodavadiya, Nisarg; Chapanari, Amisha; Zinzala, Jignesh; Ray, Jaymin; Pandya, Samir

2018-05-01

An II-VI group semiconductor is Wide band gap materials and has been widely studied due to their fundamental optical, structural, and electrical properties. Cadmium sulphide (CdS) is one of the most emerged materials in II-VI group. It has many applications such as buffer later in photovoltaic cell, multilayer light emitting diodes, optical filters, thin film field effect transistors, gas sensors, light detectors etc. It is fundamentally an n-type material with an optical band gap of 2.4 eV. Owing to these properties we had studied CdS thin films synthesis and characterized by Raman, Ultraviolet - Visible spectroscopy (UV-VIS) and Hot probe method. CdS thin films were prepared by spin coating of the Cadmium-thiourea precursor solution. Visual inspection after 20 minute thermolysis time the films were looks uniform and shiny pale yellow in color. Raman confirms the A1 vibration of pure CdS. UV-VIS gives the band gap about 2.52 eV, which confirms the formation of nanocrystalline form of CdS. Finally, hot probe signifies the n-type conductivity of the CdS film.

Synthesis, characterization, and mercury adsorption properties of hybrid mesoporous aluminosilicate sieve prepared with fly ash

PubMed Central

Liu, Minmin; Hou, Li-an; Xi, Beidou; Zhao, Ying; Xia, Xunfeng

2013-01-01

A novel hybrid mesoporous aluminosilicate sieve (HMAS) was prepared with fly ash and impregnated with zeolite A precursors. This improved the mercury adsorption of HMAS compared to original MCM-41. The HMAS was characterized by X-ray diffraction (XRD), nitrogen adsorption–desorption, Fourier transform infrared (FTIR) analysis, transmission electron microscopy (TEM) images and 29Si and 27Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectra. These showed that the HMAS structure was still retained after impregnated with zeolite A. But the surface area and pore diameter of HMAS decreased due to pore blockage. Adsorption of mercury from aqueous solution was studied on untreated MCM-41and HMAS. The mercury adsorption rate of HMAS was higher than that of origin MCM-41. The adsorption of mercury was investigated on HMAS regarding the pH of mercury solution, initial mercury concentration, and the reaction temperature. The experimental data fit well to Langmuir and Freundlich isotherm models. The Dublin–Radushkevich isotherm and the characterization show that the mercury adsorption on HMAS involved the ion-exchange mechanisms. In addition, the thermodynamic parameters suggest that the adsorption process was endothermic in nature. The adsorption of mercury on HMAS followed the first order kinetics. PMID:23687400

Synthesis, characterization, and mercury adsorption properties of hybrid mesoporous aluminosilicate sieve prepared with fly ash.

PubMed

Liu, Minmin; Hou, Li-An; Xi, Beidou; Zhao, Ying; Xia, Xunfeng

2013-05-15

A novel hybrid mesoporous aluminosilicate sieve (HMAS) was prepared with fly ash and impregnated with zeolite A precursors. This improved the mercury adsorption of HMAS compared to original MCM-41. The HMAS was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption, Fourier transform infrared (FTIR) analysis, transmission electron microscopy (TEM) images and 29 Si and 27 Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectra. These showed that the HMAS structure was still retained after impregnated with zeolite A. But the surface area and pore diameter of HMAS decreased due to pore blockage. Adsorption of mercury from aqueous solution was studied on untreated MCM-41and HMAS. The mercury adsorption rate of HMAS was higher than that of origin MCM-41. The adsorption of mercury was investigated on HMAS regarding the pH of mercury solution, initial mercury concentration, and the reaction temperature. The experimental data fit well to Langmuir and Freundlich isotherm models. The Dublin-Radushkevich isotherm and the characterization show that the mercury adsorption on HMAS involved the ion-exchange mechanisms. In addition, the thermodynamic parameters suggest that the adsorption process was endothermic in nature. The adsorption of mercury on HMAS followed the first order kinetics.

Nano-liposomal dry powder inhaler of tacrolimus: Preparation, characterization, and pulmonary pharmacokinetics

PubMed Central

Chougule, Mahavir; Padhi, Bijay; Misra, Ambikanandan

2007-01-01

The studies were undertaken to evaluate feasibility of pulmonary delivery of liposomaly encapsulated tacrolimus dry powder inhaler for prolonged drug retention in lungs as rescue therapy to prevent refractory rejection of lungs after transplantation. Tacrolimus encapsulated liposomes were prepared by thin film evaporation technique and liposomal dispersion was passed through high pressure homogenizer. Tacrolimus nano-liposomes (NLs) were separated by centrifugation and characterized. NLs were dispersed in phosphate buffer saline (PBS) pH 7.4 containing different additives like lactose, sucrose, and trehalose, and L-leucine as antiadherent. The dispersion was spray dried and spray dried powders were characterized. In vitro and in vivo pulmonary deposition was performed using Andersen Cascade Impactor and intratracheal instillation in rats respectively. NLs were found to have average size of 140 nm, 96% ± 1.5% drug entrapment, and zeta potential of 1.107 mV. Trehalose based formulation was found to have low density, good flowability, particle size of 9.46 ± 0.8 μm, maximum fine particle fraction (FPF) of 71.1 ± 2.5%, mean mass aerodynamic diameter (MMAD) 2.2 ± 0.1 μm, and geometric standard deviation (GSD) 1.7 ± 0.2. Developed formulations were found to have in vitro prolonged drug release up to 18 hours, following Higuchi’s Controlled Release model. In vivo studies revealed maximal residence of tacrolimus within lungs of 24 hours, suggesting slow clearance from the lungs. The investigation provides a practical approach for direct delivery of tacrolimus encapsulated in NLs for controlled and prolonged retention at the site of action. It may play a promising role as rescue therapy in reducing the risk of acute rejection and chronic rejection. PMID:18203434

Preparation and characterization of phosphine-tetraborane(8)

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

Jock, C.P.; Kodama, G.

1988-09-21

The preparation of B/sub 4/H/sub 8/ x PH/sub 3/ by cleaving pentaborane, B/sub 5/H/sub 11/, with PH/sub 3/ is reported herein. The formation of a reaction intermediate, B/sub 5/H/sub 11/ x PH/sub 3/, which decomposes above -80/degrees/C in dichloromethane, is also reported. The /sup 11/B NMR spectrum of B/sub 4/H/sub 8/ x PH/sub 3/ indicates that the compound exists in two isomeric forms, endo and exo forms. 18 references, 3 figures, 1 table.

Polymeric nanoparticles containing diazepam: preparation, optimization, characterization, in-vitro drug release and release kinetic study

NASA Astrophysics Data System (ADS)

Bohrey, Sarvesh; Chourasiya, Vibha; Pandey, Archna

2016-03-01

Nanoparticles formulated from biodegradable polymers like poly(lactic-co-glycolic acid) (PLGA) are being extensively investigated as drug delivery systems due to their two important properties such as biocompatibility and controlled drug release characteristics. The aim of this work to formulated diazepam loaded PLGA nanoparticles by using emulsion solvent evaporation technique. Polyvinyl alcohol (PVA) is used as stabilizing agent. Diazepam is a benzodiazepine derivative drug, and widely used as an anticonvulsant in the treatment of various types of epilepsy, insomnia and anxiety. This work investigates the effects of some preparation variables on the size and shape of nanoparticles prepared by emulsion solvent evaporation method. These nanoparticles were characterized by photon correlation spectroscopy (PCS), transmission electron microscopy (TEM). Zeta potential study was also performed to understand the surface charge of nanoparticles. The drug release from drug loaded nanoparticles was studied by dialysis bag method and the in vitro drug release data was also studied by various kinetic models. The results show that sonication time, polymer content, surfactant concentration, ratio of organic to aqueous phase volume, and the amount of drug have an important effect on the size of nanoparticles. Hopefully we produced spherical shape Diazepam loaded PLGA nanoparticles with a size range under 250 nm with zeta potential -23.3 mV. The in vitro drug release analysis shows sustained release of drug from nanoparticles and follow Korsmeyer-Peppas model.

The Preparation and Characterization of Tetrafluoro-lambda 6-Sulfanes

NASA Astrophysics Data System (ADS)

Zhong, Linbin

Synthetic access to systematically substituted tetrafluoro-λ6-sulfanes was challenging and the research in this area had been largely abandoned. The original reports of disubstituted-tetrafluoro-λ6-sulfanes were limited to substitution by diphenyl and dialkyl groups. The dialkyl-tetrafluoro-λ6-sulfanes were reactive while the diphenyl substituted compounds showed decreased reactivity. In this dissertation, the systematic substitution on tetrafluoro-λ6-sulfanes has enabled the studies of the substitution effects on reactivity. The synthesis of substituted-tetrafluoro-λ6-sulfanyl chlorides were facilitated by a convenient preparation of CF3SF4Cl and aryl-SF4Cl. The scope and limits of the free radical promoted reaction of these compounds were explored by addition to alkenes and alkynes. Especially interesting is that several of the resulting adducts were crystallized in non-centrosymmetric structures. Novel polymers linked by SF4 groups were also prepared. As a derivative of SF5Cl, substituted-tetrafluoro-λ6-sulfanes are expected to have similar reactivity, specifically, when the trans-(trifluoromethyl)-tetrafluoro-λ6-sulfanyl is incorporated into to molecules. The physicochemical properties of these compounds may surpass those of the SF5 analogs. Subsequent transformations of the addition products, such as the preparations of alkyl-SF4Cl substituted alkenes, alkynes, carboxylic acid, ketones, and aldehydes will be described.

Jumbo squid (Dosidicus gigas) mantle collagen: extraction, characterization, and potential application in the preparation of chitosan-collagen biofilms.

PubMed

Uriarte-Montoya, Mario Hiram; Arias-Moscoso, Joe Luis; Plascencia-Jatomea, Maribel; Santacruz-Ortega, Hisila; Rouzaud-Sández, Ofelia; Cardenas-Lopez, Jose Luis; Marquez-Rios, Enrique; Ezquerra-Brauer, Josafat Marina

2010-06-01

Collagen-based biomaterials have been widely used due to its binding capabilities. However the properties and potential use of new collagen sources are still under investigation. Fish by-products are an excellent source of collagen. Thus, acid-soluble collagen (ASC) was extracted, and biochemical and physicochemically characterized from one under-utilized specie, jumbo squid (Dosidicus gigas). In addition, commercial chitosan (95-50%)-ASC (5-50%) blend films were successfully prepared by casting, and characterized by infrared spectroscopy (FT-IR) and differential scanning calorimetry (DSC). The molecular masses of the ASC subunits were about 190kDa, 110kDa, and 97kDa, the content of proline and hydroxyproline was 10.9% and 2.8%, respectively. The FT-IR and nuclear magnetic resonance spectra ((1)H NMR) confirmed collagen peptidic crosslinks, and one endothermic peak was found at 119 degrees C. The FT-IR spectrum showed that chitosan and ASC remain linked into the films mainly due to hydrogen bonding. The 85:15 (chitosan:ASC) ratio was selected for its thermal and mechanical analyses. The thermograms of this film indicated the presence of two peaks, one at 87-98 degrees C and the other at 142-182 degrees C. The chitosan:ASC blend produced a transparent and brittle film, with high percentage of elongation at break, and low tensile strength in comparison to chitosan films. D. gigas mantle might be useful as a new source of plasticizer agent in the preparation of biofilms in composites with chitosan. Copyright 2010 Elsevier Ltd. All rights reserved.

High spatial resolution PEELS characterization of FeAl nanograins prepared by mechanical alloying

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

Valdre, G.; Botton, G.A.; Brown, L.M.

The authors investigate the nanograin ``chemical`` structure in a nanostructured material of possible industrial application (Fe-Al system) prepared by conventional mechanical alloying via ball milling in argon atmosphere. They restrict themselves to the structural and nanochemical behavior of ball-milled nanocrystalline Fe-Al powders with atomic composition Fe{sub 3}Al, corresponding to a well-known intermetallic compound of the Fe-Al system. Scanning transmission electron microscopy (STEM) equipped with a parallel detection electron energy loss spectrometer (PEELS) has provided an insight on the ``chemical`` structure of both nanograins and their surface at a spatial resolution of better than 1 nm. The energy loss near edgemore » structure of the Al L loss reveals that the Al coordination is similar to a B2 compound and the oxidation of the powder during processing may play a significant role in the stabilization of the intermetallic phases. Conventional transmission electron microscopy (TEM) was used for the structural characterization of the material after the ball milling; powder X-ray diffraction (XRD) aided the investigation.« less

Preparation and characterization of dextran nanobubbles for oxygen delivery.

PubMed

Cavalli, R; Bisazza, A; Giustetto, P; Civra, A; Lembo, D; Trotta, G; Guiot, C; Trotta, M

2009-11-03

Dextran nanobubbles were prepared with a dextran shell and a perfluoropentan core in which oxygen was stored. To increase the stability polyvinylpirrolidone was also added to the formulation as stabilizing agent. Rhodamine B was used as fluorescent marker to obtain fluorescent nanobubbles. The nanobubble formulations showed sizes of about 500nm, a negative surface charge and a good capacity of loading oxygen, no hemolytic activity or toxic effect on cell lines. The fluorescent labelled nanobubbles could be internalized in Vero cells. Oxygen-filled nanobubbles were able to release oxygen in different hypoxic solutions at different time after their preparation in in vitro experiments. The oxygen release kinetics could be enhanced after nanobubble insonation with ultrasound at 2.5MHz. The oxygen-filled nanobubble formulations might be proposed for therapeutic applications in various diseases.

Preparation, characterization, dielectric properties and diffusion studies of styrene butadiene rubber (SBR)/manganous tungstate (MnWO4) nanocomposites

NASA Astrophysics Data System (ADS)

Jasna, V. C.; Ramesan, M. T.

2017-06-01

Nanocomposites based on SBR with different content of manganous tungstate nanoparticles were prepared and characterized by FTIR, UV-visible spectroscopy, XRD, SEM, TGA, DSC and impedance analysis. The interaction between nanoparticles and the elastomer was clear from the shift in peaks of UV and FTIR. XRD and SEM analysis showed the uniform arrangement of nanoparticles in SBR matrix. Glass transition temperature, thermal stability and dielectric properties of composites were enhanced by the addition of nanoparticles. Sorption studies of nanocomposites were done in aromatic solvents at different temperature. Sorption data obtained were used to estimate the thermodynamic properties.

Preparation, characterization, and transport of dexamethasone-loaded polymeric nanoparticles across a human placental in vitro model

PubMed Central

Ali, Hazem; Kalashnikova, Irina; White, Mark Andrew; Sherman, Michael; Rytting, Erik

2013-01-01

The purpose of this study was to prepare dexamethasone-loaded polymeric nanoparticles and evaluate their potential for transport across human placenta. Statistical modeling and factorial design was applied to investigate the influence of process parameters on the following nanoparticle characteristics: particle size, polydispersity index, zeta potential, and drug encapsulation efficiency. Dexamethasone and nanoparticle transport was subsequently investigated using the BeWo b30 cell line, an in vitro model of human placental trophoblast cells, which represent the rate-limiting barrier for maternal-fetal transfer. Encapsulation efficiency and drug transport were determined using a validated high performance liquid chromatography method. Nanoparticle morphology and drug encapsulation were further characterized by cryo-transmission electron microscopy and X-ray diffraction, respectively. Nanoparticles prepared from poly(lactic-co-glycolic acid) were spherical, with particle sizes ranging from 140–298 nm, and encapsulation efficiency ranging from 52–89%. Nanoencapsulation enhanced the apparent permeability of dexamethasone from the maternal compartment to the fetal compartment more than 10-fold in this model. Particle size was shown to be inversely correlated with drug and nanoparticle permeability, as confirmed with fluorescently-labeled nanoparticles. These results highlight the feasibility of designing nanoparticles capable of delivering medication to the fetus, in particular, potential dexamethasone therapy for the prenatal treatment of congenital adrenal hyperplasia. PMID:23850397

Effort versus Reward: Preparing Samples for Fungal Community Characterization in High-Throughput Sequencing Surveys of Soils

PubMed Central

Song, Zewei; Schlatter, Dan; Kennedy, Peter; Kinkel, Linda L.; Kistler, H. Corby; Nguyen, Nhu; Bates, Scott T.

2015-01-01

Next generation fungal amplicon sequencing is being used with increasing frequency to study fungal diversity in various ecosystems; however, the influence of sample preparation on the characterization of fungal community is poorly understood. We investigated the effects of four procedural modifications to library preparation for high-throughput sequencing (HTS). The following treatments were considered: 1) the amount of soil used in DNA extraction, 2) the inclusion of additional steps (freeze/thaw cycles, sonication, or hot water bath incubation) in the extraction procedure, 3) the amount of DNA template used in PCR, and 4) the effect of sample pooling, either physically or computationally. Soils from two different ecosystems in Minnesota, USA, one prairie and one forest site, were used to assess the generality of our results. The first three treatments did not significantly influence observed fungal OTU richness or community structure at either site. Physical pooling captured more OTU richness compared to individual samples, but total OTU richness at each site was highest when individual samples were computationally combined. We conclude that standard extraction kit protocols are well optimized for fungal HTS surveys, but because sample pooling can significantly influence OTU richness estimates, it is important to carefully consider the study aims when planning sampling procedures. PMID:25974078

Adsorption characterization of gaseous volatile organic compound on mesoporous silica particles prepared from spent diatomaceous earth.

PubMed

Bei, Lei-Lei; Tao, Hong; Ma, Chih-Ming; Shiue, Angus; Chang, Chang-Tang

2014-04-01

This study used spent diatomaceous earth (SDE) from drink processing as source of Si and cationic surfactant (CTAB) as a template for the synthesis of mesoporous silica Materials (MSM) through hydrothermal method. The MSM was characterized by Small-angle X-ray Diffraction (SXRD), Scanning Electron Microscopy (SEM), Thermo Gravimetric Analysis (TGA), Fourier Transform Infrared (FT-IR) spectroscopy and N2 adsorption-desorption analyzer. The results showed that the surface area, pore volume and pore size was roughly ranged from 880 to 1060 m2 g(-1), 1.05 cm3 g(-1) and 4.0 nm, respectively. The properties of the synthesized MSM were also compared with those prepared from pure silica sources (MCM-41) and got almost the same characteristics. The synthesized MSM was used as adsorbent at 25 degrees C with carrier gas of air. The adsorption equilibrium revealed that adsorption capacity of MSM was 59.6, 65.7, 69.6, 84.9 mg g(-1) while the acetone concentration was 600, 800, 1000 ppm, 1600 ppm respectively. Results showed that breakthrough curves correlate to the challenge vapor concentration, adsorbent loading, and the flow rate. The results obtained in the present work demonstrated that it was feasibility of using the SDE as a potential source of silica to prepare MSM.

Monolithic Solid Based on Single-Walled Carbon Nanohorns: Preparation, Characterization, and Practical Evaluation as a Sorbent.

PubMed

Fresco-Cala, Beatriz; López-Lorente, Ángela I; Cárdenas, Soledad

2018-05-25

A monolithic solid based solely on single walled carbon nanohorns (SWNHs) was prepared without the need of radical initiators or gelators. The procedure involves the preparation of a wet jelly-like system of pristine SWNHs followed by slow drying (48 h) at 25 °C. As a result, a robust and stable porous network was formed due to the interaction between SWNHs not only via π-π and van der Waals interactions, but also via the formation of carbon bonds similar to those observed within dahlia aggregates. Pristine SWNHs and the SWNH monolith were characterized by several techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), confocal laser scanning microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and nitrogen intrusion porosimetry. Taking into account the efficiency of carbon nanoparticles in sorption processes, the potential applicability of the SWNH-monolith in this research field was explored using toluene; m-, p-, and o-xylene; ethylbenzene; and styrene, as target analytes. Detection limits were 0.01 µg·L -1 in all cases and the inter-day precision was in the interval 7.4⁻15.7%. The sorbent performance of the nanostructured monolithic solid was evaluated by extracting the selected compounds from different water samples with recovery values between 81.5% and 116.4%.

Preparation and characterization of copper telluride thin films by modified chemical bath deposition (M-CBD) method

NASA Astrophysics Data System (ADS)

Pathan, H. M.; Lokhande, C. D.; Amalnerkar, D. P.; Seth, T.

2003-09-01

Copper telluride thin films were deposited using modified chemical method using copper(II) sulphate; pentahydrate [CuSO 4·5H 2O] and sodium tellurite [Na 2TeO 3] as cationic and anionic sources, respectively. Modified chemical method is based on the immersion of the substrate into separately placed cationic and anionic precursors. The preparative conditions such as concentration, pH, immersion time, immersion cycles, etc. were optimized to get good quality copper telluride thin films at room temperature. The films have been characterized for structural, compositional, optical and electrical transport properties by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), Rutherford back scattering (RBS), optical absorption/transmission, electrical resistivity and thermoemf measurement techniques.

Optically active substituted polyacetylene@carbon nanotube hybrids: Preparation, characterization and infrared emissivity property study

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

Bu, Xiaohai; Zhou, Yuming, E-mail: ymzhou@seu.edu.cn; Zhang, Tao

Optically active substituted polyacetylene@multiwalled carbon nanotubes (SPA@MWCNTs) nanohybrids were fabricated by wrapping helical SPA copolymers onto the surface of modified nanotubes through ester bonding linkage. SPA copolymer based on chiral phenylalanine and serine was pre-polymerized by a rhodium zwitterion catalyst in THF, and evidently proved to possess strong optical activity and adopt a predominately one-handed helical conformation. Various characterizations including Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and transmission electron microscopy (TEM) demonstrated that the SPA had been covalently grafted onto the nanotubes without destroying their original graphite structure. The wrapped SPA was found tomore » exhibit an enhancement in thermal stability and still maintained considerable optical activity after grafting. The infrared emissivity property of the nanohybrids at 8–14 μm was investigated in addition. The results indicated that the SPA@MWCNTs hybrid matrix could possess a much lower infrared emissivity value (ε=0.707) than raw MWCNTs, which might be due to synergistic effect of the unique helical conformation of optically active SPA and strengthened interfacial interaction between the organic polymers and inorganic nanoparticles. - Graphical abstract: Optically active SPA@MWCNTs nanohybrids with low infrared emissivity. - Highlights: • Synthesis of optically active SPA copolymer derived from serine and phenylalanine. • Preparation and characterization of optically active SPA@MWCNTs nanohybrids. • Application study of the SPA@MWCNTs nanohybrids (ε=0.707) in lowering the infrared emissivity.« less

Preparation and Characterization of Biochars from Eichornia crassipes for Cadmium Removal in Aqueous Solutions.

PubMed

Li, Feng; Shen, Kaixuan; Long, Xiaolin; Wen, Jiasheng; Xie, Xiaojie; Zeng, Xiangyun; Liang, Yanyan; Wei, Yansha; Lin, Zefeng; Huang, Wenrou; Zhong, Ruida

2016-01-01

The study investigated the preparation and characterization of biochars from water hyacinth at 300°C to 700°C for cadmium (Cd) removal from aqueous solutions. The adsorption process was dominated by oxygen-containing functional groups with irregular surfaces via esterification reactions. Furthermore, the mineral components in the biochars also contributed to Cd absorption through precipitation. Parameters such as the effects of solution pH, contact time, and initial concentration were studied. The optimum pH value was observed at 5.0, in which nearly 90% of Cd was removed. The maximum Cd adsorption capacities based on the Langmuir isotherm were calculated at 49.837, 36.899, and 25.826 mg g(-1). The adsorption processes of the biochars followed the pseudo-second-order kinetics, with the equilibrium achieved around 5 h. The biochar from E. crassipes is a promising adsorbent for the treatment of wastewater, which can in turn convert one environmental problem to a new cleaning Technology.

Preparation and Characterization of Biochars from Eichornia crassipes for Cadmium Removal in Aqueous Solutions

PubMed Central

Li, Feng; Shen, Kaixuan; Long, Xiaolin; Wen, Jiasheng; Xie, Xiaojie; Zeng, Xiangyun; Liang, Yanyan; Wei, Yansha; Lin, Zefeng; Huang, Wenrou; Zhong, Ruida

2016-01-01

The study investigated the preparation and characterization of biochars from water hyacinth at 300°C to 700°C for cadmium (Cd) removal from aqueous solutions. The adsorption process was dominated by oxygen-containing functional groups with irregular surfaces via esterification reactions. Furthermore, the mineral components in the biochars also contributed to Cd absorption through precipitation. Parameters such as the effects of solution pH, contact time, and initial concentration were studied. The optimum pH value was observed at 5.0, in which nearly 90% of Cd was removed. The maximum Cd adsorption capacities based on the Langmuir isotherm were calculated at 49.837, 36.899, and 25.826 mg g−1. The adsorption processes of the biochars followed the pseudo-second-order kinetics, with the equilibrium achieved around 5 h. The biochar from E. crassipes is a promising adsorbent for the treatment of wastewater, which can in turn convert one environmental problem to a new cleaning Technology. PMID:26882239

Preparation and Characterization of Biomass-Derived Advanced Carbon Materials for Lithium-Ion Battery Applications

NASA Astrophysics Data System (ADS)

Hardiansyah, Andri; Chaldun, Elsy Rahimi; Nuryadin, Bebeh Wahid; Fikriyyah, Anti Khoerul; Subhan, Achmad; Ghozali, Muhammad; Purwasasmita, Bambang Sunendar

2018-04-01

In this study, carbon-based advanced materials for lithium-ion battery applications were prepared by using soybean waste-based biomass material, through a straightforward process of heat treatment followed by chemical modification processes. Various types of carbon-based advanced materials were developed. Physicochemical characteristics and electrochemical performance of the resultant materials were characterized systematically. Scanning electron microscopy observation revealed that the activated carbon and graphene exhibits wrinkles structures and porous morphology. Electrochemical impedance spectroscopy (EIS) revealed that both activated carbon and graphene-based material exhibited a good conductivity. For instance, the graphene-based material exhibited equivalent series resistance value of 25.9 Ω as measured by EIS. The graphene-based material also exhibited good reversibility and cyclic performance. Eventually, it would be anticipated that the utilization of soybean waste-based biomass material, which is conforming to the principles of green materials, could revolutionize the development of advanced material for high-performance energy storage applications, especially for lithium-ion batteries application.

Preparation, characterization, and testing of metal-doped carbon xerogels as catalyst for phenol CWAO.

PubMed

Pleşa Chicinaş, Raluca; Coteţ, L Cosmin; Măicăneanu, Andrada; Vasilescu, Mihai; Vulpoi, Adriana

2017-01-01

Co-, Ce-, and Ni-doped carbon xerogels (Me-CX) synthesized by sol-gel method followed by an ion exchange process were used as catalysts for catalytic wet air oxidation (CWAO) of phenol. The prepared catalysts were characterized using TEM, SEM, BET surface area, and XRD. Me-CX catalysts were tested in mild conditions (20-60 °C, atmospheric pressure) in a semi-batch reactor in various reaction conditions (30-60 L/h, 0.05-0.2 g catalysts, 50-175 mg phenol/L). Total organic carbon (TOC) removal efficiency values obtained decrease in the following order Co-CX ≅ Ce-CX > Ni1-CX > K-CX for the catalysts obtained using the same procedure. TOC removal efficiencies of up to 72% were reached in case of Co-CX catalyst at 20 °C, 40 L/h, using 0.15 g catalyst and a solution of 100 mg phenol/L.

Preparation and Characterization of Biomass-Derived Advanced Carbon Materials for Lithium-Ion Battery Applications

NASA Astrophysics Data System (ADS)

Hardiansyah, Andri; Chaldun, Elsy Rahimi; Nuryadin, Bebeh Wahid; Fikriyyah, Anti Khoerul; Subhan, Achmad; Ghozali, Muhammad; Purwasasmita, Bambang Sunendar

2018-07-01

In this study, carbon-based advanced materials for lithium-ion battery applications were prepared by using soybean waste-based biomass material, through a straightforward process of heat treatment followed by chemical modification processes. Various types of carbon-based advanced materials were developed. Physicochemical characteristics and electrochemical performance of the resultant materials were characterized systematically. Scanning electron microscopy observation revealed that the activated carbon and graphene exhibits wrinkles structures and porous morphology. Electrochemical impedance spectroscopy (EIS) revealed that both activated carbon and graphene-based material exhibited a good conductivity. For instance, the graphene-based material exhibited equivalent series resistance value of 25.9 Ω as measured by EIS. The graphene-based material also exhibited good reversibility and cyclic performance. Eventually, it would be anticipated that the utilization of soybean waste-based biomass material, which is conforming to the principles of green materials, could revolutionize the development of advanced material for high-performance energy storage applications, especially for lithium-ion batteries application.

Preparation and characterization of CuO catalyst for the thermolysis treatment of distillery wastewater.

PubMed

Sharma, Deepak; Prajapati, Abhinesh Kumar; Choudhary, Rumi; Kaushal, Rajesh Kumar; Pal, Dharm; Sawarkar, Ashish N

2017-08-16

CuO catalyst was prepared from copper sulfate by alkali precipitation method followed by drying and calcination. Characterization of CuO catalyst using X-ray diffraction, Brunauer-Emmett-Teller, and Barrett-Joyner-Halenda surface area analysis envisaged the effectiveness of CuO as a catalyst for the treatment of biodigester effluent (BDE) emanated from distilleries. The catalytic thermolysis is an efficient advance treatment method for distillery biodigester effluent (BDE). CT treatment of BDE was carried out in a 0.5 dm 3 thermolytic batch reactor using CuO as a catalyst at different pH (1-9), temperatures (80-110°C), and catalyst loadings (1-4 kg/m 3 ). With CuO catalyst, a temperature of 110°C, catalyst loading of 4 kg/m 3 , and pH of 2 was found to be optimal, providing a maximum reduction in chemical oxygen demand of 65%. The settling characteristics at different temperatures of CT-treated sludge were also presented.

Preparation and characterization of a new microwave immobilized poly(2-phenylpropyl)methylsiloxane stationary phase for reversed phase high-performance liquid chromatography.

PubMed

Begnini, Fernanda R; Jardim, Isabel C S F

2013-07-05

A new reversed phase high-performance liquid chromatography (RP-HPLC) stationary phase was prepared and its chromatographic and physical-chemical properties were evaluated. The new stationary phase was prepared with a silica support and poly(2-phenylpropyl)methylsiloxane (PPPMS), a phenyl type polysiloxane copolymer. Since this is a new copolymer and there is little information in the literature, it was submitted to physical-chemical characterization by infrared spectroscopy and thermogravimetry. The chromatographic phase was prepared through sorption and microwave immobilization of the copolymer onto a silica support. The chromatographic performance was evaluated by employing test procedures suggested by Engelhardt and Jungheim, Tanaka and co-workers, Neue, and Szabó and Csató. These test mixtures provide information about the hydrophobic selectivity, silanophilic activity, ion-exchange capacity, shape selectivity and interaction with polar analytes of the new Si-PPPMS reversed phase. Stability tests were developed using accelerated aging tests under both basic and acidic conditions to provide information about the lifetime of the packed columns. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation, characterization and catalytic properties of MCM-48 supported tungstophosphoric acid mesoporous materials for green synthesis of benzoic acid

NASA Astrophysics Data System (ADS)

Wu, Hai-Yan; Zhang, Xiao-Li; Chen, Xi; Chen, Ya; Zheng, Xiu-Cheng

2014-03-01

MCM-48 and tungstophosphoric acid (HPW) were prepared and applied for the synthesis of HPW/MCM-48 mesoporous materials. The characterization results showed that HPW/MCM-48 obtained retained the typical mesopore structure of MCM-48, and the textural parameters decreased with the increase loading of HPW. The catalytic oxidation results of benzyl alcohol and benzaldehyde with 30% H2O2 indicated that HPW/MCM-48 was an efficient catalyst for the green synthesis of benzoic acid. Furthermore, 35 wt% HPW/MCM-48 sample showed the highest activity under the reaction conditions.

Ciprofloxacin HCl-loaded calcium carbonate nanoparticles: preparation, solid state characterization, and evaluation of antimicrobial effect against Staphylococcus aureus.

PubMed

Maleki Dizaj, Solmaz; Lotfipour, Farzaneh; Barzegar-Jalali, Mohammad; Zarrintan, Mohammad-Hossein; Adibkia, Khosro

2017-05-01

Ciprofloxacin HCl-loaded calcium carbonate (CaCO 3 ) nanoparticles were prepared via a w/o microemulsion method and characterized by dynamic light scattering, scanning electron microscopy, X-ray powder diffraction (XRPD) analysis, differential scanning calorimetry (DSC), and Fourier transform infrared spectroscopy (FTIR). The in vitro drug release profiles as well as antimicrobial effect against Staphylococcus aureus (S. aureus) were also evaluated. The antibacterial effect was studied using serial dilution technique to determine the minimum inhibitory concentration (MIC) of the nanoparticles and was confirmed by streak cultures. The mean particle size, drug loading and entrapment efficiency were calculated to be 116.09 nm, 20.49% and 44.05%, respectively. PXRD and FTIR studies confirmed that both vaterite and calcite polymorphs of CaCO 3 were formed during the preparation process. In vitro release profiles of the nanoparticles showed slow release pattern for 12 h. The drug-loaded nanoparticles showed similar MICs against S. aureus compared to untreated drug. However, a preserved antimicrobial effect was observed for drug-loaded nanoparticles compared to untreated drug after 2 days of incubation.

Polyurethane with Tethered Copper(II)-Cyclen Complex: Preparation, Characterization and Catalytic Generation of Nitric Oxide from S-Nitrosothiols

PubMed Central

Hwang, Sangyeul

2008-01-01

The preparation and characterization of a commercial biomedical grade polyurethane (Tecophilic, SP-93A-100) material possessing covalently linked copper(II)-cyclen moieties as a nitric oxide (NO) generating polymer are described. Chemiluminescence NO measurements demonstrate that the prepared polymer can decompose endogenous S-nitrosothiols (RSNOs) such as S-nitrosoglutathione and S-nitrosocysteine to NO in the presence of thiol reducing agents (RSHs; e.g., glutathione and cysteine) at physiological pH. Since such RSNO and RSH already exist in blood, the proposed polymer is capable of spontaneously generating NO when in contact with fresh blood. This is demonstrated by utilizing the polymer as an outer coating at the distal end of an amperometric NO sensor to create a device that generates response toward the RSNO species in the blood. This polymer possesses the combined benefits of a commercial biomedical grade polyurethane with the ability to generate biologically active NO when on contact with blood, and thus may serve as a useful coating to improve the hemocompatibility of various medical devices. PMID:18314189

Preparation, characterization and in vitro anticoagulant activity of corn stover xylan sulfates.

PubMed

Cheng, He-Li; Liu, Hao; Feng, Qing-Hua; Xie, Yi-Min; Zhan, Huai-Yu

2017-02-01

A new anticoagulant agent was prepared by introducing sulfate groups into corn stover xylan through homogeneous reactions. Three organic solvents, N, N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and formamide (FA), were adopted as reaction media, with the assistance of LiCl. Structural characterization by FT-IR and 13 CNMR showed that xylan sulfate (XS) could be successfully synthesized with SO 3 ∙Pyridine (SO 3 ∙Py) complexes sulfation reagent in the three media. The effect of sulfation temperature, sulfation time, media type and molar ratio of -SO 3 /-OH on the degree of substitution (DS) and degree of the polymerization (DP) were studied. DMF/LiCl were more effective than DMSO/LiCl and FA/LiCl in preparation of xylan sulfate with high DS. The optimal conditions for sulfation were obtained when SO 3 ∙Py complex was added to DMF/LiCl with -SO 3 /-OH ratio of 1.5:1 and maintained at 50 °C for 3 h. Degree of polymerization of xylan was decreased during the sulfation process and DMF/LiCl offered the least xylan degradation as compared with DMSO/LiCl or FA/LiCl. Anticoagulant activities of the resultant xylan sulfates with different DS were evaluated by using activated partial thromboplastin time (APTT), thrombin time (TT), and prothrombin time (PT). Results indicated that the introducing of sulfate groups into xylan did endow the polysaccharides with anticoagulant activity. The APTT and TT of XS with DS of 1.20 reached 141 and 45.3 s at a dosage of 20 μg/mL, while the APTT and TT values for the blank sample were only 35.5 and 15.6 s. Furthermore, coagulation time was prolonged with the increase of DS and the concentration of XS. Our findings provide new insights into the value-added utilization of agricultural biomass.

Preparation and characterization of safe microparticles based on xylan.

PubMed

Cartaxo da Costa Urtiga, Silvana; Aquino Azevedo de Lucena Gabi, Camilla; Rodrigues de Araújo Eleamen, Giovanna; Santos Souza, Bartolomeu; Pessôa, Hilzeth de Luna Freire; Marcelino, Henrique Rodrigues; Afonso de Moura Mendonça, Elisângela; Egito, Eryvaldo Sócrates Tabosa do; Oliveira, Elquio Eleamen

2017-10-01

This work describes the preparation and evaluation of safe xylan-based microparticles prepared by cross-linking polymerization using sodium trimetaphosphate. The resulting microparticles were evaluated for morphology, particle size, polymer-cross-link agent interaction, and in vitro toxicity. The microparticles showed narrow monodisperse size distributions with their mean sizes being between 3.5 and 12.5 µm in dried state. FT-IR analyzes confirmed the interaction between sodium trimetaphosphate and xylan during the cross-linking process with formation of phosphate ester bonds. Additionally, the X-ray diffraction patterns and FT-IR analyzes suggested that little or no cross-linking agent remained inside the microparticles. Furthermore, the in-vitro studies using Artemia salina and human erythrocytes revealed that the microparticles are not toxic. Therefore, the overall results suggest that these xylan microparticles can be used as a platform for new drug delivery system.

In Vitro and In Vivo Characterization of Drug Nanoparticles Prepared Using PureNano™ Continuous Crystallizer to Improve the Bioavailability of Poorly Water Soluble Drugs.

PubMed

Tahara, Kohei; Nishikawa, Masahiro; Matsui, Ko; Hisazumi, Koji; Onodera, Risako; Tozuka, Yuichi; Takeuchi, Hirofumi

2016-09-01

The aim of this study was to enhance the dissolution and oral absorption of poorly water-soluble active pharmaceutical ingredients (APIs) using nanoparticle suspensions prepared with a PureNano™ continuous crystallizer (PCC). Nanoparticle suspensions were prepared with a PCC, which is based on microfluidics reaction technology and solvent-antisolvent crystallization. Phenytoin, bezafibrate, flurbiprofen, and miconazole were used as model APIs. These APIs were dissolved in ethanol and precipitated by the addition of water and polyvinyl alcohol. Batch crystallization (BC) using a beaker was also performed to prepare the suspensions. Both PCC and BC formulations were freeze-dried before being characterized in vitro and in vivo. The particle sizes of the nanoparticle suspensions prepared with the PCC were smaller than those prepared by BC. The dissolution rate of each API in vitro significantly increased after crystallization. Reducing the particle size of either the BC or PCC formulation led to increased API flux across Caco-2 cell monolayers. PCC preparations showed higher plasma concentrations after oral administration, demonstrating the advantages of a fast dissolution rate and increased interaction with the gastrointestinal tract owing to the smaller particle size. PCC can continuously produce nanoparticle APIs and is an efficient approach for improving their oral bioavailability.

[Preparation and characterization of monoclonal antibodies against Micrococcus luteus Rpf domain].

PubMed

Fan, Ai-lin; Shi, Chang-hong; Su, Ming-quan; Ma, Jing; Bai, Yin-lan; Cheng, Xiao-dong; Xu, Zhi-kai; Hao, Xiao-ke

2008-05-01

To express Micrococcus luteus Rpf domain in prokaryotic cells and prepare monoclonal antibodies against Rpf domain. The gene encoding Micrococcus luteus Rpf domain was amplified from genome of Micrococcus luteus by polymerase chain reaction(PCR), and inserted into cloning vector pUC-19. After sequenced, Micrococcus luteus Rpf domain gene was subcloned into the expression vector pPro-EXHT and transfected into E.coli DH5alpha. After induced by IPTG, the bacteria controlled by T7 promoter expressed the fused Micrococcus luteus Rpf domain protein with a hexahistidine tail at its N-terminal and the target protein was purified under denaturing conditions. Using this protein as antigen to immunize the BALB/c mice and prepare monoclonal antibodies against Micrococcus luteus Rpf domain. Then specifities and relative affinities of mAbs were identified by ELISA. The fusion protein was purified by metal chelate affinity chromatography under denaturing condition. Three cloned mAbs were prepared from the mice immunized by Rpf domain. All of them could recognize Rpf domain. specifically. The prepared mAbs against Rpf domain have strong specificity with high titers, which provides useful tools for further study of the function of Rpf domain in TB prevention.

The Preparation and Structural Characterization of Three Structural Types of Gallium Compounds Derived from Gallium (II) Chloride

NASA Technical Reports Server (NTRS)

Gordon, Edward M.; Hepp, Aloysius F.; Duraj. Stan A.; Habash, Tuhfeh S.; Fanwick, Phillip E.; Schupp, John D.; Eckles, William E.; Long, Shawn

1997-01-01

The three compounds Ga2Cl4(4-mepy)2 (1),[GaCl2(4-mepy)4]GaCl4x1/2(4-mepy); (2) and GaCl2(4-mepy)2(S2CNEt2); (3) (4-mepy= 4-methylpyridine) have been prepared from reactions of gallium (II) chloride in 4-methylpyridine and characterized by single-crystal X-ray analysis. Small variations in the reaction conditions for gallium(II) chloride can produce crystals with substantially different structural properties. The three compounds described here encompass a neutral gallium(II) dimer in which each gallium is four-coordinate, an ionic compound containing both anionic and cationic gallium complex ions with different coordination numbers and a neutral six-coordinate heteroleptic

Preparation and characterization of cross-linked poly (vinyl alcohol)-graphene oxide nanocomposites as an interlayer for Schottky barrier diodes

NASA Astrophysics Data System (ADS)

Badrinezhad, Lida; Bilkan, Çigdem; Azizian-Kalandaragh, Yashar; Nematollahzadeh, Ali; Orak, Ikram; Altindal, Şemsettin

2018-01-01

Cross-linked polyvinyl alcohol (PVA) graphene oxide (GO) nanocomposites were prepared by simple solution-mixing route and characterized by Raman, UV-visible and fourier transform infrared (FT-IR) spectroscopy analysis, X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The XRD pattern and SEM analysis showed significant changes in the nanocomposite structures, and the FT-IR spectroscopy results confirmed the chemical interaction between the GO filler and the PVA matrix. After these morphological characterizations, PVA-GO-based diodes were fabricated and their electrical properties were characterized using current-voltage (I-V) and impedance-voltage-frequency (Z-V-f) measurements at room temperature. Semilogarithmic I-V characteristics of diode showed a good rectifier behavior. The values of C and G/ω increased with decreasing frequency due to the surface/interface states (Nss) which depend on the relaxation time and the frequency of the signal. The voltage, dependent profiles of Nss and series resistance (Rs) were obtained from the methods of high-low frequency capacitance and Nicollian and Brews, respectively. The obtained values of Nss and Rs were attributed to the use of cross-linked PVA-GO interlayer at the Au/n-Si interface.

Alginate-perlite encapsulated Pseudomonas putida A (ATCC 12633) cells: Preparation, characterization and potential use as plant inoculants.

PubMed

Liffourrena, Andrés S; Lucchesi, Gloria I

2018-04-30

Microbial immobilization can be used to prepare encapsulated inoculants. Here, we characterize and describe the preparation of Ca-alginate-perlite microbeads loaded with cells of plant growth-promoting Pseudomonas putida A (ATCC 12633), for their future application as agricultural inoculants. The microbeads were prepared by dropwise addition of a CaCl 2 -paraffin emulsion mixture to an emulsion containing alginate 2% (w/v), perlite 0.1-0.4% (w/v) and bacterial suspension in 0.9% NaCl (10 10  CFU/mL). For all perlite concentrations used, microbead size was 90-120 μm, the trapped population was 10 8  CFU/g microbeads and the increase in mechanical stability was proportional to perlite concentration. Microbeads containing 0.4% (w/v) perlite were able to release bacteria into the medium after 30 days of incubation. When we evaluated how P. putida A (ATCC 12633) entrapped in Ca-alginate-perlite (0.4% (w/v)) microbeads colonized the Arabidopsis thaliana rhizosphere, an increase in colonization over time was detected (from an initial 2.1 × 10 4 to 9.2 × 10 5  CFU/g soil after 21 days). With this treatment, growth promotion of A. thaliana occurred with an increase in the amount of proteins, and in root and leaf biomass. It was concluded that the microbeads could be applied as possible inoculants, since they provide protection and a controlled release of microorganisms into the rhizosphere. Copyright © 2018. Published by Elsevier B.V.

Preparation and characterization of bioadhesive system containing hypericin for local photodynamic therapy.

PubMed

Borghi-Pangoni, Fernanda Belincanta; Junqueira, Mariana Volpato; de Souza Ferreira, Sabrina Barbosa; Silva, Larissa Lachi; Rabello, Bruno Ribeiro; de Castro, Lidiane Vizioli; Baesso, Mauro Luciano; Diniz, Andréa; Caetano, Wilker; Bruschi, Marcos Luciano

2017-09-01

Hypericin (Hyp) is a natural photoactive pigment utilized in the treatment of different types of cancer and antimicrobial inactivation using photodynamic therapy (PDT). Hyp is poorly soluble in water leading to problems of administration, getting close contact with the site, and bio-availability. Therefore, this study aimed to develop bioadhesive thermoresponsive system containing Hyp for local PDT. Carbomer 934P, poloxamer 407, and Hyp were used to prepare the thermoresponsive bioadhesive formulations. They were characterized for sol-gel transition temperature, mechanical, mucoadhesive, rheological (continuous flow and oscillatory) and dielectric properties, syringeability, in vitro Hyp release kinetics, ex vivo permeability, and photodynamic activity. The formulations displayed suitable gelation temperature and rheological characteristics. The compressional, mechanical and mucoadhesive properties, as well the syringeability showed the easiness of administration and the permanence of the system adhered to the mucosa or skin. The dielectric analysis helped to understand the Hyp availability, and its release presented an anomalous behavior. The system did not permeate the pig skin nor rat intestine and showed good biological photodynamic activity. Therefore, data obtained from the bioadhesive system indicate a potentially useful role as a platform for local hypericin delivery in PDT, suggesting it is worthy of in vivo evaluation. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and characterization of bee venom-loaded PLGA particles for sustained release.

PubMed

Park, Min-Ho; Jun, Hye-Suk; Jeon, Jong-Woon; Park, Jin-Kyu; Lee, Bong-Joo; Suh, Guk-Hyun; Park, Jeong-Sook; Cho, Cheong-Weon

2016-12-14

Bee venom-loaded poly(lactic-co-glycolic acid) (PLGA) particles were prepared by double emulsion-solvent evaporation, and characterized for a sustained-release system. Factors such as the type of organic solvent, the amount of bee venom and PLGA, the type of PLGA, the type of polyvinyl alcohol, and the emulsification method were considered. Physicochemical properties, including the encapsulation efficiency, drug loading, particle size, zeta-potential and surface morphology were examined by Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), and X-ray diffraction (XRD). The size of the bee venom-loaded PLGA particles was 500 nm (measured using sonication). Zeta-potentials of the bee venom-loaded PLGA particles were negative owing to the PLGA. FT-IR results demonstrated that the bee venom was completely encapsulated in the PLGA particles, indicated by the disappearance of the amine and amide peaks. In addition, sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis indicated that the bee venom in the bee venom-loaded PLGA particles was intact. In vitro release of the bee venom from the bee venom-loaded PLGA particles showed a sustained-release profile over 1 month. Bee venom-loaded PLGA particles can help improve patients' quality of life by reducing the number of injections required.

Theoretical studies of Pt-Ti nanoparticles for potential use as PEMFC electrocatalysts.

PubMed

Jennings, Paul C; Pollet, Bruno G; Johnston, Roy L

2012-03-07

A theoretical investigation is presented of alloying platinum with titanium to form binary Pt-Ti nanoalloys as an alternative to the expensive pure platinum catalysts commonly used for Proton Exchange Membrane Fuel Cell cathode electrocatalysts. Density Functional Theory calculations are performed to investigate compositional effects on structural properties as well as Oxygen Reduction Reaction kinetics and poisoning effects. High symmetry A(32)-B(6) clusters are studied to investigate structural properties. From these structures binding energies of hydroxyl and carbon monoxide are studied on a range of sites on the surface of the clusters. Promising results are obtained suggesting that the bimetallic Pt-Ti nanoalloys may exhibit enhanced properties compared to pure platinum catalysts.

Intracerebral Cell Implantation: Preparation and Characterization of Cell Suspensions.

PubMed

Rossetti, Tiziana; Nicholls, Francesca; Modo, Michel

2016-01-01

Intracerebral cell transplantation is increasingly finding a clinical translation. However, the number of cells surviving after implantation is low (5-10%) compared to the number of cells injected. Although significant efforts have been made with regard to the investigation of apoptosis of cells after implantation, very little optimization of cell preparation and administration has been undertaken. Moreover, there is a general neglect of the biophysical aspects of cell injection. Cell transplantation can only be an efficient therapeutic approach if an optimal transfer of cells from the dish to the brain can be ensured. We therefore focused on the in vitro aspects of cell preparation of a clinical-grade human neural stem cell (NSC) line for intracerebral cell implantation. NSCs were suspended in five different vehicles: phosphate-buffered saline (PBS), Dulbecco's modified Eagle medium (DMEM), artificial cerebral spinal fluid (aCSF), HypoThermosol, and Pluronic. Suspension accuracy, consistency, and cell settling were determined for different cell volume fractions in addition to cell viability, cell membrane damage, and clumping. Maintenance of cells in suspension was evaluated while being stored for 8 h on ice, at room temperature, or physiological normothermia. Significant differences between suspension vehicles and cellular volume fractions were evident. HypoThermosol and Pluronic performed best, with PBS, aCSF, and DMEM exhibiting less consistency, especially in maintaining a suspension and preserving viability under different storage conditions. These results provide the basis to further investigate these preparation parameters during the intracerebral delivery of NSCs to provide an optimized delivery process that can ensure an efficient clinical translation.

Preparation and characterization of Phase change material microcapsules by a core-shell-like emulsion polymerization method

NASA Astrophysics Data System (ADS)

Ding, Li-ming; Pei, Guang-ling

2015-07-01

Phase change material microcapsules (MicroPCMs) were synthesized by a coreshell-like emulsion polymerization method. Styrene and methylacrylic acid copolymer (PS- MAA) was used as a wall material, and paraffin was used as a core material in order to prepare spherical, high resistance and high enthalpy MicroPCMs. Scanning Electron Microscope (SEM), laser particle size analyzer, Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetry (TG) and Differential Scanning Calorimeter (DSC) were employed to characterize the MicroPCMs. The results indicated that the average particle size of MicroPCMs was 42.29 μm, and the content of paraffin within microcapsules was 57.6%. The melting temperature and crystallization temperature were 30.7°C and 25.2°C.The melting enthalpy and crystallization enthalpy were -84.1 J/g and 91.3 J/g, respectively.

Tuning the onset of ferromagnetism in heterogeneous bimetallic nanoparticles by gas phase doping

NASA Astrophysics Data System (ADS)

Bohra, Murtaza; Grammatikopoulos, Panagiotis; Singh, Vidyadhar; Zhao, Junlei; Toulkeridou, Evropi; Steinhauer, Stephan; Kioseoglou, Joseph; Bobo, Jean-François; Nordlund, Kai; Djurabekova, Flyura; Sowwan, Mukhles

2017-11-01

In the nanoregime, chemical species can reorganize in ways not predicted by their equilibrium bulk behavior. Here, we engineer Ni-Cr nanoalloys at the magnetic end of their compositional range (i.e., 0-15 at. % Cr), and we investigate the effect of Cr incorporation on their structural stability and resultant magnetic ordering. To ensure their stoichiometric compositions, the nanoalloys are grown by cluster beam deposition, a method that allows one-step, chemical-free fabrication of bimetallic nanoparticles. While full Cr segregation toward nanoparticle surfaces is thermodynamically expected for low Cr concentrations, metastability occurs as the Cr dopant level increases in the form of residual Cr in the core region, yielding desirable magnetic properties in a compensatory manner. Using nudged elastic band calculations, residual Cr in the core is explained based on modifications in the local environment of individual Cr atoms. The resultant competition between ferromagnetic and antiferromagnetic ordering gives rise to a wide assortment of interesting phenomena, such as a cluster-glass ground state at very low temperatures and an increase in Curie temperature values. We emphasize the importance of obtaining the commonly elusive magnetic nanophase diagram for M -Cr (M =Fe , Co, and Ni) nanoalloys, and we propose an efficient single-parameter method of tuning the Curie temperature for various technological applications.

Preparation and Characterization of Cellulose Gels from Corn Cobs

USDA-ARS?s Scientific Manuscript database

Aqueous cellulose gels were prepared by extraction of ground corn cobs with hot aqueous sodium hydroxide/sodium hypochlorite and shearing. Initial shearing in a blender broke up cob tissue structure into individual cells and resulted in a gel. Subsequent shearing in a high pressure homogenizer incre...

Preparation and characterization of cellulose gels from corn cobs

USDA-ARS?s Scientific Manuscript database

Aqueous cellulose gels were prepared by extraction of ground corn cobs with hot aqueous sodium hydroxide/sodium hypochlorite and shearing. Initial shearing in a blender broke up cob tissue structure into individual cells and resulted in a gel. Subsequent shearing in a high pressure homogenizer incre...

Optical characterization of composite layers prepared by plasma polymerization

NASA Astrophysics Data System (ADS)

Radeva, E.; Hikov, T.; Mitev, D.; Stroescu, H.; Nicolescu, M.; Gartner, M.; Presker, R.; Pramatarova, L.

2016-02-01

Thin composite layers from polymer/nanoparticles (Ag-nanoparticles and detonation nanodiamonds) were prepared by plasma polymerization process on the base of hexamethyldisiloxane. The variation of the layer composition was achieved by changing the type of nanoparticles. The optical measurement techniques used were UV-VIS-NIR ellipsometry (SE), Fourier-transformed infrared spectroscopy (FTIR) and Raman spectroscopy. The values of the refractive index determined are in the range 1.30 to 1.42. All samples are transparent with transmission between 85-95% and very smooth. The change in Raman and FTIR spectra of the composites verify the expected bonding between polymer and diamond nanoparticles due to the penetration of the fillers in the polymer matrix. The comparison of the spectra of the corresponding NH3 plasma treated composites revealed that the composite surface becomes more hydrophilic. The obtained results indicate that preparation of layers with desired compositions is possible at a precise control of the detonation nanodiamond materials.

Porous Nanocrystalline Silicon Supported Bimetallic Pd-Au Catalysts: Preparation, Characterization, and Direct Hydrogen Peroxide Synthesis

PubMed Central

Potemkin, Dmitriy I.; Maslov, Dmitry K.; Loponov, Konstantin; Snytnikov, Pavel V.; Shubin, Yuri V.; Plyusnin, Pavel E.; Svintsitskiy, Dmitry A.; Sobyanin, Vladimir A.; Lapkin, Alexei A.

2018-01-01

Bimetallic Pd-Au catalysts were prepared on the porous nanocrystalline silicon (PSi) for the first time. The catalysts were tested in the reaction of direct hydrogen peroxide synthesis and characterized by standard structural and chemical techniques. It was shown that the Pd-Au/PSi catalyst prepared from conventional H2[PdCl4] and H[AuCl4] precursors contains monometallic Pd and a range of different Pd-Au alloy nanoparticles over the oxidized PSi surface. The PdAu2/PSi catalyst prepared from the [Pd(NH3)4][AuCl4]2 double complex salt (DCS) single-source precursor predominantly contains bimetallic Pd-Au alloy nanoparticles. For both catalysts the surface of bimetallic nanoparticles is Pd-enriched and contains palladium in Pd0 and Pd2+ states. Among the catalysts studied, the PdAu2/PSi catalyst was the most active and selective in the direct H2O2 synthesis with H2O2 productivity of 0.5 mol gPd-1 h-1 at selectivity of 50% and H2O2 concentration of 0.023 M in 0.03 M H2SO4-methanol solution after 5 h on stream at −10°C and atmospheric pressure. This performance is due to high activity in the H2O2 synthesis reaction and low activities in the undesirable H2O2 decomposition and hydrogenation reactions. Good performance of the PdAu2/PSi catalyst was associated with the major part of Pd in the catalyst being in the form of the bimetallic Pd-Au nanoparticles. Porous silicon was concluded to be a promising catalytic support for direct hydrogen peroxide synthesis due to its inertness with respect to undesirable side reactions, high thermal stability, and conductivity, possibility of safe operation at high temperatures and pressures and a well-established manufacturing process. PMID:29637068

Characterization and phenol adsorption performance of activated carbon prepared from tea residue by NaOH activation.

PubMed

Tao, Jun; Huo, Peili; Fu, Zongheng; Zhang, Jin; Yang, Zhen; Zhang, Dengfeng

2017-10-05

The preparation of activated carbon (AC) using tea residue was addressed in this work. The preparation process incorporated two-step pyrolysis and activation using NaOH. The influence of activation temperature between 500°C and 700°C on the properties of the AC sample was investigated. The physicochemical properties of the AC sample were characterized. The results show that the optimum temperature for the activation process is 700°C, which generates the AC sample with higher specific surface area and total pore volume, respectively, of 819 m 2  g -1 and 0.443 cm 3  g -1 . The oxygen-containing functional groups evolve on the AC sample during the activation process. The phenol adsorption test was performed to evaluate the adsorption performance of the AC sample. The adsorption data confirm that phenol adsorption on the AC sample obtained at 700°C follows the pseudo-second-order kinetics model. Hereby, the electron donor-acceptor interaction mechanism can describe the adsorption process. The AC sample obtained at 700°C performs superior phenol adsorption performance. The maximum phenol adsorption capacity is 320 mg g -1 , which is higher than that of several AC samples reported previously. Thus, the tea residue acts as a good precursor for the AC with promising adsorption capacity by the NaOH chemical activation method.

Preparation and characterization of Fe3O4@Au-C225 composite targeted nanoparticles for MRI of human glioma

PubMed Central

Ge, Yaoqi; Zhong, Yuejiao; Ji, Guozhong; Lu, Qianling; Dai, Xinyu; Guo, Zhirui; Zhang, Peng; Peng, Gang; Zhang, Kangzhen; Li, Yuntao

2018-01-01

Objective To study the characterization of Fe3O4@Au-C225 composite targeted MNPs. Methods Fe3O4@Au-C225 was prepared by the absorption method. The immunosorbent assay was used to evaluate its absorption efficiency at C225 Fc. ZETA SIZER3000 laser particle size analyzer, ultraviolet photometer and its characteristics were analyzed by VSM. the targeting effect of Fe3O4@Au-C225 composite targeted MNPs on U251 cells in vitro were detected by 7.0 Tesla Micro-MR; and subcutaneous transplanted human glioma in nude mice were performed the targeting effect in vivo after tail vein injection of Fe3O4@Au-C225 composite targeted MNPs by MRI. Results The self-prepared Fe3O4@Au composite MNPs can adsorb C225 with high efficiency of adsorption so that Fe3O4@Au-C225 composite targeted MNPs were prepared successfully. Fe3O4@Au-C225 composite targeted MNPs favorably targeted human glioma cell line U251 in vitro; Fe3O4@Au-C225 composite targeted MNPs have good targeting ability to xenografted glioma on nude mice in vivo, and can be traced by MRI. Conclusion The Fe3O4@Au-C225 composite targeted MNPs have the potential to be used as a tracer for glioma in vivo. PMID:29652919

Preparation and characterization of Fe3O4@Au-C225 composite targeted nanoparticles for MRI of human glioma.

PubMed

Ge, Yaoqi; Zhong, Yuejiao; Ji, Guozhong; Lu, Qianling; Dai, Xinyu; Guo, Zhirui; Zhang, Peng; Peng, Gang; Zhang, Kangzhen; Li, Yuntao

2018-01-01

To study the characterization of Fe3O4@Au-C225 composite targeted MNPs. Fe3O4@Au-C225 was prepared by the absorption method. The immunosorbent assay was used to evaluate its absorption efficiency at C225 Fc. ZETA SIZER3000 laser particle size analyzer, ultraviolet photometer and its characteristics were analyzed by VSM. the targeting effect of Fe3O4@Au-C225 composite targeted MNPs on U251 cells in vitro were detected by 7.0 Tesla Micro-MR; and subcutaneous transplanted human glioma in nude mice were performed the targeting effect in vivo after tail vein injection of Fe3O4@Au-C225 composite targeted MNPs by MRI. The self-prepared Fe3O4@Au composite MNPs can adsorb C225 with high efficiency of adsorption so that Fe3O4@Au-C225 composite targeted MNPs were prepared successfully. Fe3O4@Au-C225 composite targeted MNPs favorably targeted human glioma cell line U251 in vitro; Fe3O4@Au-C225 composite targeted MNPs have good targeting ability to xenografted glioma on nude mice in vivo, and can be traced by MRI. The Fe3O4@Au-C225 composite targeted MNPs have the potential to be used as a tracer for glioma in vivo.

Preparation and Characterization of Cellulose and Nanocellulose from Agro-industrial Waste - Cassava Peel

NASA Astrophysics Data System (ADS)

Widiarto, S.; Yuwono, S. D.; Rochliadi, A.; Arcana, I. M.

2017-02-01

Cassava peel is an agro-industrial waste which is available in huge quantities in Lampung Province of Indonesia. This work was conducted to evaluate the potential of cassava peel as a source of cellulose and nanocellulose. Cellulose was extracted from cassava peel by using different chemical treatment, and the nanocellulose was prepared by hydrolysis with the use of sulfuric acid. The best methods of cellulose extraction from cassava peels are using alkali treatment followed by a bleaching process. The cellulose yield from this methods was 17.8% of dry base cassava peel, while the yield from nitric and sulfuric methods were about 10.78% and 10.32% of dry base cassava peel respectively. The hydrolysis was performed at the temperature of 50 °C for 2 hours. The intermediate reaction product obtained after each stage of the treatments was characterized. Fourier transform infrared spectroscopy showed the removal of non-cellulosic constituent. X-ray Diffraction (XRD) analysis revealed that the crystallinity of cellulose increased after hydrolysis. Morphological investigation was performed using Scanning Electron Microscopy (SEM). The size of particle was confirmed by Particle Size Analyzer (PSA) and Transmission Electron Microscopy (TEM).

Preparation and Characterization of Space Durable Polymer Nanocomposite Films from Functionalized Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Delozier, D. M.; Connell, J. W.; Smith, J. G.; Watson, K. A.

2003-01-01

Low color, flexible, space durable polyimide films with inherent, robust electrical conductivity have been under investigation as part of a continuing materials development activity for future NASA space missions involving Gossamer structures. Electrical conductivity is needed in these films to dissipate electrostatic charge build-up that occurs due to the orbital environment. One method of imparting conductivity is through the use of single walled carbon nanotubes (SWNTs). However, the incompatibility and insolubility of the SWNTs severely hampers their dispersion in polymeric matrices. In an attempt to improve their dispersability, SWNTs were functionalized by the reaction with an alkyl hydrazone. After this functionalization, the SWNTs were soluble in select solvents and dispersed more readily in the polymer matrix. The functionalized SWNTs were characterized by Raman spectroscopy and thermogravimetric analysis (TGA). The functionalized nanotubes were dispersed in the bulk of the films using a solution technique. The functionalized nanotubes were also applied to the surface of polyimide films using a spray coating technique. The resultant polyimide nanocomposite films were evaluated for nanotube dispersion, electrical conductivity, mechanical, and optical properties and compared with previously prepared polyimide-SWNT samples to assess the effects of SWNT functionalization.

Preparation and Characterization of Niobium Doped Lead-Telluride Glass Ceramics

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

Sathish, M.; Eraiah, B.; Anavekar, R. V.

2011-07-15

Niobium-lead-telluride glass ceramics of composition xNb{sub 2}O{sub 5}-(20-x) pbO-80TeO{sub 2}(where x = 0.1 mol% to 0.5 mol%) were prepared by using conventional melt quenching method. The prepared glass samples were initially amorphous in nature after annealed at 400 deg. c all samples were crystallized. This was confined by X-ray diffraction and scanning electron microscopy. The particle size of these glass ceramics have been calculated by using Debye-Scherer formula and the particle size is in the order of 15 nm to 60 nm. The scanning electron microscopy (SEM) photograph shows the presence of needle-like crystals in these samples.

Preparation, characterization and biological activity of novel metal-NNNN donor Schiff base complexes

NASA Astrophysics Data System (ADS)

Mohamed, Gehad G.; Omar, M. M.; Ibrahim, Amr A.

2010-02-01

Novel Schiff base (H 2L) ligand is prepared via condensation of benzil and triethylenetetraamine. The ligand is characterized based on elemental analysis, mass, IR and 1H NMR spectra. Metal complexes are reported and characterized based on elemental analyses, IR, 1H NMR, solid reflectance, magnetic moment, molar conductance, and thermal analyses (TG, DTG and DTA). 1:1 [M]:[H 2L] complexes are found from the elemental analyses data having the formulae [M(H 2L)Cl 2]· yH 2O (M = Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II)), [Fe(H 2L)Cl 2]Cl·H 2O, [Th(H 2L)Cl 2]Cl 2·3H 2O and [UO 2(H 2L)](CH 3COO) 2·2H 2O. The metal chelates are found to be non-electrolytes except Fe(III), Th(IV) and UO 2(II) complexes are electrolytes. IR spectra show that H 2L is coordinated to the metal ions in a neutral tetradentate manner with 4Ns donor sites of the two azomethine N and two NH groups. The geometrical structures of these complexes are found to be octahedral. The thermal behaviour of these chelates is studied where the hydrated complexes lose water molecules of hydration in the first step followed immediately by decomposition of the anions and ligand molecules in the subsequent steps. The activation thermodynamic parameters are calculated using Coats-Redfern method. The ligand (H 2L), in comparison to its metal complexes, is screened for its antibacterial activity. The activity data show that the metal complexes have antibacterial activity more than the parent Schiff base ligand and cefepime standard against one or more bacterial species.

Preparation and characterization of corn cob activated carbon coated with nano-sized magnetite particles for the removal of Cr(VI).

PubMed

Nethaji, S; Sivasamy, A; Mandal, A B

2013-04-01

Activated carbon prepared from corn cob biomass, magnetized by magnetite nanoparticles (MCCAC) was used for the adsorption of hexavalent chromium from aqueous solution. The adsorbent was characterized by SEM, TEM, XRD, VSM, surface functionality and zero-point charge. The iron oxide nanoparticles were of 50 nm sizes and the saturation magnetization value for the adsorbent is 48.43 emu/g. Adsorption was maximum at pH 2. Isotherm data were modeled using Langmuir, Freundlich and Temkin isotherm. The prepared MCCAC had a heterogeneous surface. The maximum monolayer adsorption capacity was 57.37 mg/g. Kinetic studies were carried out and the data fitted the pseudo second-order equation. The mechanism of the adsorption process was studied by incorporating the kinetic data with intraparticle diffusion model, Bangham equation and Boyd plot. The adsorption was by chemisorption and the external mass transfer was the rate-determining step. A micro column was designed and the basic column parameters were estimated. Copyright © 2013 Elsevier Ltd. All rights reserved.

L-Cysteine capped CdTe-CdS core-shell quantum dots: preparation, characterization and immuno-labeling of HeLa cells.

PubMed

Zhang, Hongyan; Sun, Pan; Liu, Chang; Gao, Huanyu; Xu, Linru; Fang, Jin; Wang, Meng; Liu, Jinling; Xu, Shukun

2011-01-01

Functionalized CdTe-CdS core-shell quantum dots (QDs) were synthesized in aqueous solution via water-bathing combined hydrothermal method using L-cysteine (L-Cys) as a stabilizer. This method possesses both the advantages of water-bathing and hydrothermal methods for preparing high-quality QDs with markedly reduced synthesis time, and better stability than a lone hydrothermal method. The QDs were characterized by transmission electronic microscopy and powder X-ray diffraction and X-ray photoelectron spectroscopy. The CdTe-CdS QDs with core-shell structure showed both enhanced fluorescence and better photo stability than nude CdTe QDs. After conjugating with antibody rabbit anti-CEACAM8 (CD67), the as-prepared l-Cys capped CdTe-CdS QDs were successfully used as fluorescent probes for the direct immuno-labeling and imaging of HeLa cells. It was indicated that this kind of QD would have application potential in bio-labeling and cell imaging. Copyright © 2009 John Wiley & Sons, Ltd.

Lecithin-based microemulsion of a peptide for oral administration: preparation, characterization, and physical stability of the formulation.

PubMed

Cilek, Ayşe; Celebi, Nevin; Tirnaksiz, Figen

2006-01-01

The objective of our study was to prepare and characterize a stable microemulsion formulation for oral administration of a peptide, e.g., rh-insulin. The microemulsions were prepared using Labrafil M 1944 CS, Phospholipon 90G (lecithin), absolute alcohol, and bidistilled water. Commercially available soybean lecithins (namely, Phospholipon 80, phosphatidylcholine purity 76 +/- 3%, and Phospholipon 90G, phosphatidylcholine purity 93 +/- 3%) were used in the study. The results showed that the phase diagram obtained using a low purity lecithin was not similar to that obtained with a high purity lecithin. We observed that the microemulsion area was wider at the phase diagram obtained with the higher purity lecithin. We found that the extent of the microemulsion region depended upon both the purity of the lecithin and the surfactant/co-surfactant (s/co-s) mixing ratios (K(m)). The rheological studies showed that microemulsions followed a Newtonian behavior. Such physical characteristics as viscosity, turbidity, density, conductivity, refractive index, droplet size, physical appearance, and phase separation of the microemulsion were measured at different temperatures (4 degrees C, 25 degrees C, and 40 degrees C) during 6 months. The results indicated that the physical characteristics of the developed microemulsions did not change under different storage temperatures (p > 0.05).

Host-guest inclusion system of ferulic acid with p-Sulfonatocalix[n]arenes: Preparation, characterization and antioxidant activity

NASA Astrophysics Data System (ADS)

Chao, Jianbin; Wang, Huijuan; Song, Kailun; Wang, Yongzhao; Zuo, Ying; Zhang, Liwei; Zhang, Bingtai

2017-02-01

The inclusion complexes of ferulic acid (FA) with p-Sulfonatocalix[n]arenes (SCXn, n = 4, 6, 8) were prepared and characterized both in the solid state and in solution using fluorescence spectroscopy, 1H nuclear magnetic resonance (1H NMR), attenuated total reflectance-fourier transform infrared spectroscopy (ATR-FTIR), atomic force microscopy (AFM) and differential scanning calorimetry (DSC). The results show that FA is able to form inclusion complexes with SCXn in a molar ratio of 1:1, causing a significant decrease in the fluorescence intensity of FA. The association constant of the inclusion complexes was calculated from the fluorescence titration data. 1H NMR spectroscopy analysis demonstrates that the aromatic ring and methoxy group of FA are partially covered by SCXn.

Preparation and characterization of hydrophobic P(TFE) blend electrospun gel polymer electrolyte fibrous membranes for Li-O2 battery

NASA Astrophysics Data System (ADS)

Padmaraj, O.; Suthanthiraraj, S. Austin

2018-04-01

A novel stable electrospun gel polymer electrolyte [(100-x)% P(VdF-co-HFP)+(x)% P(TFE), (x = 5, 10, 15, 20, 25 & 30)/1 M Li(CF3SO2)2N-] fibrous membranes with an addition of various concentrations of hydrophobic P(TFE) polymer were prepared by an electrospinning technique. All the prepared electrospun polymer blend fibrous membranes were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, differential scanning calorimetry, high resolution scanning electron microscopy techniques and water contact angle measurements. The newly developed electrospun pure and hydrophobic P(TFE) blend fibrous membranes were activated into separator-cum gel polymer electrolyte fibrous membranes by soaking in an electrolyte solution contains 1 M Li(CF3SO2)2N- in EC: PC (1:1, v/v) in an argon filled glove box. Among the various concentrations of hydrophobic P(TFE) blend polymer fibrous membranes, the electrospun gel polymer blend electrolyte with 5% P(TFE) showed low crystallinity, high thermal stability, high electrolyte uptake, good hydrophobicity and high ionic conductivity (2.680×10-2 S cm-1) at room temperature.

Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

PubMed

Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

2008-01-01

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

Biodegradable nanoparticles for improved kidney bioavailability of rhein: preparation, characterization, plasma, and kidney pharmacokinetics.

PubMed

Wei, Yinghui; Luo, Xiaoting; Guan, Jiani; Ma, Jianping; Zhong, Yicong; Luo, Jingwen; Li, Fanzhu

2017-11-01

The aim of this work is to develop biodegradable nanoparticles for improved kidney bioavailability of rhein (RH). RH-loaded nanoparticles were prepared using an emulsification solvent evaporation method and fully characterized by several techniques. Kidney pharmacokinetics was assessed by implanting a microdialysis probe in rat's kidney cortex. Blood samples were simultaneously collected (via femoral artery) for assessing plasma pharmacokinetics. Optimized nanoparticles were small, with a mean particle size of 132.6 ± 5.95 nm, and homogeneously dispersed. The charge on the particles was nearly zero, the encapsulation efficiency was 62.71 ± 3.02%, and the drug loading was 1.56 ± 0.15%. In vitro release of RH from the nanoparticles showed an initial burst release followed by a sustained release. Plasma and kidney pharmacokinetics showed that encapsulation of RH into nanoparticles significantly increased its kidney bioavailability (AUC kidney /AUC plasma  = 0.586 ± 0.072), clearly indicating that nanoparticles are a promising strategy for kidney drug delivery.

Preparation and structural characterization of zwitterionic surfactant intercalated into NiZn-layered hydroxide salts

NASA Astrophysics Data System (ADS)

Liu, Jiexiang; Wang, Jianlong; Zhang, Xiaoguang; Fang, Binbin; Hu, Pan; Zhao, Xuyang

2015-10-01

Three zwitterionic surfactants, dodecyl dimethyl carboxylbetaine (DCB), dodecyl dimethyl sulfobetaine (DSB) and N-dodecyl-β-aminoprpionate (DAP), intercalated into NiZn-layered hydroxide salts (NZL-DCB, NZL-DSB and NZL-DAP) were synthesized by the coprecipitation method. The effect of surfactant content, pH, temperature and time of hydrothermal treatment on preparation was investigated and discussed. The NZL-DCB, NZL-DSB and NZL-DAP were characterized by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), and thermogravimetry analysis and differential thermal analysis (TGA/DTA). The results showed that basal spacings of NZL-DCB, NZL-DSB and NZL-DAP were around 3.45, 3.68 and 3.94 nm, respectively. DCB, DSB and DAP probably form an overlapped bilayer in the gallery. TGA/DTA data indicated that NZL-DCB, NZL-DSB and NZL-DAP displayed three loss weight stages: loss of adsorbed and structural water, dehydroxylation of matrix and decomposition of nitrate ions, decomposition and combustion of surfactants. Furthermore, chemical analysis data, BET surface area and scanning electron microscopic (SEM) were also measured and analyzed.

Risks of musculoskeletal disorders among betel quid preparers in Taiwan.

PubMed

Chang, Jer-Hao; Wu, Jyun-De; Chen, Chih-Yong; Sumd, Shih-Bin; Yin, Hsin-I; Hsu, Der-Jen

2014-04-01

Betel quid chewing is common in Taiwan. The work of betel quid preparers is characterized by long hours of static work, awkward working posture and highly repetitive hand/wrist motion. However, the musculoskeletal health of betel quid preparers receives very little attention. The Chinese version of the Standardized Nordic Musculoskeletal Questionnaire (NMQ) was administered, and electrogoniometers and electromyography were used in this cross-sectional study to characterize the hand/wrist motion of the subjects. Physical examinations on the thumbs and wrists of the subjects were conducted by means of Phalen's test and Finkelstein's test, respectively. Among the 225 participants, more than 95% attributed their musculoskeletal complaints to their work, and shoulder, neck, hand/wrist, and lower back discomfort were most frequently reported. More than 70% of the preparers did not seek medical treatment for their musculoskeletal problems. Based on the physical examination, 24% of the participants had suspected symptom of either carpal tunnel syndrome (CTS) or DeQuervain's tenosynovitis. The instrumental measurements indicated that betel quid preparation is characterized by extreme angle ranges and moderate repetition of wrist motion as well as low forceful exertion. This study concludes that betel quid preparers are a high risk group of developing musculoskeletal disorders (MSDs). Future studies by electrogoniometers and detailed physical examination on betel quid preparers are needed to determine the predisposing factors for CTS. Some intervention measures to prevent MSDs and to lessen psychological stress for this group of workers are strongly suggested. © 2014 Wiley Periodicals, Inc.

Preparation, characterization and photocatalytic behavior of WO3-fullerene/TiO2 catalysts under visible light

PubMed Central

2011-01-01

WO3-treated fullerene/TiO2 composites (WO3-fullerene/TiO2) were prepared using a sol-gel method. The composite obtained was characterized by BET surface area measurements, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, transmission electron microscopy, and UV-vis analysis. A methyl orange (MO) solution under visible light irradiation was used to determine the photocatalytic activity. Excellent photocatalytic degradation of a MO solution was observed using the WO3-fullerene, fullerene-TiO2, and WO3-fullerene/TiO2 composites under visible light. An increase in photocatalytic activity was observed, and WO3-fullerene/TiO2 has the best photocatalytic activity; it may attribute to the increase of the photo-absorption effect by the fullerene and the cooperative effect of the WO3. PMID:21774800

Adaptive kernel independent component analysis and UV spectrometry applied to characterize the procedure for processing prepared rhubarb roots.

PubMed

Wang, Guoqing; Hou, Zhenyu; Peng, Yang; Wang, Yanjun; Sun, Xiaoli; Sun, Yu-an

2011-11-07

By determination of the number of absorptive chemical components (ACCs) in mixtures using median absolute deviation (MAD) analysis and extraction of spectral profiles of ACCs using kernel independent component analysis (KICA), an adaptive KICA (AKICA) algorithm was proposed. The proposed AKICA algorithm was used to characterize the procedure for processing prepared rhubarb roots by resolution of the measured mixed raw UV spectra of the rhubarb samples that were collected at different steaming intervals. The results show that the spectral features of ACCs in the mixtures can be directly estimated without chemical and physical pre-separation and other prior information. The estimated three independent components (ICs) represent different chemical components in the mixtures, which are mainly polysaccharides (IC1), tannin (IC2), and anthraquinone glycosides (IC3). The variations of the relative concentrations of the ICs can account for the chemical and physical changes during the processing procedure: IC1 increases significantly before the first 5 h, and is nearly invariant after 6 h; IC2 has no significant changes or is slightly decreased during the processing procedure; IC3 decreases significantly before the first 5 h and decreases slightly after 6 h. The changes of IC1 can explain why the colour became black and darkened during the processing procedure, and the changes of IC3 can explain why the processing procedure can reduce the bitter and dry taste of the rhubarb roots. The endpoint of the processing procedure can be determined as 5-6 h, when the increasing or decreasing trends of the estimated ICs are insignificant. The AKICA-UV method provides an alternative approach for the characterization of the processing procedure of rhubarb roots preparation, and provides a novel way for determination of the endpoint of the traditional Chinese medicine (TCM) processing procedure by inspection of the change trends of the ICs.

Preparation, characterization, and biodistribution of letrozole loaded PLGA nanoparticles in Ehrlich Ascites tumor bearing mice.

PubMed

Mondal, Nita; Halder, Kamal Krishna; Kamila, Madan Mohan; Debnath, Mita Chatterjee; Pal, Tapan K; Ghosal, Saroj K; Sarkar, Bharat R; Ganguly, Shantanu

2010-09-15

Letrozole (LTZ) incorporated PLGA nanoparticles were prepared by solvent displacement technique and characterized by transmission electron microscopy, poly-dispersity index and zeta potential measurement. Radiolabeling of free LTZ and LTZ-loaded PLGA NPs was performed with technetium-99m with high labeling efficiency. The labeled complex showed good in vitro stability as verified by DTPA challenge test. The labeled complexes also showed significant in vivo stability when incubated in rat serum for 24 h. Biodistribution studies of (99m)Tc-labeled complexes were performed after intravenous administration in normal mice and Ehrlich Ascites tumor bearing mice. Compared to free LTZ, LTZ-loaded PLGA NPs exhibited significantly lower uptake by the organs of RES. The tumor concentration of LTZ-loaded PLGA NPs was 4.65 times higher than that of free LTZ at 4 h post-injection. This study indicates the capability of PLGA nanopartcles in enhancing the tumor uptake of letrozole. Copyright 2010 Elsevier B.V. All rights reserved.

Preparation and characterization of silver nanoparticles homogenous thin films

NASA Astrophysics Data System (ADS)

Hegazy, Maroof A.; Borham, E.

2018-06-01

The wet chemical method by metal salt reduction has been widely used to synthesize nanoparticles. Accordingly the silver nitrate used as silver precursor and sodium borohydrate as reduction agent. The silver nanoparticles were characterized by different characterization techniques including UV-VIS spectrometry, Transmission electron microscope (TEM), and Zeta potential technique. Thin films of the colloidal solution were fabricated using direct precipitation technique on ITO glass, silicon substrate and commercial glass substrate and characterized by imaging technique. The absorption peak of the silver nanoparticles colloidal solution was around 400 nm. The TEM images indicate that the silver nanoparticles had spherical shape and their sizes were from 10 to 17 nm. The particle size of the silver nanoparticles was confirmed by Zeta potential technique. The imaging technique indicated that the homogeneous distribution of the colloidal silver solution thin film on the silicon substrate was stronger than the ITO glass and inhomogeneous film was emerged on the commercial glass.

[Preparation and characterization of polyhydroxyalkanoate bioplastics with antibacterial activity].

PubMed

Lou, Qiuli; Ma, Yiming; Che, Xuemei; Zhong, Jin; Sun, Xiaoxia; Zhang, Haoqian

2016-08-25

Polyhydroxyalkanoates (PHAs), as a novel class of biopolymer, are attracting more attention due to their diverse material properties and environment-independent biodegradability. Here we report the preparation of PHA exhibiting efficient antibacterial activity by embedding Nisin, a food additive generally recognized as safe, into poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) (PHBHHx), a type of PHA with high biocompatibility. We first prepared Nisin-containing PHBHHx films using solvent casting method. Confocal laser scanning microscopy analysis showed that a well-mixed integrated structure of the films with an even distribution of the Nisin particles in the PHBHHx matrices. Then the antimicrobial activity of PHBHHx/Nisin films against Micrococcus luteus was quantified on agar plate by measuring the size of inhibition zone. Cultivation in liquid media further confirmed the releasing of Nisin from the films and the long-time antibacterial activity. Results showed that the threshold of Nisin concentration for long-time and effective inhibition against bacteria growth is 25 μg/g. These results altogether establish a technological foundation for the application of PHA in biomedicine and food industry.

Preparation and characterization of magnesium borate for special glass

NASA Astrophysics Data System (ADS)

Dou, Lishuang; Zhong, Jianchu; Wang, Hongzhi

2010-05-01

Magnesium borate with a variety of B2O3/MgO molar ratios, which can be applied for special glass, has been prepared through the reaction of light-burned magnesia with boric acid by a hydrothermal method. The effects of the B2O3/MgO molar ratio of raw materials, reaction time, temperature and liquid to solid ratio (ml g-1) on the synthetic product are investigated. The XRD and TG-DTG analyses indicate that the prepared magnesium borate is a mixture of magnesium hexaborate hydrate and ascharite. The results show that high B2O3/MgO molar ratios of raw materials and low reaction liquid-solid ratios favour the product with a high B2O3/MgO molar ratio and vice versa. There exists free MgO in the product when the reaction temperature is below 140 °C or the reaction time is not enough, because of the incomplete reaction of magnesium oxide with boric acid. The process of fractional crystallization for the magnesium borate mixture is also discussed.

Alkylidenediquinocyclopropanes and Diarylcyclopropenes and method for preparation

DOEpatents

West, Robert C.; Beyer, Douglas E.; Komatsu, Koichi

1979-01-01

Alkylidenediquinocyclopropanes and diarylcyclopropenes and the preparation of the former by oxidation of the latter and which are characterized by low energy electronic absorption, pronounced dichroism and characteristic specular reflectance.

Preparation, characterization and application in deep catalytic ODS of the mesoporous silica pillared clay incorporated with phosphotungstic acid.

PubMed

Li, Baoshan; Liu, Zhenxing; Liu, Jianjun; Zhou, Zhiyuan; Gao, Xiaohui; Pang, Xinmei; Sheng, Huiting

2011-10-15

Mesoporous silica pillared clay (SPC) materials with different contents of H(3)PW(12)O(40) (HPW) heteropoly acid were synthesized by introducing HPW into clay interlayer template in an acidic suspension using sol-gel method. Samples with similar HPW loadings were also prepared by impregnation method using SPC as the support. The results of the characterizations showed that HPW was dispersed more homogeneously in the encapsulated samples than in the impregnated samples. The encapsulated materials exhibited better catalytic performance than the impregnated samples in oxidative desulfurization of dibenzothiophene-containing model oil. The sulfur removal reached up to 98.6% for the model oil under the experiential conditions. Copyright © 2011 Elsevier Inc. All rights reserved.

Final Report for X-ray Diffraction Sample Preparation Method Development

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

Ely, T. M.; Meznarich, H. K.; Valero, T.

WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

Preparation, characterization and in vitro evaluation of microemulsion of raloxifene hydrochloride.

PubMed

Golmohammadzadeh, Shiva; Farhadian, Nafiseh; Biriaee, Amir; Dehghani, Faranak; Khameneh, Bahman

2017-10-01

Raloxifene hydrochloride (RLX) is a selective estrogen receptor modulator which is orally used for treatment of osteoporosis and prevention of breast cancer. The drug has low aqueous solubility and bioavailability. The aim of the present study is to formulate and characterize oil-in-water microemulsion systems for oral delivery of RLX. To enhance the drug aqueous solubility, microemulsion based on sesame oil was prepared. Sesame oil and Tween 80 were selected as the drug solvent oil and surfactant, respectively. In the first and second formulations, Edible glycerin and Span 80 were applied as co-surfactant, respectively. Pseudo-ternary phase diagrams showed that the best surfactant/co-surfactant ratios in the first and second formulations were 4:1 and 9:1, respectively. The particle size of all free drug-loaded and drug loaded samples were in the range of 31.25 ± 0.3 nm and 60.9 ± 0.1 nm, respectively. Electrical conductivity coefficient and refractive index of all microemulsion samples confirmed the formation of oil-in-water type of microemulsion. In vitro drug release profile showed that after 24 hours, 46% and 63% of the drug released through the first formulation in 0.1% (w/v) Tween 80 in distilled water as a release medium and phosphate buffer solution (PBS) at pH = 5.5, respectively. These values were changed to 57% and 98% for the second formulation. Results confirmed that the proposed microemulsion system containing RLX could improve and control the drug release profile in comparison to conventional dosage form.

Preparation and characterization of APTES modified magnetic MMT capable of using as anisotropic nanoparticles

NASA Astrophysics Data System (ADS)

Li, Yingjun; Chen, Hua; Wu, Jie; He, Qin; Li, Yintao; Yang, Wenbin; Zhou, Yuanlin

2018-07-01

Montmorillonite (MMT) based anisotropic magnetic nanoparticles (Fe3O4/APTES/MMT) with high anisotropy and reliable magnetism were prepared by using Fe3O4 as magnetic nanoparticles and γ-aminopropyltriethoxysilane (ATPES) as modifier. The characterization indicated that the interactions between Fe3O4 nanoparticles and MMT in Fe3O4/APTES/MMT were stronger than that of directly deposited on to MMT (Fe3O4-MMT) because APTES was chemically bonded to both Fe3O4 and MMT. Fe3O4/APTES/MMT had a greater Ms value (25.16 emu/g) than Fe3O4-MMT (23.71 emu/g). Also, ultrasonication was used to test the interactions between Fe3O4 and MMT. With 30 min of ultrasonication, the amount of Fe3O4 nanoparticles on the surface of Fe3O4/APTES/MMT was more than that of Fe3O4-MMT, and Fe3O4/APTES/MMT had a faster magnetic response to a magnetic field than that of Fe3O4-MMT because of enhanced interactions between Fe3O4 and MMT in Fe3O4/APTES/MMT. In addition, Fe3O4 nanoparticles were densely immobilized onto Fe3O4/APTES/MMT with a smaller average diameter, and the distribution of Fe3O4 nanoparticles on the surface of MMT was more uniform than that of Fe3O4-MMT. Fe3O4/APTES/MMT possessed stable and high magnetism, in ease of orientation and recycling in the magnetic field, and this makes it a promising candidate as anisotropic nanoparticles for use in preparing anisotropic inorganic/polymer composites and anisotropic adsorbents used in wastewater treatment. Finally, the mechanism of ATPES-modified magnetic MMT was investigated.

Materials Characterization Laboratory | Energy Systems Integration Facility

Science.gov Websites

| NREL Materials Characterization Laboratory Materials Characterization Laboratory The Energy Systems Integration Facility's Materials Characterization Laboratory supports the physical and photo -electrochemical characterization of novel materials. Photo of an NREL researcher preparing samples for a gas

Preparation and characterization of 6-layered functionally graded nickel-alumina (Ni-Al2O3) composites

NASA Astrophysics Data System (ADS)

Latiff, M. I. A.; Nuruzzaman, D. M.; Basri, S.; Ismail, N. M.; Jamaludin, S. N. S.; Kamaruzaman, F. F.

2018-04-01

The present research study deals with the preparation of 6-layered functionally graded (FG) metal-ceramic composite materials through powder metallurgy technique. Using a cylindrical die-punch set made of steel, the nickel-alumina (Ni-Al2O3) graded composite structure was fabricated. The samples consist of four gradual inter layers of varied nickel composition (80wt.%, 60wt.%, 40wt.%, 20wt.%) sandwiched with pure Ni and Al2O3 powders at the ends (100wt.% and 0wt.% nickel) were fabricated under 30 ton compaction load using a hydraulic press. After that, two-step sintering was carried out at sintering temperature 1200ºC and soaking time 3 hours was maintained in a tube furnace. The properties of the prepared samples were characterized by radial shrinkage, optical microscopy and hardness testing. Results showed that larger shrinkage occurred within the ceramic phase which proves that more porosities were eliminated in the ceramic rich layers. From the microstructural analysis, it was observed that alumina particles are almost uniformly distributed in nickel matrix, so as nickel particles in the ceramic matrix of alumina-dominant layers. From interfacial analyses, it was observed that a smooth transition in microstructure from one layer to the next confirms a good interfacial solid state bonding between metal-ceramic constituents and good compaction process. On the other hand, microhardness test results suggest that there might be increasing percentage of porosities in the graded structure as the ceramic content rises.

Preparation, characterization and adsorption study of o-cresol molecularly imprinted grafted silica gel sorbent synthesized by sol-gel polymerization

NASA Astrophysics Data System (ADS)

Zinalibdin, Mohamad Raizul; Jaafar, Jafariah; Majid, Zaiton Abdul; Sanagi, Mohd Marsin

2017-11-01

In this study, a new composite core-shell of o-cresol molecularly imprinted polymer grafted silica gel (MIP@SiO2) was prepared via sol-gel polymerization. It was synthesized using o-cresol as the template molecule, 3-propyl(metacrylate)trimethoxysilane (3-PMTMOS) as the functional monomer, tetraethoxysilane (TEOS) as the cross-linker and ethanol as the porogenic solvent in the surface of silica gel. The non-imprinted polymer-grafted silica gel (NIP@SiO2) was prepared with the same technique but without template molecule. This analyte was selected as a template due to the fact that it is one of toluene metabolites. The characterization of MIP@SiO2 and NIP@SiO2 were observed by N2 adsorption analysis and Field emission scanning electron microscopy-energy dispersive x-ray (FESEM-EDX). The MIP@SiO2 and NIP@SiO2 were employed as an adsorbent for the extraction of o-cresol, a metabolite in urine sample for the monitoring of occupational toluene exposure in workers. Based on the results of the adsorption study, the MIP prepared using 0.5 mmol 3-(propylmethacrylate)trimethoxysilane), 10 mL of ethanol, 4 mmol TEOS,0.05 mmol o-cresol, 0.1g silica gel and 1mL of 0.01 mol/L acetic acid was found the adsorption capacity (0.9920 mg g-1) and imprint factor (5.21).

Different preparation methods and characterization of magnetic maghemite coated with chitosan

NASA Astrophysics Data System (ADS)

Hojnik Podrepšek, Gordana; Knez, Željko; Leitgeb, Maja

2013-06-01

The preparation of maghemite (γ-Fe2O3) micro- and nanoparticles coated with chitosan, used as carriers for immobilized enzymes, was investigated. γ-Fe2O3 nanoparticles were synthesized by coprecipitation of Fe2+ and Fe3+ ions in the presence of ammonium. They were coated with chitosan by the microemulsion process, suspension cross-linking technique, and covalent binding of chitosan on the γ-Fe2O3 surface. The methods distinguished the concentration of chitosan, concentration of acetic acid solution, concentration of a cross-linking agent, temperature of synthesis, pH of the medium, and time of synthesis. γ-Fe2O3 micro- and nanoparticles coated with chitosan prepared after three preparation methods were evaluated by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy analysis, energy dispersive spectrometry, thermogravimetric analysis, differential scanning calorimetry analysis, vibrating sample magnetometry, dynamic light scattering, laser diffraction granulometry, and X-ray diffractometry. These positive attributes demonstrated that these magnetic micro- and nanoparticles coated with chitosan may be used as a promising carrier for further diverse biomedical applications.

Physical-chemical and biological characterization of different preparations of equine chorionic gonadotropin

PubMed Central

Natal, Fabio Luis Nogueira; Ribela, Maria Teresa Carvalho Pinto; de Almeida, Beatriz Elane; de Oliveira, João Ezequiel; Bartolini, Paolo

2016-01-01

Ovarian stimulation with commercial preparations of equine chorionic gonadotropin (eCG) produces extremely variable responses in domestic animals, ranging from excessive stimulation to practically no stimulation, when applied on the basis of their declared unitage. This study was conducted to analyze four commercial preparations from different manufacturers via reversed-phase HPLC (RP-HPLC) in comparison with a reference preparation and an official International Standard from the World Health Organization. The peaks obtained by this qualitative and quantitative physical–chemical analysis were compared using an in vivo bioassay based on the ovarian weight gain of prepubertal female rats. The RP-HPLC data showed one or two peaks close to a main peak (tR = 27.9 min), which were related to the in vivo bioactivity. Commercial preparations that have this altered peak showed very little or no in vivo activity, as demonstrated by rat ovarian weight and in peripubertal gilts induced to ovulate. Overall, these findings indicate that RP-HPLC can be a rapid and reliable tool to reveal changes in the physicochemical profile of commercial eCG that is apparently related to decreased biological activity of this hormone. PMID:27297410

Preparation and Characterization of C60/Graphene Hybrid Nanostructures.

PubMed

Chen, Chuanhui; Mills, Adam; Zheng, Husong; Li, Yanlong; Tao, Chenggang

2018-05-15

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We present methods for depositing and passively manipulating C60 molecules on rippled graphene that advance the pursuit of realizing applications involving 1D C60/graphene hybrid structures. The techniques applied in this exposition are geared towards high vacuum systems with preparation areas capable of supporting molecular deposition as well as thermal annealing of the samples. We focus on C60 deposition at low pressure using a homemade Knudsen cell connected to a scanning tunneling microscopy (STM) system. The number of molecules deposited is regulated by controlling the temperature of the Knudsen cell and the deposition time. One-dimensional (1D) C60 chain structures with widths of two to three molecules can be prepared via tuning of the experimental conditions. The surface mobility of the C60 molecules increases with annealing temperature allowing them to move within the periodic potential of the rippled graphene. Using this mechanism, it is possible to control the transition of 1D C60 chain structures to a hexagonal close packed quasi-1D stripe structure.

High photoactive and visible-light responsive graphene/titanate nanotubes photocatalysts: preparation and characterization.

PubMed

Qianqian, Zhai; Tang, Bo; Guoxin, Hu

2011-12-30

A series of graphene/titanate nanotubes (TNTs) photocatalysts using graphene and nanoscale TiO(2) or P25 as original materials were fabricated by hydrothermal method. Both low hydrothermal temperature and proper amount of graphene are propitious to better photoactivity. The photocatalytic activities of these nanocomposites far exceed that of P25, pure TNTs and reported TiO(2)-based nanocomposites for the degradation of Rhodamine-B under visible-light irradiation. These prepared photocatalysts were characterized by TEM, XRD, XPS, BET, FTIR and UV-vis diffuse reflection spectra, and the results indicate that the outstanding photoactivities in visible-light region result from sensitization effect of graphene rather than impurity level in the band gap of TNTs. Furthermore, large BET surface areas of these photocatalysts (almost 10 times larger than that of previously reported graphene/TiO(2) nanoparticles) evidently enhance their absorption abilities and photocatalytic performances (the rate constants of degrading Rhodamine-B are at least 5 times higher than that of previously reported photocatalysts). These photocatalysts show good stability, and their photoactivities do not obviously decrease after four times of repeated uses. A detailed photocatalytic mechanism is suggested, as well. Copyright © 2011 Elsevier B.V. All rights reserved.

Preparation and characterization of phase transition/graphite foam composite materials.

PubMed

Yu, Jia; Tang, ChenLong; Yu, ZhiChao

2016-07-04

Phase transition/graphite foam (PCM/GF) composite materials are a kind of composite materials that fill graphite foam with phase change materials. In this paper, graphite foam was prepared firstly by the soft template method, the heat conductivity of which at room temperature is 5.44 W/(m∙K). Then, four phase change materials including eicosane, acetamide, xylitol, and erythritol were chosen for filling into the prepared graphite foam to obtain PCM/GF composite materials. Among the four kinds of materials, erythritol composite material has the highest melting point (118.5°C) and the highest enthalpy of fusion (266.3J/g), weight loss ratios of xylitol composite material after ten cycles is the lowest (2.1%), the compressive strength of xylitol composite material is the highest (9.08 MPa) and that of eicosane composite material is the lowest (3.32 MPa).

Visible-light induced anti-bacterial and self-cleaning waterborne polyacrylic coating modified with TiO2/polypyrrole nanocomposite; preparation and characterization

NASA Astrophysics Data System (ADS)

Nosrati, Rahimeh; Olad, Ali; Maryami, Fatemeh

2018-07-01

Nowadays, self-cleaning technology is used in various industries to decreasing the time, energy consumption and costs of surface servicing as well as the increasing of surface durability. Self-cleaning and anti-bacterial coatings can be made by the addition of suitable additives to a polymer matrix with good properties. In the present research, TiO2/polypyrrole nanocomposites were prepared in different TiO2 to polypyrrole weight ratios and used in various percent as an additive in waterborne commercial grade polyacrylic latex. Characterization and evaluation of structural and morphological features of nanocomposites and coatings were performed by FTIR, XRD, UV-Vis and FESEM techniques. By the addition of prepared nanocomposites as an additive to the polyacrylic matrix, the hydrophilic, water resistant, anti-bacterial, and photocatalytic coatings were prepared. The TiO2 to polypyrrole weight ratio of TiO2/polypyrrole nanocomposites and the percent of nanocomposite additive in the polymeric matrix were optimized. According to the results, the coating containing 2% and 3% of TiO2/polypyrrole nanocomposite with TiO2 to polypyrrole weight ratio of 100:10 are proposed as the best coating formulations in the formulations examined in this work, due to their good properties in the most of experiments.

Preparation, characterization and biological test of 3D-scaffolds based on chitosan, fibroin and hydroxyapatite for bone tissue engineering.

PubMed

Lima, Paulo Autran Leite; Resende, Cristiane Xavier; Soares, Glória Dulce de Almeida; Anselme, Karine; Almeida, Luís Eduardo

2013-08-01

This work describes the preparation and characterization of porous 3D-scaffolds based on chitosan (CHI), chitosan/silk fibroin (CHI/SF) and chitosan/silk fibroin/hydroxyapatite (CHI/SF/HA) by freeze drying. The biomaterials were characterized by X-ray diffraction, attenuated total reflection Fourier transform infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry, scanning electron microscopy and energy dispersive spectroscopy. In addition, studies of porosity, pore size, contact angle and biological response of SaOs-2osteoblastic cells were performed. The CHI scaffolds have a porosity of 94.2±0.9%, which is statistically higher than the one presented by CHI/SF/HA scaffolds, 89.7±2.6%. Although all scaffolds were able to promote adhesion, growth and maintenance of osteogenic differentiation of SaOs-2 cells, the new 3D-scaffold based on CHI/SF/HA showed a significantly higher cell growth at 7 days and 21 days and the level of alkaline phosphatase at 14 and 21 days was statistically superior compared to other tested materials. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation and characterization of calcium phosphate ceramics and composites as bone substitutes

NASA Astrophysics Data System (ADS)

Zhang, Xing

Marine CaCO3 skeletons have tailored architectures created by nature, which give them structural support and other functions. For example, seashells have dense lamellar structures, while coral, cuttlebone and sea urchin spines have interconnected porous structures. In our experiments, seashells, coral and cuttlebone were hydrothermally converted to hydroxyapatite (HAP), and sea urchin spines were converted to Mg-substituted tricalcium phosphate (beta-TCMP), while maintaining their original structures. Partially converted shell samples have mechanical strength, which is close to that of compact human bone. After implantation of converted shell and spine samples in rat femoral defects for 6 weeks, there was newly formed bone growth up to and around the implants. Some new bone was found to migrate through the pores of converted spine samples and grow inward. These results show good bioactivity and osteoconductivity of the implants, indicating the converted shell and spine samples can be used as bone defect fillers. Calcium phosphate powders were prepared through different synthesis methods. Micro-size HAP rods were synthesized by hydrothermal method through a nucleation-growth mechanism. On the other hand, HAP particles, which have good crystallinity, were prepared by wet precipitation with further hydrothermal treatment. beta-TCP or beta-TCMP powders were prepared by a two-step process: wet precipitation of apatitic tricalcium phosphate ('precursor') and calcination of the precursor at 800°C for 3 hours. beta-TCMP or beta-TCP powders were also prepared by solid-state reactions from CaHPO4 and CaCO 3 with/without MgO. Biphasic calcium phosphate, which is mixture of HAP and beta-TCP, can be prepared though mechanical mixing of HAP and beta-TCP powders synthesized as above. Dense beta-TCP and beta-TCMP ceramics can be produced by pressing green bodies at 100MPa and further sintering above 1100°C for 2 hours. beta-TCMP ceramics ˜99.4% relative dense were prepared by

Preparation and characterization of azithromycin--Aerosil 200 solid dispersions with enhanced physical stability.

PubMed

Li, Xuechao; Peng, Huanhuan; Tian, Bin; Gou, Jingxin; Yao, Qing; Tao, Xiaoguang; He, Haibing; Zhang, Yu; Tang, Xing; Cai, Cuifang

2015-01-01

The main purpose of this study was to investigate the feasibility of azithromycin (AZI)--Aerosil 200 solid dispersions specifically with high stability under accelerated condition (40 °C/75% RH). Ball milling (BM) and hot-melt extrusion (HME) were used to prepare AZI solid dispersions. The physical properties of solid dispersions were evaluated by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric analysis (TGA). For solid dispersions prepared with both methods, no crystalline of AZI was detected (except for AZI: Aerosil 200=75:25) by DSC or PXRD, indicating the amorphous state of AZI in solid dispersions. The FT-IR results demonstrated the loss of crystallization water and the formation of hydrogen bonds between Aerosil 200 and AZI during the preparation of solid dispersions. After 4 weeks storage under accelerated condition, the degree of crystallinity of AZI increased in solid dispersions prepared by BM, whereas for solid dispersions containing AZI, Aerosil 200 and glyceryl behenate (GB) prepared by HME, no crystalline of AZI was identified. This high stability can be attributed to the hydrophobic properties of GB and the presence of hydrogen bonds. Based on the above results, it is inferred the protection of hydrogen bonds between AZI and Aerosil 200 formed during preparation process effectively inhibited the recrystallization of AZI and improved the physical stability of amorphous AZI in the presence of Aerosil 200. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and characterization of teniposide PLGA nanoparticles and their uptake in human glioblastoma U87MG cells.

PubMed

Mo, Liqian; Hou, Lianbing; Guo, Dan; Xiao, Xiaoyan; Mao, Ping; Yang, Xixiao

2012-10-15

Many studies have demonstrated the uptake mechanisms of various nanoparticle delivery systems with different physicochemical properties in different cells. In this study, we report for the first time the preparation and characterization of teniposide (VM-26) poly(D,L-lactide-co-glycolide) (PLGA) nanoparticles (NPs) and their cellular uptake pathways in human glioblastoma U87MG cells. The nanoparticles prepared with oil-in-water (O/W) single-emulsion solvent evaporation method had a small particle size and spherical shape and provided effective protection against degradation of teniposide in PBS solution. Differential scanning calorimeter (DSC) thermograms concluded that VM-26 was dispersed as amorphous or disordered crystalline phase in the PLGA matrix. A cytotoxicity study revealed that, in a 24h period, blank PLGA NPs had no cytotoxicity, whereas teniposide-loaded PLGA NPs (VM-26-NPs) had U87MG cytotoxicity levels similar to free teniposide. Confocal laser scanning microscopy (CLSM) and transmission electron microscopy (TEM) images showed the distribution and degradation processes of nanoparticles in cells. An endocytosis inhibition test indicated that clathrin-mediated endocytosis and macropinocytosis were the primary modes of engulfment involved in the internalization of VM-26-NPs. Our findings suggest that PLGA nanoparticles containing a sustained release formula of teniposide may multiplex the therapeutic effect and ultimately degrade in lysosomal within human glioblastoma U87MG cells. Copyright © 2012 Elsevier B.V. All rights reserved.

Dramatic improvement of the solubility of pseudolaric acid B by cyclodextrin complexation: preparation, characterization and validation.

PubMed

Chi, Liandi; Liu, Ruihao; Guo, Tao; Wang, Manli; Liao, Zuhua; Wu, Li; Li, Haiyan; Wu, Deling; Zhang, Jiwen

2015-02-20

As one of the most important technologies to improve the solubility of poorly water-soluble drugs, the solubilization effects of cyclodextrins (CDs) complexation are, on occasions, not as large as expected, which tends to detract from the wider application of CDs. In this study, a dramatic improvement of the solubility of pseudolaric acid B (PAB) by CDs has been found with a 600 fold increase by HP-β-CD complexation. In addition, the solubility enhancement of PAB by various CDs, including α-CD, β-CD, γ-CD, HP-β-CD and SBE-β-CD was investigated by phase solubility studies. The inclusion complex of PAB/HP-β-CD was prepared by different methods and characterized by differential scanning calorimetry (DSC), powder X-ray diffractometry (XRD), nuclear magnetic resonance spectroscopy ((1)H NMR) together with molecular simulation. The results indicated that the solubility of PAB was increased to 15.78mgmL(-1) in the presence of 30% HP-β-CD, which is a 600 fold increase compared with that in pure water. And the chemical stability of PAB in PBS (pH 7.4) can be enhanced. The results of DSC and XRD showed the absence of crystallinity in the PAB/HP-β-CD inclusion complex prepared by the saturated water solution method. The results of (1)H NMR together with molecular simulation indicated the conjugated diene side-chain of PAB was included into the cavity of HP-β-CD, with the free energy of -20.34±4.69kJmol(-1). While the enzymatic degradation site of the carboxyl polar bond is located in the hydrophilic outer of HP-β-CD resulted in no significant difference for the enzymatic degradation rate between PAB and PAB/HP-β-CD complexes in rat plasma. In summary, the PAB/HP-β-CD inclusion complex prepared in this study can greatly improve the solubility and chemical stability of PAB, which will result in the in vivo administration of PAB as a liquid solution. Copyright © 2015 Elsevier B.V. All rights reserved.

Characterization of Laboratory Prepared Concrete Pastes Exposed to High Alkaline and High Sodium Salt Solutions

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

Langton, C. A.

The objective of this study was to identify potential chemical degradation mechanisms for the Saltstone Disposal Unit (SDU) concretes, which over the performance life of the structures may be exposed to highly alkaline sodium salt solutions containing sulfate, hydroxide, and other potentially corrosive chemicals in salt solution and saltstone flush water, drain water, leachate and / or pore solution. The samples analyzed in this study were cement pastes prepared in the SIMCO Technologies, Inc. concrete laboratory. They were based on the paste fractions of the concretes used to construct the Saltstone Disposal Units (SDUs). SDU 1 and 4 concrete pastesmore » were represented by the PV1 test specimens. The paste in the SDU 2, 3, 5, and 6 concrete was represented by the PV2 test specimens. SIMCO Technologies, Inc. selected the chemicals and proportions in the aggressive solutions to approximate proportions in the saltstone pore solution [2, 3, 5, and 6]. These test specimens were cured for 56 days in curing chamber before being immersed in aggressive solutions. After exposure, the samples were frozen to prevent additional chemical transport and reaction. Selected archived (retrieved from the freezer) samples were sent to the Savannah River National Laboratory (SRNL) for additional characterization using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive x-ray (EDX) spectroscopy. Characterization results are summarized in this report. In addition, a correlation between the oxide composition of the pastes and their chemical durability in the alkaline salt solutions is provided.« less

Characterization of thermochromic VO2 (prepared at 250 °C) in a wide temperature range by spectroscopic ellipsometry

NASA Astrophysics Data System (ADS)

Houska, J.; Kolenaty, D.; Rezek, J.; Vlcek, J.

2017-11-01

The paper deals with thermochromic VO2 prepared by reactive high-power impulse magnetron sputtering and characterized by spectroscopic ellipsometry. We focus on the dispersion of optical constants in a wide temperature range and on the transmittance predicted using the optical constants. While the thermochromic behavior of VO2 in itself has been reported previously (particularly above the room temperature, RT), in this paper we present (i) optical properties achieved at a low deposition temperature of 250 °C and without any substrate bias voltage (which dramatically increases the application potential of the coating) and (ii) changes of these properties not only above but also below RT (down to -30 °C). The properties include very low (for VO2) extinction coefficient at RT (0.10 at 550 nm), low transition temperature of around or even below 50 °C (compared to the frequently cited 68 °C) and high modulation of the predicted infrared transmittance (e.g. 39% at -30 °C, 30% at RT and 3.4% above the transition temperature at 2000 nm for a 100 nm thick coating on glass). The results are important for the design of thermochromic coatings, and pathways for their preparation under industry-friendly conditions, for various technological applications.

Preparation of solid lipid nanoparticles as drug carriers for levothyroxine sodium with in vitro drug delivery kinetic characterization.

PubMed

Rostami, E; Kashanian, S; Azandaryani, A H

2014-05-01

The aim of this work was to produce and characterize solid lipid nanoparticles (SLN) containing levothyroxine sodium for oral administration, and to evaluate the kinetic release of these colloidal carriers. SLNs were prepared by microemulsion method. The particle size and zeta potential of levothyroxine sodium-loaded SLNs were determined to be around 153 nm,-43 mV (negatively charged), respectively by photon correlation spectroscopy. The levothyroxine entrapment efficiency was over 98%. Shape and surface morphology were determined by TEM and SEM. They revealed fairly spherical shape of nanoparticles.SLN formulation was stable over a period of 6 months. There were no significant changes in particle size, zeta potential and polydispersity index and entrapment efficiency, indicating that the developed SLNs were fairly stable.

Preparation, characterization and in vitro antioxidative potential of synbiotic fermented dairy products.

PubMed

Shah, C; Mokashe, N; Mishra, V

2016-04-01

The present study, evaluates the antioxidative potential of two synbiotic dairy products viz. synbiotic lassi with honey and whey based synbiotic drink with inulin and orange juice, along with their physicochemical and microbiological activity during storage period. Antioxidative potential of raw ingredients and probiotic cultures used to prepare synbiotic products was also evaluated. Synbiotic lassi with honey was prepared using Streptococcus thermophilus MTCC 5460 (MD2) and Lactobacillus helveticus MTCC 5463 (V3) as probiotics and honey as prebiotic. For preparation of whey based synbiotic drink, Lactobacillus helveticus MTCC 5463 and inulin were used as probiotic and prebiotic, respectively and orange juice was also incorporated. Titratable acidity and pH of both synbiotic products followed a similar pattern of increase or decrease during storage. Furthermore, no major changes were observed in viability of probiotic cultures under storage conditions adapted. The hydroxyl radical scavenging activity of synbiotic lassi with honey was found to significantly decrease from 107.76 to 79.41 % at the end of storage whereas, the activity of whey based synbiotic drink was 100.32 % which declined sharply to 79.21 % on 7th day but further increased to 102.59 % on 14th day. The DPPH (α, α-Diphenyl-β-Picrylhydrazyl) radical scavenging activity of freshly prepared synbiotic lassi with honey was 28.43 % which decreased to 23.03 % on 7th day while for whey based synbiotic drink decreased from 26.85 % (0 day) to 17.12 % (7th day) and continued to decline. Moreover, probiotic strains used for synbiotic preparation also demonstrated good antioxidative activity.

One-step multiple component isolation from the oil of Crinitaria tatarica (Less.) Sojak. by preparative capillary gas with characterization by spectroscopic and spectrometric techniques and evaluation of biological activity

USDA-ARS?s Scientific Manuscript database

In the present work multiple component isolation from the oil of Crinitaria tatarica (Less.) Sojak. by Preparative Capillary Gas Chromatography (PCGC) with characterization by mass spectrometry (MS) and nuclear magnetic resonance (NMR) spectroscopy have been carried out. Gas chromatography (GC-FID) ...

Ultrasonication-assisted preparation and characterization of emulsions and emulsion gels for topical drug delivery.

PubMed

Singh, Vinay K; Behera, Baikuntha; Pramanik, Krishna; Pal, Kunal

2015-03-01

The current study describes the use of ultrasonication for the preparation of biphasic emulsions and emulsion gels for topical drug delivery. Sorbitan monostearate (SMS) was used as the surfactant for stabilizing the interface of sesame oil (apolar phase) and water (polar phase). Emulsions were formed at lower concentrations of SMS, whereas emulsion gels were formed at higher concentrations of SMS. The formulations were characterized by fluorescent microscopy, X-ray diffraction, viscosity, stress relaxation, spreadability, and differential scanning calorimetry studies. Fluorescence microscopy suggested formation of oil-in-water type of formulations. There was an increase in the viscosity, bulk resistance, and firmness of the formulations as the proportions of SMS was increased. The emulsion gels were viscoelastic in nature. Thermal studies suggested higher thermodynamic stability at higher proportions of either SMS or water. Metronidazole, a model antimicrobial drug, was incorporated within the formulations. The release of the drug from the formulations was found to be diffusion mediated. The drug-loaded formulations showed sufficient antimicrobial efficiency to be used as carriers for topical antimicrobial drug delivery. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Preparation and characterization of functional poly(vinylidene fluoride) (PVDF) membranes with ultraviolet-absorbing property

NASA Astrophysics Data System (ADS)

Dong, Li; Liu, Xiangdong; Xiong, Zhengrong; Sheng, Dekun; Lin, Changhong; Zhou, Yan; Yang, Yuming

2018-06-01

We first reported a strategy to prepare functional poly(vinylidene fluoride) (PVDF) membranes with excellent ultraviolet-absorbing property through chemically induced grafting. Herein, the polymerizable ultraviolet (UV) absorber 2-hydroxy-4-(3-methacryloxy-2-hydroxylpropoxy) benzophenone (BPMA) made by ourselves was grafted onto the PVDF chains that have been pretreated with tetraethylammonium hydroxide (TEAH) alkaline solution. Moreover, the effect of experiment conditions such as the alkali and monomer concentrations, alkali treatment time on the UV-absorbing property of the obtained PVDF-g-PBPMA membranes were studied in detail. The chemical structure of the modified membranes was confirmed by 1H NMR, FT-IR and XPS measurements. Meanwhile, the thermal and UV-absorbing properties were characterized by TGA, DSC and UV-Vis spectrophotometer, respectively. The results indicated that BPMA side chains were successfully introduced onto PVDF backbones. Most importantly, the obtained PVDF-g-PBPMA membranes exhibited excellent UV-absorbing property. The transmittance of UV light at 300 nm decreased to as low as 0.02% and the UV light below 388 nm could be completely absorbed by the PVDF-g-PBPMA membrane made under optimal condition.

Preparation and characterization of cross-linked excipient of coprocessed xanthan gum-acacia gum as matrix for sustained release tablets

NASA Astrophysics Data System (ADS)

Surini, Silvia; Wati, Dina Risma; Syahdi, Rezi Riadhi

2018-02-01

Sustained release tablet is solid dosage form which is designed to release drugs slowly in the body. This research was intended to prepare and characterize the cross-linked excipients of co-processed xanthan gum-acacia gum (CL-Co-XGGA) as matrices for sustained release tablets with gliclazide as a model drug. CL-Co-XGGA excipients were cross-linked materials of co-processed excipients of xanthan gum-acacia gum (Co-XGGA) using sodium trimetaphosphate. Co-processed excipients of xanthan gum-acacia gum were prepared in the ratio of each excipient 1:2, 1:1 and 2:1. Co-XGGA and CL-Co-XGGA excipients were characterized physically, chemically and functionally. Then, the sustained release (SR) tablets were formulated by wet granulation method using CL-Co-XGGA excipients as matrices. Also, the dissolution study of the gliclazide SR tablets was carried out in phosphate buffer medium pH 7,4 containing sodium lauryl sulphate 0.2% for 12 hours. The results showed that the degree of substitution (DS) of CL-Co-XGGA 1:2, 1:1, 2:1 excipients were respectively 0.067, 0.082 and 0.08. Besides that, the excipients gel strengths were 14.03, 17.27 and 20,70 gF, respectively. The cross-linked excipients had improved flow properties and swelling capability compared to the Co-XGGA excipients. The results of the gliclazide SR tablets evaluations showed that all tablets were passed all tablet requirements. Moreover, the gliclazide release from SR tablets F1 - F6 revealed the sustained release profile, which was following zero order kinetics (F1, F2, F3, F6) and Higuchi kinetics (F4 and F5). It could be concluded that the obtained CL-Co-XGGA excipients might be used as matrices for sustained release tablets and could retard drug release up to 8 until 32 hours.

Sterically Hindered Square-Planar Nickel(II) Organometallic Complexes: Preparation, Characterization, and Substitution Behavior

ERIC Educational Resources Information Center

Martinez, Manuel; Muller, Guillermo; Rocamora, Merce; Rodriguez, Carlos

2007-01-01

The series of experiments proposed for advanced undergraduate students deal with both standard organometallic preparative methods in dry anaerobic conditions and with a kinetic study of the mechanisms operating in the substitution of square-planar complexes. The preparation of organometallic compounds is carried out by transmetallation or…

Preparation and characterization of thick-film Ni/MH battery.

PubMed

Do, Jing-Shan; Yu, Sen-Hao; Cheng, Suh-Fen

2004-07-30

Using the porous polypropylene (PP) films sputtered with gold and the Ni as current collectors, the electroactive materials (Ni(OH)2 and metal hydride (MH)) of positive and negative electrodes were prepared on the current collector using thick-film technology. Two types of cell configurations were prepared and the characteristics of these batteries were compared. The cycle number for the formation of batteries based on the porous PP film was found to be 2, which was significantly less than that of batteries based on the ceramic substrates. Using the porous PP film as substrate, the number of cycles for the formation of battery increased from 2 to 5 with the increase of the charge/discharge rate from 0.1C/0.025C to 2.0C/0.5C. The silver oxides dendrites formed by the oxidation of silver paste used to adhere the current collectors and the conducting wires in the charge/discharge process caused a short contact between the positive and negative electrodes, which then caused the battery failure. The cycle life of the battery based on the porous PP film was found to be greater than 400 when the charge/discharge rate was 2.0C/0.5C.

Characterization of polycrystalline nickel cobaltite nanostructures prepared by DC plasma magnetron co-sputtering for gas sensing applications

NASA Astrophysics Data System (ADS)

Hammadi, Oday A.; Naji, Noor E.

2018-03-01

In this work, a gas sensor is fabricated from polycrystalline nickel cobaltite nano films deposited on transparent substrates by closed-field unbalanced dual-magnetrons (CFUBDM) co-sputtering technique. Two targets of nickel and cobalt are mounted on the cathode of discharge system and co-sputtered by direct current (DC) argon discharge plasma in presence of oxygen as a reactive gas. The total gas pressure is 0.5 mbar and the mixing ratio of Ar:O2 gases is 5:1. The characterization measurements performed on the prepared films show that their transmittance increases with the incident wavelength, the polycrystalline structure includes 5 crystallographic planes, the average particle size is about 35 nm, the electrical conductivity is linearly increasing with increasing temperature, and the activation energy is about 0.41 eV. These films show high sensitivity to ethanol vapor.

Preparation and characterization of a novel conformed bipolymer paclitaxel-nanoparticle using tea polysaccharides and zein.

PubMed

Li, Shuqin; Wang, Xiuming; Li, Weiwei; Yuan, Guoqi; Pan, Yuxiang; Chen, Haixia

2016-08-01

To improve the aqueous solubility of the anticancer agent paclitaxel (PTX), a newly conformed bipolymer paclitaxel-nanoparticle using tea polysaccharide (TPS) and zein was prepared and characterized. Tea polysaccharide was used as a biopolymer shell and zein was as the core and the optimal formula was subjected to the characteristic study by TEM, DSC, FTIR and in vitro release study. Results showed that the optimal particle was acquired with particle yield at 40.01%, drug loading at 0.12% and diameters around 165nm when the concentration of tea polysaccharide was set at 0.2%, and the amount of PTX:zein=1:10. The particle was a nanoparticle with spherical surface and the encapsulated PTX was in an amorphous form rather than cystalline form. PTX was interacted with zein and polysaccharide through O H and CO groups and it had a sustained release. The results suggested that the novel bipolymer might be a promising agent for PTX delivery and tea polysaccharide was demonstrated its function in drug delivery system. Copyright © 2016 Elsevier Ltd. All rights reserved.

Preparation, characterization and activity evaluation of heterostructure In(2)O(3)/In(OH)(3) photocatalyst.

PubMed

Shifu, Chen; Xiaoling, Yu; Huaye, Zhang; Wei, Liu

2010-08-15

In this paper, the heterostructure In(2)O(3)/In(OH)(3) photocatalyst was prepared by programmed thermal treatment of In(OH)(3) using In(NO(3))(3).9H(2)O as the precursor. Various characterization methods such as X-ray power diffraction (XRD), UV-vis diffuse reflectance spectroscopy (DRS), Fourier transform infrared spectrometry (FT-IR) and transmission electron microscopy (TEM) were employed to investigate the structure, morphologies, and optical properties. Terephthalic acid was used as a probe molecule to detect the generation of hydroxyl radicals (OH) on the surface of UV-illuminated photocatalyst by a photoluminescence (PL) technique. The results showed that the photocatalytic activity of the heterostructure In(2)O(3)/In(OH)(3) was higher than that of single In(2)O(3) or In(OH)(3). The increased photocatalytic activity may be attributed to the formation of the heterojunction between In(2)O(3) and In(OH)(3), which suppresses the recombination of photoexcited electrons-hole pairs. Copyright 2010 Elsevier B.V. All rights reserved.

Preparation and characterization of host-guest system between inosine and β-cyclodextrin through inclusion mode

NASA Astrophysics Data System (ADS)

Prabu, Samikannu; Sivakumar, Krishnamurty; Swaminathan, Meenakshisundaram; Rajamohan, Rajaram

2015-08-01

Inosine is a nucleoside that is formed when hypoxanthine is attached to a ribose ring (also known as a ribofuranose) via a β-N9-glycosidic bond. Inosine is commonly found in tRNAs. Inosine (INS) has been used widely as an antiviral drug. The inclusion complex of INS with β-CDx in solution phase is studied by ground and excited state with UV-visible and fluorescence spectroscopy, respectively. A binding constant and stoichiometric ratio between INS and β-CDx are calculated by BH equation. The lifetime and relative amplitude of INS is increases with increasing the concentrations of β-CDx, confirms the formation of inclusion complex in liquid state. The solid complexes are prepared by kneading method (KM) and co-precipitation method (CP). The solid complex is characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and differential scanning colorimetry (DSC). CP method gives the solid product with good yield than that of physical mixture and KM method. The structure of complex is proposed based on the study of Patch - Dock server.

Preparation and characterization of microparticles of β-cyclodextrin/glutathione and chitosan/glutathione obtained by spray-drying.

PubMed

Webber, Vanessa; de Siqueira Ferreira, Daniel; Barreto, Pedro Luis Manique; Weiss-Angeli, Valeria; Vanderlinde, Regina

2018-03-01

Reduced glutathione (GSH) is an efficient antioxidant on limitation of browning, of the loss of aromas and off-flavor formation in white wines. The encapsulation of GSH in a polymer system to be added in white wines may prolong its antioxidant action. The aim of this work was to prepare and characterize spray-dried microparticles using β-cyclodextrin (β-CD) or chitosan as polymers for encapsulation of GSH for its addition to wine to prevent oxidation. The microparticles obtained after the drying process were characterized regarding morphology, chemical interaction between GSH and polymers, thermal stability, microstructure, encapsulation efficiency and in vitro GSH release. SEM showed spherical microparticles, with wrinkled surfaces for β-CD/GSH and smooth surfaces for chitosan/GSH. A wide distribution of particle size was observed. In general, β-CD/GSH showed an average diameter smaller than the chitosan/GSH microparticles. FT-IR showed a possible interaction between GSH and both polymers. DSC and DRX showed that encapsulation process produced a marked decrease in GSH crystallinity. The encapsulation efficiency was 25.0% for chitosan/GSH and 62.4% for β-CD/GSH microparticles. The GSH release profiles from microparticles showed that β-CD can control the release behaviors of GSH better than chitosan in a model wine. Cumulative release data were fitted to an empirical equation to compute diffusional exponent (n), which indicates a trend the non-Fickian release of GSH. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characterization and Identification of Pediococcus Species Isolated from Forage Crops and Their Application for Silage Preparation

PubMed Central

Cai, Yimin; Kumai, Sumio; Ogawa, Masuhiro; Benno, Yoshimi; Nakase, Takashi

1999-01-01

Pediococcus species isolated from forage crops were characterized, and their application to silage preparation was studied. Most isolates were distributed on forage crops at low frequency. These isolates could be divided into three (A, B, and C) groups by their sugar fermentation patterns. Strains LA 3, LA 35, and LS 5 are representative isolates from groups A, B, and C, respectively. Strains LA 3 and LA 35 had intragroup DNA homology values above 93.6%, showing that they belong to the species Pediococcus acidilactici. Strain LS 5 belonged to Pediococcus pentosaceus on the basis of DNA-DNA relatedness. All three of these strains and strain SL 1 (Lactobacillus casei, isolated from a commercial inoculant) were used as additives to alfalfa and Italian ryegrass silage preparation at two temperatures (25 and 48°C). When stored at 25°C, all of the inoculated silages were well preserved and exhibited significantly (P < 0.05) reduced fermentation losses compared to that of their control in alfalfa and Italian ryegrass silages. When stored at 48°C, silages inoculated with strains LA 3 and LA 35 were also well preserved, with a significantly (P < 0.05) lower pH, butyric acid and ammonia-nitrogen content, gas production, and dry matter loss and significantly (P < 0.05) higher lactate content than the control, but silages inoculated with LS 5 and SL 1 were of poor quality. P. acidilactici LA 3 and LA 35 are considered suitable as potential silage inoculants. PMID:10388681

Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

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

Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.

Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less

Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

DOE PAGES

Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.; ...

2016-08-25

Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less

Preparation and physico-chemical characterization of β-cyclodextrin incorporated chitosan biosorbent beads with potential environmental applications

NASA Astrophysics Data System (ADS)

Munim, Somayyah Abdul; Tahir Saddique, Muhammad; Raza, Zulfiqar Ali; Majeed, Muhammad Irfan

2018-06-01

Biosorption is one of the most efficient and feasible methods for eliminating noxious wastes from the aqueous systems. The use of non-hazardous, low-cost and biodegradable chitosan as a biosorbent is of significant importance in the above context. Present study was aimed to develop a β-cyclodextrin (β-CD) incorporated chitosan biosorbent in the form of beads. The prepared biosorbent beads were characterized using scanning electron microscopy (SEM), Fourier transform infrared (FTIR), x-ray diffraction (XRD) analysis, and thermo gravimetric analysis (TGA). The values of point of zero charge (PZC) of chitosan and β-CD incorporated chitosan beads were determined in the presence of an electrolyte by means of different methods including mass titration, salt addition and zeta potential ones. The SEM images exhibited roughened and porous morphologies which could enhance the adsorption of metal ions. The values of PZC of chitosan and β-CD incorporated chitosan biosorbent beads were found to be 6.38 and 7.12, respectively.

Food preparation supplies predict children's family meal and home-prepared dinner consumption in low-income households.

PubMed

Appelhans, Bradley M; Waring, Molly E; Schneider, Kristin L; Pagoto, Sherry L

2014-05-01

Frequent family meals and home food preparation are considered important for children's nutritional health and weight maintenance. This cross-sectional study tested whether these parent-driven behaviors are related to the availability of food preparation supplies in low-income urban households. Caregivers of children ages 6-13 provided information on family meal frequency, child consumption of home-prepared dinners, household food insecurity, and attitudes towards cooking. Researchers used a newly developed Food Preparation Checklist (FPC) to assess the availability of 41 food preparation supplies during a physical audit of the home environment. Caregivers and children provided anthropometric measurements and jointly reported on child dietary intake. In ordinal logistic regression models, greater home availability of food preparation supplies was associated with more frequent family meals and child consumption of home-prepared dinners. Associations were independent of household financial strain, food insecurity, caregiver attitudes toward cooking, and sociodemographic characteristics. Fewer food preparation supplies were available in households characterized by greater food insecurity, lower income, and negative caregiver attitudes towards cooking, but did not differ by child or caregiver weight status. As in prior studies, more frequent family meals and consumption of home-prepared dinners were associated with healthier child dietary intake in several areas. We conclude that food preparation supplies are often limited in the most socioeconomically disadvantaged households, and their availability is related to the frequency with which children consume family meals and home-prepared dinners. The potential role of food preparation supplies as contributors to socioeconomic disparities in child nutritional health and obesity deserves further study. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparation and Characterization of Silica Aerogel Microspheres

PubMed Central

Chen, Qifeng; Wang, Hui; Sun, Luyi

2017-01-01

Silica aerogel microspheres based on alkali silica sol were synthesized using the emulsion method. The experimental results revealed that the silica aerogel microspheres (4–20 µm in diameter) were mesoporous solids with an average pore diameter ranging from 6 to 35 nm. The tapping densities and specific surface areas of the aerogel microspheres are in the range of 0.112–0.287 g/cm3 and 207.5–660.6 m2/g, respectively. The diameter of the silica aerogel microspheres could be tailored by varying the processing conditions including agitation rate, water/oil ratio, mass ratio of Span 80: Tween 80, and emulsifier concentration. The effects of these parameters on the morphology and textural properties of the synthesized silica aerogel microspheres were systematically investigated. Such silica aerogel microspheres can be used to prepare large-scale silica aerogels at an ambient pressure for applications in separation and high efficiency catalysis, which requires features of high porosity and easy fill and recovery. PMID:28772795

Preparation and Characterization of Silica Aerogel Microspheres.

PubMed

Chen, Qifeng; Wang, Hui; Sun, Luyi

2017-04-20

Silica aerogel microspheres based on alkali silica sol were synthesized using the emulsion method. The experimental results revealed that the silica aerogel microspheres (4-20 µm in diameter) were mesoporous solids with an average pore diameter ranging from 6 to 35 nm. The tapping densities and specific surface areas of the aerogel microspheres are in the range of 0.112-0.287 g/cm³ and 207.5-660.6 m²/g, respectively. The diameter of the silica aerogel microspheres could be tailored by varying the processing conditions including agitation rate, water/oil ratio, mass ratio of Span 80: Tween 80, and emulsifier concentration. The effects of these parameters on the morphology and textural properties of the synthesized silica aerogel microspheres were systematically investigated. Such silica aerogel microspheres can be used to prepare large-scale silica aerogels at an ambient pressure for applications in separation and high efficiency catalysis, which requires features of high porosity and easy fill and recovery.

Preparation Characterization and Electrical Study of New Polymeric Mixture (Consist of Three Polymers) Nanocomposites

NASA Astrophysics Data System (ADS)

AL-Abodi, Entisar E.; Farouk, Azhar

2018-05-01

By using hummers’ method, graphene oxide (GO) was synthesized and by reducing it gave reduced graphene oxide (RGO). The polymeric blend contain three polymers; Poly Aniline (PANI), Poly Vinyl Acetate( PVAc),and Pecten(Pc) wich have been prepared at studied amount. The composites for above polymers with various concentrations of, graphene oxide (GO) and with reduced graphene oxide (RGO)were prepared, and than pour into films(chips). The dielectric constant properties of chips were measured, which its point the electrical conductivity values for the prepared chips increase with increasing of frequency. As well, the electrical conductivity is research in terms of the Arrhenius plot, it is plotted against the reverse temperature for the prepared films at different applied frequencies.

The Preparation and Enzymatic Hydrolysis of a Library of Esters

ERIC Educational Resources Information Center

Sanford, Elizabeth M.; Smith, Traci L.

2008-01-01

An investigative case study involving the preparation of a library of esters using Fischer esterification and alcoholysis of acid chlorides and their subsequent enzymatic hydrolysis by pig liver esterase and orange peel esterase is described. Students work collaboratively to prepare and characterize the library of esters and complete and evaluate…

Instruments for preparation of heterogeneous catalysts by an impregnation method

NASA Astrophysics Data System (ADS)

Yamada, Yusuke; Akita, Tomoki; Ueda, Atsushi; Shioyama, Hiroshi; Kobayashi, Tetsuhiko

2005-06-01

Instruments for the preparation of heterogeneous catalysts in powder form have been developed. The instruments consist of powder dispensing robot and an automated liquid handling machine equipped with an ultrasonic and a vortex mixer. The combination of these two instruments achieves the catalyst preparation by incipient wetness and ion exchange methods. The catalyst library prepared with these instruments were tested for dimethyl ether steam reforming and characterized by transmission electron microscopy observations.

Hydroxyapatite with Permanent Electrical Polarization: Preparation, Characterization, and Response against Inorganic Adsorbates.

PubMed

Rivas, Manuel; Del Valle, Luis J; Armelin, Elaine; Bertran, Oscar; Turon, Pau; Puiggalí, Jordi; Alemán, Carlos

2018-04-16

Permanently polarized hydroxyapatite (HAp) particles have been prepared by applying a constant DC of 500 V at 1000 °C for 1 h to the sintered mineral. This process causes important chemical changes, as the formation of OH - defects (vacancies), the disappearance of hydrogenophosphate ions at the mineral surface layer, and structural variations reflected by the increment of the crystallinity. As a consequence, the electrochemical properties and electrical conductivity of the polarized mineral increase noticeably compared with as-prepared and sintered samples. Moreover, these increments remain practically unaltered after several months. In addition, permanent polarization favours significantly the ability of HAp to adsorb inorganic bioadsorbates in comparison with as-prepared and sintered samples. The adsorbates cause a significant increment of the electrochemical stability and electrical conductivity with respect to bare polarized HAp, which may have many implications for biomedical applications of permanently polarized HAp. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ethnopharmacological and Chemical Characterization of Salvia Species Used in Valencian Traditional Herbal Preparations

PubMed Central

Martínez-Francés, Vanessa; Hahn, Emeline; Ríos, Segundo; Rivera, Diego; Reich, Eike; Vila, Roser; Cañigueral, Salvador

2017-01-01

In Valencia Region (Spain), some wild and cultivated sages are used for medicinal purposes. Among them, Salvia officinalis subsp. lavandulifolia (SL) is widely employed and known for production of Spanish sage oil and herbal products. Nevertheless, it shares the market with S. blancoana subsp. mariolensis (SB) and, to a lesser extent, with their hybrid S. x hegelmaieri (SH). The knowledge on these two species is far low and confusion between them is possible. The aim of the present paper is to improve the ethnopharmacological, morphological and chemical knowledge of these sages, and to contribute to setting up quality specifications for improving identification and distinction from other Salvia species, such as, S. officinalis subsp. officinalis, S. x auriculata and S. microphylla var. microphylla. Samples were collected in Valencia Region and surrounding mountain areas during the ethnopharmacological field work. Twenty-nine medicinal uses were reported for SL, 13 of them being also recorded for SB. Of particular interest is a homemade liquor, used as digestive and known as “salvieta,” which is mainly prepared with SB. The macro- and microscopic characters are insufficient for identification of cut, crushed or powdered material. The study of the essential oil and a HPTLC (High Performance Thin Layer Chromatography) fingerprint of their extracts could help to distinguish SB from the other sages. The essential oil from dried aerial parts of SB (content: 1.8–4.5%) was characterized by GC-FID (Gas Chromatography with Flame Ionization Detector) and GC-MS (Gas Chromatography coupled to Mass Spectrometry) showing a composition close to that currently accepted for Spanish sage essential oil in the European Pharmacopoeia, ISO (International Standard Organization) and UNE (Una Norma Española) standards, with 1,8-cineole (13.7–45.7%) and camphor (12.1–28.6%) as major constituents. HPTLC methods, based on the analysis of hydroalcoholic and dichloromethane extracts

Preparation and characterization of oxybenzone-loaded gelatin microspheres for enhancement of sunscreening efficacy.

PubMed

Patel, M; Jain, Sunil K; Yadav, Awesh K; Gogna, D; Agrawal, G P

2006-01-01

The objective of our present study was to prepare and evaluate gelatin microspheres of oxybenzone to enhance its sunscreening efficacy. The gelatin microspheres of oxybenzone were prepared by emulsion method. Process parameters were analyzed to optimize the formulation. The in vitro drug release study was performed in pH 7.4 using cellulose acetate membrane. Microspheres prepared using oxybenzone:gelatin ratio of 1:6 showed slowest drug release and those prepared with oxybenzone:gelatin ratio of 1:2 showed fastest drug release. The gelatin microspheres of oxybenzone were incorporated in aloe vera gel. Sun exposure method using sodium nitroprusside solution was used for in vitro sunscreen efficacy testing. The formulation C5 containing oxybenzone-bearing gelatin microspheres in aloe vera gel showed best sunscreen efficacy. The formulations were evaluated for skin irritation test in human volunteers, sun protection factor, and minimum erythema dose in albino rats. These studies revealed that the incorporation of sunscreening agent-loaded microspheres into aloe vera gel greatly increased the efficacy of sunscreen formulation more than four times.

Preparation and characterization of collagen-hydroxyapatite/pectin composite.

PubMed

Wenpo, Feng; Gaofeng, Liang; Shuying, Feng; Yuanming, Qi; Keyong, Tang

2015-03-01

Pectin, a kind of plant polysaccharide, was introduced into collagen-hydroxyapatite composite system, and prepared collagen-hydroxyapatite/pectin (Col-HA/pectin) composite in situ. The structure of the composite was investigated by XRD, SEM, and FT-IR. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity of the composite were investigated as well. The results show that the inorganic substance in the composite materials is hydroxyapatite in relatively low crystallinity. A new interface appeared by the interaction among hydroxyapatite and collagen-pectin, and formed smooth fine particles. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity indicate a potential use in bone replacement for the new composite. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and characterization of aluminium-silica metal matrix composite

NASA Astrophysics Data System (ADS)

Mallikarjuna, G. B.; Basavaraj, E.

2018-04-01

Aluminum alloys are widely used in aerospace and automobile industries due to their low density and good mechanical properties, better corrosion resistance and wear, low thermal coefficient of expansion as compared to conventional metals and alloys. The excellent properties of these materials and relatively low production cost make them a very attractive for a variety of applications. In this present work, Al alloy LM13-SiO2 composites were produced by stir casting method. The reinforcement SiO2 particle size used for preparation of composites are 106 µm, 150 µm, 250 µm and 355 µm with varying amount of 3 to 12 wt% in steps of 3. The prepared composite specimens were machined as per test standards. Effects of weight percentage of SiO2 particles on wear, tensile strength of Al alloy LM13-SiO2 composites have been investigated. The microstructures of the composites were studied to know the dispersion of the SiO2 particles in matrix. Experimental results shows that there is enhanced mechanical properties, when silica weighing 9% was added to the base aluminium alloy and also similar trend exists in all four different micron size of silica and also it has been observed that addition of SiO2 particles significantly improves wear resistance properties as compared with that of unreinforced matrix.

Preparation and characterization of nano liposomes of Orthosiphon stamineus ethanolic extract in soybean phospholipids.

PubMed

Aisha, Abdalrahim F A; Majid, Amin Malik Shah Abdul; Ismail, Zhari

2014-03-27

O. stamineus is a medicinal herb with remarkable pharmacological properties. However, poor solubility of the active principles limits its medicinal value. This study sought to prepare nano liposomes of OS ethanolic extract in unpurified soybean phospholipids in order to improve its solubility and permeability. OS liposomes were prepared by the conventional film method, and were characterized for solubility, entrapment efficiency, Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), particle size and zeta potential, release, absorption in everted rat intestinal sacs, and DPPH scavenging effect. OS liposomes showed substantial enhancement of extract's solubility from 956 ± 34 to 3979 ± 139 μg/ml, with entrapment efficiency of 66.2 ± 0.9%. FTIR study indicates interaction between soybean phospholipids and OS extract. TEM and dynamic light scattering showed presence of round anionic nano liposomes with particle size and zeta potential of 152.5 ± 1.1 nm and -49.8 ± 1.0 mV, respectively. A study using the fluorescent probe pyrene showed the critical micellar concentration is 9.2 ± 2.9 μg/ml. Release studies showed 94 ± 0.1% release in non-formulated extract and 62.4 ± 0.1% in OS liposomes. Released extract from OS liposomes showed improvement in DPPH scavenging effect, IC50 = 23.5 ± 1.1 μg/ml compared to 32.4 ± 0.5 μg/ml in non-formulated extract. OS liposomes were stable at pH 5.5 and 7.4, but showed reversible agglomeration at pH 1.6. Absorption in everted rat intestinal sacs showed substantial improvement in permeability of 3'-hydroxy-5, 6, 7, 4″-tetramethoxyflavone, sinensetin, eupatorin, and 3 other unknown compounds. Enhanced solubility, absorption and antioxidant effect may improve the overall pharmacological effects and medicinal value of OS ethanolic extract.

Preparation and characterization of nano liposomes of Orthosiphon stamineus ethanolic extract in soybean phospholipids

PubMed Central

2014-01-01

Background O. stamineus is a medicinal herb with remarkable pharmacological properties. However, poor solubility of the active principles limits its medicinal value. This study sought to prepare nano liposomes of OS ethanolic extract in unpurified soybean phospholipids in order to improve its solubility and permeability. OS liposomes were prepared by the conventional film method, and were characterized for solubility, entrapment efficiency, Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), particle size and zeta potential, release, absorption in everted rat intestinal sacs, and DPPH scavenging effect. Results OS liposomes showed substantial enhancement of extract’s solubility from 956 ± 34 to 3979 ± 139 μg/ml, with entrapment efficiency of 66.2 ± 0.9%. FTIR study indicates interaction between soybean phospholipids and OS extract. TEM and dynamic light scattering showed presence of round anionic nano liposomes with particle size and zeta potential of 152.5 ± 1.1 nm and −49.8 ± 1.0 mV, respectively. A study using the fluorescent probe pyrene showed the critical micellar concentration is 9.2 ± 2.9 μg/ml. Release studies showed 94 ± 0.1% release in non-formulated extract and 62.4 ± 0.1% in OS liposomes. Released extract from OS liposomes showed improvement in DPPH scavenging effect, IC50 = 23.5 ± 1.1 μg/ml compared to 32.4 ± 0.5 μg/ml in non-formulated extract. OS liposomes were stable at pH 5.5 and 7.4, but showed reversible agglomeration at pH 1.6. Absorption in everted rat intestinal sacs showed substantial improvement in permeability of 3′-hydroxy-5, 6, 7, 4″-tetramethoxyflavone, sinensetin, eupatorin, and 3 other unknown compounds. Conclusions Enhanced solubility, absorption and antioxidant effect may improve the overall pharmacological effects and medicinal value of OS ethanolic extract. PMID:24674107

Preparation and characterization of cellulose acetate organic/inorganic hybrid films

Treesearch

Saeed S. Shojaie; Timothy G. Rials; Stephen S. Kelley

1995-01-01

A series of organic/inorganic hybrid (OIH) films were prepared using cellulose acetate (CA) as the organic component and tetraethyl orthosilicate (TEOS) as the inorganic component. The chemical, morphological, and mechanical properties of these films were evaluated with a variety of analytical techniques. The results of these evaluations showed that crosslinked CA OIH...

Nickel hydroxide nanoparticles-reduced graphene oxide nanosheets film: layer-by-layer electrochemical preparation, characterization and rifampicin sensory application.

PubMed

Rastgar, Shokoufeh; Shahrokhian, Saeed

2014-02-01

Electrochemical deposition, as a well-controlled synthesis procedure, has been used for subsequently layer-by-layer preparation of nickel hydroxide nanoparticle-reduced graphene oxide nanosheets (Ni(OH)2-RGO) on a graphene oxide (GO) film pre-cast on a glassy carbon electrode surface. The surface morphology and nature of the nano-hybrid film (Ni(OH)2-RGO) was thoroughly characterized by scanning electron and atomic force microscopy, spectroscopy and electrochemical techniques. The modified electrode appeared as an effective electro-catalytic model for analysis of rifampicin (RIF) by using linear sweep voltammetry (LSV). The prepared modified electrode exhibited a distinctly higher activity for electro-oxidation of RIF than either GO, RGO nanosheets or Ni(OH)2 nanoparticles. Enhancement of peak currents is ascribed to the fast heterogeneous electron transfer kinetics that arise from the synergistic coupling between the excellent properties of RGO nanosheets (such as high density of edge plane sites, subtle electronic characteristics and attractive π-π interaction) and unique properties of metal nanoparticles. Under the optimized analysis conditions, the modified electrode showed two oxidation processes for rifampicin at potentials about 0.08 V (peak I) and 0.69 V (peak II) in buffer solution of pH 7.0 with a wide linear dynamic range of 0.006-10.0 µmol L(-1) and 0.04-10 µmol L(-1) with a detection limit of 4.16 nmol L(-1) and 2.34 nmol L(-1) considering peaks I and II as an analytical signal, respectively. The results proved the efficacy of the fabricated modified electrode for simple, low cost and highly sensitive medicine sensor well suited for the accurate determinations of trace amounts of rifampicin in the pharmaceutical and clinical preparations. © 2013 Elsevier B.V. All rights reserved.

Preparation of graphite intercalation compounds containing oligo and polyethers

NASA Astrophysics Data System (ADS)

Zhang, Hanyang; Lerner, Michael M.

2016-02-01

Layered host-polymer nanocomposites comprising polymeric guests between inorganic sheets have been prepared with many inorganic hosts, but there is limited evidence for the incorporation of polymeric guests into graphite. Here we report for the first time the preparation, and structural and compositional characterization of graphite intercalation compounds (GICs) containing polyether bilayers. The new GICs are obtained by either (1) reductive intercalation of graphite with an alkali metal in the presence of an oligo or polyether and an electrocatalyst, or (2) co-intercalate exchange of an amine for an oligo or polyether in a donor-type GIC. Structural characterization of products using powder X-ray diffraction, Raman spectroscopy, and thermal analyses supports the formation of well-ordered, first-stage GICs containing alkali metal cations and oligo or polyether bilayers between reduced graphene sheets.Layered host-polymer nanocomposites comprising polymeric guests between inorganic sheets have been prepared with many inorganic hosts, but there is limited evidence for the incorporation of polymeric guests into graphite. Here we report for the first time the preparation, and structural and compositional characterization of graphite intercalation compounds (GICs) containing polyether bilayers. The new GICs are obtained by either (1) reductive intercalation of graphite with an alkali metal in the presence of an oligo or polyether and an electrocatalyst, or (2) co-intercalate exchange of an amine for an oligo or polyether in a donor-type GIC. Structural characterization of products using powder X-ray diffraction, Raman spectroscopy, and thermal analyses supports the formation of well-ordered, first-stage GICs containing alkali metal cations and oligo or polyether bilayers between reduced graphene sheets. Electronic supplementary information (ESI) available: Domain size, additional Raman spectra info, compositional calculation, and packing fractions. See DOI: 10.1039/c5

Preparation and Characterization of Fluorescent Derivatives of Chicken Egg White Lysozyme

NASA Technical Reports Server (NTRS)

Sumida, John; Forsythe, Elizabeth; Pusey, Marc

2000-01-01

Fluorescence is one of the most versatile and powerful tools for the study of macromolecules. While most proteins are intrinsically fluorescent, working at crystallization concentrations require the use of covalently prepared derivatives added as tracers. This approach requires derivatives that do not markedly affect the crystal packing. We have prepared a number of fluorescent derivatives of chicken egg white lysozyme with probes bound to one of two different sites on the protein molecule. Lucifer yellow, cascade blue, and 5-(2-aminoethyl)aminonapthalene-l-sulfonic acid (EDANS) have been attached to the side chain carboxyl of asp101 using a carbodiimide coupling procedure. asp101 lies within the active site cleft, and it is believed that the probes are at least partially "buried" within that cleft. Lucifer yellow and MANS probes with iodoacetamide reactive groups have been bound to hisl5, located on the "back side" of the molecule relative to the active site. The fluorescently labeled protein is readily purified from the starting material by cation exchange chromatography. All the derivatives fluoresce in both the solution and the crystalline states. Fluorescence characterization has focused on determining the bound probe quantum yields, lifetimes, absorption and emission spectra, and quenching by added solutes in comparison to the free probe. No appreciable changes are found in the lifetimes of any of the probes except for cascade blue, where Tau(sub free) = 3.52 ns vrs Tau(sub bound) = 2.8 ns. Spectral shifts are found in most cases. Particularly strong quenching upon binding is found in the case of the cascade blue derivative, likely due to probe interactions with the active site cleft. While none of the asp101 bound probes are well quenched by commonly employed solutes, such as potassium and sodium iodide, acrylamide, primuline, the chloride salts of manganese, cesium, and cobalt, trifluoroacetamide, trichloroethanol, and thallium iodide, in those cases where

Optimized preparation and characterization of CLEA-lipase from cocoa pod husk.

PubMed

Khanahmadi, Soofia; Yusof, Faridah; Amid, Azura; Mahmod, Safa Senan; Mahat, Mohd Khairizal

2015-05-20

Cross-linked enzyme aggregate (CLEA) is easily prepared from crude enzyme and has many advantages to the environment and it is considered as an economic method in the context of industrial biocatalysis compared to free enzyme. In this work, a highly active and stable CLEA-lipase from cocoa pod husk (CPH) which is a by-product after removal of cocoa beans, were assayed for their hydrolytic activity and characterized under the optimum condition successfully. Face centered central composite design (FCCCD) under response surface methodology (RSM) was used to get the optimal conditions of the three significant factors (concentration of ammonium sulfate, concentration of glutaraldehyde and concentration of additive) to achieve higher enzyme activity of CLEA. From 20 runs, the highest activity recorded was around 9.407U (83% recovered activity) under the condition of using 20% saturated ammonium sulfate, 60mM glutaraldehyde as cross-linker and 0.17mM bovine serum albumin as feeder. Moreover, the optimal reaction temperature and pH value in enzymatic reaction for both crude enzyme and immobilized were found to be 45°C at pH 8 and 60°C at pH 8.2, respectively. A systematic study of the stability of CLEA and crude enzyme was taken with regards to temperature (25-60°C) and pH (5-10) value and in both factors, CLEA-lipase showed more stability than free lipase. The Km value of CLEA was higher compared to free enzyme (0.55mM vs. 0.08mM). The CLEA retained more than 60% of the initial activity after six cycles of reuse compared to free enzyme. The high stability and recyclability of CLEA-lipase from CPH make it efficient for different industrial applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and characterization of NiW-nHA composite catalyst for hydrocracking

NASA Astrophysics Data System (ADS)

Zhou, Gang; Hou, Yongzhao; Liu, Lei; Liu, Hongru; Liu, Can; Liu, Jing; Qiao, Huiting; Liu, Wenyong; Fan, Yubo; Shen, Shituan; Rong, Long

2012-11-01

The synthesis, characterization and catalytic capability of the NiW-nano-hydroxyapatite (NiW-nHA) composite were investigated in this paper. The NiW-nHA catalyst was prepared by a co-precipitation method. Then Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDX) were used to analyze this material. In addition, the catalytic capacity of the NiW-nHA composite was also examined by FT-IR and gas chromatography (GC). The results of FT-IR analysis indicated that Ni, W and nHA combined closely. TEM observation revealed that this catalyst was needle shaped and the crystal retained a nanometer size. XRD data also suggested that a new phase of CaWO4 appeared and the lattice parameters of nHA changed in this system. nHA was the carrier of metals. The rates of Ni/W-loading were 73.24% and 65.99% according to the EDX data, respectively. Furthermore, the conversion of 91.88% Jatropha oil was achieved at 360 °C and 3 MPa h-1 over NiW-nHA catalyst. The straight chain alkanes ranging from C15 to C18 were the main components in the production. The yield of C15-C18 alkanes was up to 83.56 wt%. The reaction pathway involved hydrocracking of the C&z.dbd;C bonds of these triglycerides from Jatropha oil. This paper developed a novel non-sulfided catalyst to obtain a ``green biofuel'' from vegetable oil.

Preparation of Monodomain Liquid Crystal Elastomers and Liquid Crystal Elastomer Nanocomposites.

PubMed

Kim, Hojin; Zhu, Bohan; Chen, Huiying; Adetiba, Oluwatomiyin; Agrawal, Aditya; Ajayan, Pulickel; Jacot, Jeffrey G; Verduzco, Rafael

2016-02-06

LCEs are shape-responsive materials with fully reversible shape change and potential applications in medicine, tissue engineering, artificial muscles, and as soft robots. Here, we demonstrate the preparation of shape-responsive liquid crystal elastomers (LCEs) and LCE nanocomposites along with characterization of their shape-responsiveness, mechanical properties, and microstructure. Two types of LCEs - polysiloxane-based and epoxy-based - are synthesized, aligned, and characterized. Polysiloxane-based LCEs are prepared through two crosslinking steps, the second under an applied load, resulting in monodomain LCEs. Polysiloxane LCE nanocomposites are prepared through the addition of conductive carbon black nanoparticles, both throughout the bulk of the LCE and to the LCE surface. Epoxy-based LCEs are prepared through a reversible esterification reaction. Epoxy-based LCEs are aligned through the application of a uniaxial load at elevated (160 °C) temperatures. Aligned LCEs and LCE nanocomposites are characterized with respect to reversible strain, mechanical stiffness, and liquid crystal ordering using a combination of imaging, two-dimensional X-ray diffraction measurements, differential scanning calorimetry, and dynamic mechanical analysis. LCEs and LCE nanocomposites can be stimulated with heat and/or electrical potential to controllably generate strains in cell culture media, and we demonstrate the application of LCEs as shape-responsive substrates for cell culture using a custom-made apparatus.

Preparation of Stable Amyloid-β Oligomers Without Perturbative Methods.

PubMed

Kotler, Samuel A; Ramamoorthy, Ayyalusamy

2018-01-01

Soluble amyloid-β (Aβ) oligomers have become a focal point in the study of Alzheimer's disease due to their ability to elicit cytotoxicity. A number of recent studies have concentrated on the structural characterization of soluble Aβ oligomers to gain insight into their mechanism of toxicity. Consequently, providing reproducible protocols for the preparation of such oligomers is of utmost importance. The method presented in this chapter details a protocol for preparing an Aβ oligomer, with a primarily disordered secondary structure, without the need for chemical modification or amino acid substitution. Due to the stability of these disordered Aβ oligomers and the reproducibility with which they form, they are amenable for biophysical and high-resolution structural characterization.

Polyimide Nanocomposites Prepared from High-Temperature, Reduced Charge Organoclays

NASA Technical Reports Server (NTRS)

Delozier, D. M.; Orwoll, R. A.; Cahoon, J. F.; Ladislaw, J. S.; Smith, J. G., Jr.; Connell, J. W.

2003-01-01

Montmorillonite clays modified with the dihydrochloride salt of 1,3-bis(3-aminophenoxy)benzene (APB) were used in the preparation of polyimide/organoclay hybrid films. Organoclays with varying surface charge based upon APB were prepared and examined for their dispersion behavior in the polymer matrix. High molecular weight poly(amide acid) solutions were prepared in the presence of the organoclays. Films were cast and subsequently heated to 300C to cause imidization. The resulting nanocomposite films, containing 3 wt% of organoclay, were characterized by transmission electron microscopy and X-ray diffraction. The clay's cation exchange capacity (CEC) played a key role in determining the extent of dispersion in the polyimide matrix. Considerable dispersion was observed in some of the nanocomposite films. The most effective organoclay was found to have a CEC of 0.70 meq/g. Nanocomposite films prepared with 3-8 wt% of this organoclay were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin-film tensile testing. High levels of clay dispersion could be achieved even at the higher clay loadings. Results from mechanical testing revealed that while the moduli of the nanocomposites increased with increasing clay loadings, both strength and elongation decreased.

Troubling Methods-Centric "Teacher Production": Social Foundations in Dance Education Teacher Preparation

ERIC Educational Resources Information Center

Risner, Doug; Barr, Sherrie

2015-01-01

Preparing dance specialist teachers to successfully educate an increasingly diverse student population highlights a number of challenges within an educational policy landscape characterized by technical production, methods-centric teacher preparation, teacher-proof curriculum, and standardization. The ramifications of these policies have…

Transdermal glimepiride delivery system based on optimized ethosomal nano-vesicles: Preparation, characterization, in vitro, ex vivo and clinical evaluation.

PubMed

Ahmed, Tarek A; El-Say, Khalid M; Aljaeid, Bader M; Fahmy, Usama A; Abd-Allah, Fathy I

2016-03-16

This work aimed to develop an optimized ethosomal formulation of glimepiride then loading into transdermal films to offer lower drug side effect, extended release behavior and avoid first pass effect. Four formulation factors were optimized for their effects on vesicle size (Y1), entrapment efficiency (Y2) and vesicle flexibility (Y3). Optimum desirability was identified and, an optimized formulation was prepared, characterized and loaded into transdermal films. Ex-vivo permeation study for the prepared films was conducted and, the permeation parameters and drug permeation mechanism were identified. Penetration through rat skin was studied using confocal laser microscope. In-vivo study was performed following transdermal application on human volunteers. The percent of alcohol was significantly affecting all the studied responses while the other factors and their interaction effects were varied on their effects on each response. The optimized ethosomal formulation showed observed values for Y1, Y2 and Y3 of 61 nm, 97.12% and 54.03, respectively. Ex-vivo permeation of films loaded with optimized ethosomal formulation was superior to that of the corresponding pure drug transdermal films and this finding was also confirmed after confocal laser microscope study. Permeation of glimepiride from the prepared films was in favor of Higushi-diffusion model and exhibited non-Fickian or anomalous release mechanism. In-vivo study revealed extended drug release behavior and lower maximum drug plasma level from transdermal films loaded with drug ethosomal formulation. So, the ethosomal formulation could be considered a suitable drug delivery system especially when loaded into transdermal vehicle with possible reduction in side effects and controlling the drug release. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation, characterization and dye adsorption of Au nanoparticles/ZnAl layered double oxides nanocomposites

NASA Astrophysics Data System (ADS)

Zhang, Yu Xin; Hao, Xiao Dong; Kuang, Min; Zhao, Han; Wen, Zhong Quan

2013-10-01

In this work, Au/ZnAl-layer double oxides (LDO) nanocomposties were prepared through a facile calcination process of AuCl4- intercalated ZnAl-layered double hydroxides (LDHs) nanocomposites. The morphology and crystal structure of these nanocomposites were characterized by Scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and N2 sorption analysis. By tailoring the process parameter, such as calcination temperature, heating time and the component composition, the adsorption properties of methyl orange (MO) on the Au/ZnAl-LDO nanocomposites were investigated in this work. In a typical adsorption process, it was found that 0.985 mg of MO (0.01 g L-1, 100 mL, 1 mg of MO in total) can be removed in 60 min by utilizing only 2.5 mg of Au/ZnAl-LDO (Au content, 1%) as adsorbents. Our adsorption data obtained from the Langmuir model also gave good values of the determination coefficient, and the saturated adsorption capacity of Au/ZnAl-LDO nanocomposites for MO was found to be 627.51 mg/g under ambient condition (e.g., room temperature, 1 atm). In principle, these hybrid nanostructures with higher adsorption abilities could be very promising adsorbents for wastewater treatment.

Optically active polyurethane@indium tin oxide nanocomposite: Preparation, characterization and study of infrared emissivity

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

Yang, Yong; Zhou, Yuming, E-mail: ymzhou@seu.edu.cn; Ge, Jianhua

Highlights: ► Silane coupling agent of KH550 was used to connect the ITO and polyurethanes. ► Infrared emissivity values of the hybrids were compared and analyzed. ► Interfacial synergistic action and orderly secondary structure were the key factors. -- Abstract: Optically active polyurethane@indium tin oxide and racemic polyurethane@indium tin oxide nanocomposites (LPU@ITO and RPU@ITO) were prepared by grafting the organics onto the surfaces of modified ITO nanoparticles. LPU@ITO and RPU@ITO composites based on the chiral and racemic tyrosine were characterized by FT-IR, UV–vis spectroscopy, X-ray diffraction (XRD), SEM, TEM, and thermogravimetric analysis (TGA), and the infrared emissivity values (8–14 μm)more » were investigated in addition. The results indicated that the polyurethanes had been successfully grafted onto the surfaces of ITO without destroying the crystalline structure. Both composites possessed the lower infrared emissivity values than the bare ITO nanoparticles, which indicated that the interfacial interaction had great effect on the infrared emissivity. Furthermore, LPU@ITO based on the optically active polyurethane had the virtue of regular secondary structure and more interfacial synergistic actions between organics and inorganics, thus it exhibited lower infrared emissivity value than RPU@ITO based on the racemic polyurethane.« less

Preparation and characterization of sprayed FTO thin films

NASA Astrophysics Data System (ADS)

Abd-Lefdil, M.; Diaz, R.; Bihri, H.; Aouaj, M. Ait; Rueda, F.

2007-06-01

Fluorine doped tin oxide (FTO) thin films have been prepared by spray pyrolysis technique with no further annealing. Films with 2.5% of fluorine grown at 400 °C present a single phase and exhibit a tetragonal structure with lattice parameters a = 4.687 Å and c = 3.160 Å. Scanning electron micrographs showed homogeneous surfaces with average grain size around 190 nm. The films are transparent in the visible zone and exhibit a high reflectance in the near infrared region. The best electrical resistivity was 6.3 × 10-4 Ω cm for FTO with 2.5% of fluorine. The ratio of transmittance in the visible to the sheet resistance are in the 0.57 × 10-2 1.96 × 10-2 {Ω }-1 range.

Preparation and Characterization of the Solid Spherical HMX/F2602 by the Suspension Spray-Drying Method

NASA Astrophysics Data System (ADS)

Ji, Wei; Li, Xiaodong; Wang, Jingyu; Ye, Baoyun; Wang, Cailing

2016-10-01

Solid spherical octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine/fluororubber2602 (HMX/F2602) was prepared by the suspension spray-drying method as follows: firstly, thinning octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) was obtained by a solvent-anti-solvent method. Secondly, thinning HMX suspended in ethyl acetate solvent in a solution of a binder-F2602-was made into a suspension. Finally, the samples were prepared by spray drying. The samples were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectrometry (XPS), X-ray diffraction (XRD), and Fourier transform infrared (FTIR), and its thermal stability as well as mechanical and spark sensitivities were measured. The results of SEM showed that the grain of HMX/F2602 was solid spherical and the particle distribution was homogeneous. The results of XPS indicated that F2602 can be successfully coated on the surface of HMX crystals. Compared to raw HMX, th characteristic drop height was increased from 19.60 to 40.37 cm, an increase of 79.10%. The friction sensitivities of HMX reduced from 100 to 28% and the spark sensitivity of HMX/F2602 increased. The critical explosion temperatures of raw HMX and HMX/F2602 were 275.43 and 274.30°C, respectively. The amount of gas evolution of raw HMX and HMX/F2602 was 0.15 and 0.12 ml.(5 g)-1, respectively. The results of DSC and vacuum stability tests (VSTs) indicate that the thermal stability of HMX/F2602 was equal to that of raw HMX and HMX and F2602 had good compatibility.

Preparation and Characterization of Minoxidil Loaded Nanostructured Lipid Carriers.

PubMed

Wang, Wenxi; Chen, Lina; Huang, Xinyan; Shao, Anna

2017-02-01

Nanostructured lipid carriers (NLCs) are interesting delivery systems for enhancing the penetration of an active substance through the skin after topical administration. The present paper described the development of a novel NLCs for minoxidil (MXD) topical delivery. Stearic acid and oleic acid that showed the highest solubility for MXD were selected as solid lipid and liquid lipid, respectively, and the NLCs were prepared by hot high pressure homogenization method. The minoxidil loaded NLCs prepared accordingly to the optimal formulation exhibited spherical shape with a mean diameter of 281.4 ± 7.4 nm, polydispersity of 0.207 ± 0.009, zeta potential of -32.90 ± 1.23 mV, drug entrapment efficiency of 92.48 ± 0.31%, and drug loading of 13.85 ± 0.47%. Storage stability studies demonstrated that the particle size and entrapment efficiency of the MXD-NLCs were not changed during 3 months both at 4°C and room temperature. Moreover, the release of MXD from the NLCs was faster than drug release from SLNs. In vitro skin permeability test demonstrated that MXD-NLCs had a more pronounced permeation and retention profile than MXD-SLNs. Furthermore, no erythema was observed after administration of MXD-NLCs. All these results indicated that the developed MXD-NLCs could be a promising and effective nanocarrier for topical delivery of MXD.

Expedient preparative isolation and tandem mass spectrometric characterization of C-seco triterpenoids from Neem oil.

PubMed

Haldar, Saikat; Mulani, Fayaj A; Aarthy, Thiagarayaselvam; Dandekar, Devdutta S; Thulasiram, Hirekodathakallu V

2014-10-31

C-seco triterpenoids are widely bioactive class of natural products with high structural complexity and diversity. The preparative isolation of these molecules with high purity is greatly desirable, although restricted due to the complexity of natural extracts. In this article we have demonstrated a Medium Pressure Liquid Chromatography (MPLC) based protocol for the isolation of eight major C-seco triterpenoids of salannin skeleton from Neem (Azadirachta indica) oil. Successive application of normal phase pre-packed silica-gel columns for the fractionation followed by reverse phase in automated MPLC system expedited the process and furnished highly pure metabolites. Furthermore, eight isolated triterpenoids along with five semi-synthesized derivatives were characterized using ultra performance liquid chromatography-electrospray ionization-quadrupole/orbitrap-MS/MS spectrometry as a rapid and sensitive identification technique. The structure-fragment relationships were established on the basis of plausible mechanistic pathway for the generation of daughter ions. The MS/MS spectral information of the triterpenoids was further utilized for the identification of studied molecules in the complex extract of stem and bark tissues from Neem. Copyright © 2014 Elsevier B.V. All rights reserved.

The preparation and characterization of novel Pt/C electrocatalysts with controlled porosity and cluster size

DOE PAGES

Coker, Eric N.; Steen, William A.; Miller, Jeffrey T.; ...

2007-05-23

Small platinum clusters have been prepared in zeolite hosts through ion exchange and controlled calcination/reduction processes. In order to enable electrochemical application, the pores of the Pt-zeolite were filled with electrically conductive carbon via infiltration with carbon precursors, polymerization, and pyrolysis. The zeolite host was then removed by acid washing, to leave a Pt/C electrocatalyst possessing quasi-zeolitic porosity and Pt clusters of well-controlled size. The electrocatalysts were characterized by TEM, XRD, EXAFS, nitrogen adsorption and electrochemical techniques. Depending on the synthesis conditions, average Pt cluster sizes in the Pt/C catalysts ranged from 1.3 to 2.0 nm. The presence of orderedmore » porosity/structure in the catalysts was evident in TEM images as lattice fringes, and in XRD as a low-angle diffraction peak with d-spacing similar to the parent zeolite. The catalysts possess micro- and meso-porosity, with pore size distributions that depend upon synthesis variables. Finally, electroactive surface areas as high as 112 m 2 g Pt -1 have been achieved in Pt/C electrocatalysts which show oxygen reduction performance comparable to standard industrial catalysts.« less

Preparation and characterization of superfine ammonium perchlorate (AP) crystals through ceramic membrane anti-solvent crystallization

NASA Astrophysics Data System (ADS)

Ma, Zhenye; Li, Cheng; Wu, Rujun; Chen, Rizhi; Gu, Zhenggui

2009-10-01

In this paper, a novel ceramic membrane anti-solvent crystallization (CMASC) method was proposed for the safe and rapid preparation ammonium perchlorate (AP) crystals, in which the acetone and ethyl acetate were chosen as solvent and anti-solvent, respectively. Comparing with the conventional liquid anti-solvent crystallization (LASC), CMASC which successfully introduces ceramic membrane with regular pore structure to the LASC as feeding medium, is favorable to control the rate of feeding rate and, therefore, to obtain size and morphology controllable AP. Several kinds of micro-sized AP particles with different morphology were obtained including polyhedral-like, quadrate-like to rod-like. The effect of processing parameters on the crystal size and shape of AP crystals such as volume ratio of anti-solvent to solvent, feeding pressure and crystallization temperature were investigated. It is found that higher volume ratio of anti-solvent to solvent, higher feeding pressure and higher temperature result in smaller particle size. Scaning electron microscopy (SEM) and X-ray diffraction (XRD) were used to characterize the resulting AP crystals. The nucleation and growth kinetic of the resulting AP crystals were also discussed.

Sun light mediated synthesis of gold nanoparticles as carrier for 6-mercaptopurine: Preparation, characterization and toxicity studies in zebrafish embryo model

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

Ganeshkumar, Moorthy; Sastry, Thotapalli Parvathaleswara; Sathish Kumar, Muniram

2012-09-15

Highlights: ► Gold nanoparticles prepared using eco-friendly method with good in vitro stability. ► Can be used as drug delivery system. ► Did not show any toxicity in zebrafish embryo. ► More toxic to cancer cells when compared to N-Au-Mp and Mp. -- Abstract: The objective of this study is to synthesize green chemistry based gold nanoparticles by sun light irradiation method. The prepared gold nanoparticles (AuNPs) were modified using folic acid and then coupled with 6-mercaptopurine. These modified nanoparticles were used as a tool for targeted drug delivery to treat laryngeal cancer. In the present study, novel bionanocomposites containingmore » nutrient agar coated gold nano particles (N-AuNPs) coupled with 6-mercaptopurine (drug) (N-AuNPs-Mp), folic acid (ligand) (N-AuNPs-Mp-Fa) and rhodamine (dye) (N-AuNPs-Rd), a fluorescent agent, were prepared and characterized by IR, UV, TEM, Particle size analysis and in vitro stability. The toxicity and fluorescence of N-Au was studied using zebrafish embryo model. The in vitro cytotoxicity of free Mp, N-Au-Mp and N-Au-Mp-Fa against HEp-2 cells was compared and found that the amount of Mp required to achieve 50% of growth of inhibition (IC{sub 50}) was much lower in N-Au-Mp-Fa than in free Mp and N-Au-Mp.« less

Rigid polyurethane foam/cellulose whisker nanocomposites: preparation, characterization, and properties.

PubMed

Li, Yang; Ren, Hongfeng; Ragauskas, Arthur J

2011-08-01

Novel rigid polyurethane nanocomposite foams have been prepared by the polymerization of a sucrose-based polyol, a glycerol-based polyol and polymeric diphenylmethane diisocyanate in the presence of cellulose whiskers. Varying amounts of sulfuric acid hydrolyzed cellulose whiskers (0.25, 0.50, 0.75 and 1.00 wt%) prepared from a commercial fully bleached softwood kraft pulp were incorporated to investigate the effect of its dosage on the mechanical and thermal properties of polyurethane nanocomposites. Fourier transform infrared spectra of the nanocomposite foams suggested that additional hydrogen bonds were developed and crosslinking occurred between the hydroxyl groups of cellulose whiskers and isocyanate groups which increased the phase separation of soft and hard segments in the polyurethane. The closed cells of control foam and nanocomposite foams were homogeneously dispersed and the cell sizes were approximately 350 microm in diameter as observed by scanning electron microscope. A substantial improvement of mechanical properties at low whisker content (< or = 1.00 wt%) was obtained, especially the compressive strength and modulus at 1.00 wt% whiskers content which were increased by 269.7% and 210.0%, respectively. Thermal stability of the nanocomposites was also enhanced as determined by differential scanning calorimetry and thermogravimetric analysis.

Preparation and characterization of zinc and copper co-doped WO3 nanoparticles: Application in photocatalysis and photobiology.

PubMed

Mohammadi, Sanaz; Sohrabi, Maryam; Golikand, Ahmad Nozad; Fakhri, Ali

2016-08-01

In this study, pure, Zn, Cu, Zn,Cu co-doped WO3 nanoparticles samples were prepared by precipitation and co-precipitation methods. These nanoparticles were characterized by field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), energy dispersive X-ray spectrometer (EDX), Dynamic light scattering (DLS), UV-visible and photoluminescence (PL) spectroscopy. The synthesized pure, Zn, Cu, Zn,Cu co-doped WO3 nanoparticles have smart optical properties and average sizes with 3.2, 3.12, 3.08 and 2.97eV of band-gap, 18.1, 23.2, 25.7 and 30.2nm, respectively. Photocatalytic activity of four nanoparticles was studying towards degradation of gentamicin antibiotic under ultraviolet and visible light irradiation. The result showed that Zn,Cu co-doped WO3 possessed high photocatalytic activity. The photocatalytic activity of WO3 nanoparticles could be remarkably increased by doping the Zn and Cu impurity. This can be attributed to the fact that the red shift of absorption edge and the trapping effect of the mono and co-doped WO3 nanoparticles. The research result presents a general and effective way to prepare different photocatalysts with enhanced visible and UV light-driven photocatalytic performance. Antibacterial activity of four different WO3 nanoparticles against Escherichia coli bacterium has been assessed by the agar disc method under light irradiation and dark medium. It is concluded from the present findings that WO3 nanoparticles can be used as an efficient antibacterial agent. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation, characterization and application of dispersible and spherical Nano-SiO2@Copolymer nanocomposite in leather tanning

NASA Astrophysics Data System (ADS)

Pan, Hui; Li, Guang-Long; Liu, Rui-Qi; Wang, Su-Xia; Wang, Xiao-Dong

2017-12-01

Dispersible and spherical silica nanoparticles (nano-SiO2) were prepared with tetraethyl silicate and different surface-modifiers via a simple method. The silica nanoparticles surface-modified with methacryloxy (propyl) trimethoxysilane (denoted as MPS-SiO2), dimethyl diallyl ammoniumchloride (denoted as DMDAAC-SiO2) and poly (methacrylic acid) (denoted as PMAA-SiO2) which are known as hydrophobic, amphiphilic and hydrophilic modifiers, respectively, exhibited excellent dispersibility in various solvents or polymer matrix. The obtained bare silica nanoparticles, MPS-SiO2, DMDAAC-SiO2 and PMAA-SiO2 were characterized by Fourier transform infrared spectra (FTIR), thermogravimetric analysis (TGA), transmission electron microscope (TEM) and scanning electron microscope (SEM). A series of nanocomposites (denoted as SiO2/P, MPS-SiO2/P, DMDAAC-SiO2/P and PMAA-SiO2/P, respectively) were also prepared with the bare or surface-modified silica nanoparticles and methacrylic acid-co-acrylamide-co-acrylonitrile-co-salicylic acid tetrabasic copolymer (denoted as PMAAS) and applied in leather tanning. Compared with those of the leather tanned with the commercial acrylic resin (CHINATAN OM) and pure tetrabasic copolymer tanning agents, the physical and mechanical properties, rheological properties and thermal stabilities of the leather treated with SiO2/P, MPS-SiO2/P, DMDAAC-SiO2/P or PMAA-SiO2/P founded to be improved in a significant way. Moreover, the highest shrinkage temperature of the wet-white sheepskin tanned with PMAA-SiO2/P reached to 76 °C and the thickness increase reached to 105%.

New nanoparticles obtained by co-assembly of amphiphilic cyclodextrins and nonlamellar single-chain lipids: Preparation and characterization.

PubMed

Nguyễn, Cảnh Hưng; Putaux, Jean-Luc; Santoni, Gianluca; Tfaili, Sana; Fourmentin, Sophie; Coty, Jean-Baptiste; Choisnard, Luc; Gèze, Annabelle; Wouessidjewe, Denis; Barratt, Gillian; Lesieur, Sylviane; Legrand, François-Xavier

2017-10-15

This work aimed at preparing new nanoscale assemblies based on an amphiphilic bio-esterified β-cyclodextrin (β-CD), substituted at the secondary face with n-decanoic fatty acid chains (β-CD-C 10 ), and monoolein (MO) as new carriers for parenteral drug delivery. Stable binary (β-CD-C 10 /MO) and ternary (β-CD-C 10 /MO/stabilizer) nanoscale assemblies close to 100nm in size were successfully prepared in water by the solvent displacement method. The generated nanoparticles were fully characterized by dynamic light scattering, transmission electron microscopy, small-angle X-ray scattering, residual solvent analysis, complement activation and the contribution of each formulation parameter was determined by principal component analysis. The β-CD-C 10 units were shown to self-organize into nanoparticles with a hexagonal supramolecular packing that was significantly modulated by the molar ratio of the constituents and the presence of a steric or electrostatic stabilizer (DOPE-PEG 2000 or DOPA/POPA, respectively). Indeed, nanoparticles differing in morphology and in hexagonal lattice parameters were obtained while the co-existence of multiple mesophases was observed in some formulations, in particular for the β-CD-C 10 /MO/DOPA and β-CD-C 10 /MO/POPA systems. The mixed β-CD-C 10 /MO/DOPE-PEG 2000 nanoparticles (49:49:2 in mol%) appeared to be the most suitable for use as a drug delivery system since they contained a very low amount of residual solvent and showed a low level of complement C3 activation. Copyright © 2017 Elsevier B.V. All rights reserved.

Gold nanoparticles tethered cinnamic acid: preparation, characterization, and cytotoxic effects on MCF-7 breast cancer cell lines

NASA Astrophysics Data System (ADS)

Subramanian, Karthika; Ponnuchamy, Kumar

2018-04-01

The main objective of the study is to tether citrate-stabilized gold nanoparticles (CS©GNPs) with cinnamic acid (CA) and evaluating them against MCF-7 breast cancer cells. To achieve CA CS©GNPs, CS©GNPs prepared were blended with CA under controlled experimental conditions followed by high-throughput characterization. The result from the study demonstrates that positively charged hydrogen moiety present in O-H group of CA provides an opportunity for binding of CS©GNPs via hydrogen bonding evidenced by color change (ruby to light purple) and spectroscopic analysis (UV-visible and FT-IR spectroscopy). The size and shape of CA CS©GNPs were not the same as CS©GNPs substantiated by transmission electron microscopy (TEM) and dynamic light scattering (DLS) measurements. At the end, cytotoxic and morphological assessment against MCF-7 breast cancer cells shows effective suppression of tumor cells and thereby promoting them as promising nanoscale drug delivery system in near future.

Characterization and emulsifying properties of β-lactoglobulin-gum Acacia Seyal conjugates prepared via the Maillard reaction.

PubMed

Bi, Binwei; Yang, Hao; Fang, Yapeng; Nishinari, Katsuyoshi; Phillips, Glyn O

2017-01-01

Gum Acacia Seyal (ASY) is less valued than is gum Acacia Senegal, due to its poor emulsifying ability. The present study investigated the Maillard reaction between ASY and β-lactoglobulin (BLG) and its impact on the emulsifying properties of ASY. The reaction products of BLG/ASY mixture (r=1/4), prepared by dry-heating at 60°C and a relative humidity of 79%, as a function of incubation time, were characterized by SDS-PAGE, GPC-MALLS and DSC. The results showed that 12-24h of dry-heating under the given conditions was sufficient for conjugation, meanwhile avoiding the formation of deeply coloured and insoluble melanoidins. More than 64% of the protein was incorporated into ASY, resulting in a two-fold increase in arabinogalactan-protein (AGP) content and 3.5 times increase in weight-average molecular mass of ASY. The conjugation with BLG markedly improved the stability of ASY-stabilized emulsions and their resistance against severe conditions, such as low pH and high saline conditions. Copyright © 2016 Elsevier Ltd. All rights reserved.

Preparation, characterization and catalytic behavior of pectinase covalently immobilized onto sodium alginate/graphene oxide composite beads.

PubMed

Dai, Xiao-Yan; Kong, Li-Min; Wang, Xiao-Ling; Zhu, Qing; Chen, Kai; Zhou, Tao

2018-07-01

Pectinase was immobilized onto sodium alginate/graphene oxide beads via amide bonds by using N,N'-dicyclohexylcarbodiimide/N-hydroxysuccinimide as the activating agent. The immobilized pectinase was characterized by Fourier transform infrared spectra and scanning electron microscopy analyses. Immobilization conditions were optimized by Box-Behnken design and the response surface method. The activity of the immobilized pectinase prepared under optimal conditions reached 1236.86 ± 40.21 U/g, with an enzyme activity recovery of 83.5%. The optimal pH of free pectinase was 4.5, while that of immobilized pectinase was shifted to 4.0. The optimal temperature of immobilized pectinase was increased to 60 °C, which was 10 °C higher than that of free form. Furthermore, the immobilized pectinase possessed a superior thermal stability and storage stability to those of free pectinase. Reusability studies indicated that the immobilized pectinase retained 73% of initial activity after six times cycles. Due to these good properties, such immobilized pectinase may find application in food industry. Copyright © 2018 Elsevier Ltd. All rights reserved.

Preparation and Characterization of Polyvinyl Alcohol-Chitosan Composite Films Reinforced with Cellulose Nanofiber

PubMed Central

Choo, Kaiwen; Ching, Yern Chee; Chuah, Cheng Hock; Julai, Sabariah; Liou, Nai-Shang

2016-01-01

In this study microcrystalline cellulose (MCC) was oxidized by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation. The treated cellulose slurry was mechanically homogenized to form a transparent dispersion which consisted of individual cellulose nanofibers with uniform widths of 3–4 nm. Bio-nanocomposite films were then prepared from a polyvinyl alcohol (PVA)-chitosan (CS) polymeric blend with different TEMPO-oxidized cellulose nanofiber (TOCN) contents (0, 0.5, 1.0 and 1.5 wt %) via the solution casting method. The characterizations of pure PVA/CS and PVA/CS/TOCN films were performed in terms of field emission scanning electron microscopy (FESEM), tensile tests, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). The results from FESEM analysis justified that low loading levels of TOCNs were dispersed uniformly and homogeneously in the PVA-CS blend matrix. The tensile strength and thermal stability of the films were increased with the increased loading levels of TOCNs to a maximum level. The thermal study indicated a slight improvement of the thermal stability upon the reinforcement of TOCNs. As evidenced by the FTIR and XRD, PVA and CS were considered miscible and compatible owing to hydrogen bonding interaction. These analyses also revealed the good dispersion of TOCNs within the PVA/CS polymer matrix. The improved properties due to the reinforcement of TOCNs can be highly beneficial in numerous applications. PMID:28773763

Preparation and characterization of trihydroxamic acid functionalized carbon materials for the removal of Cu(II) ions from aqueous solution

NASA Astrophysics Data System (ADS)

Godino-Salido, M. Luz; Santiago-Medina, Antonio; López-Garzón, Rafael; Gutiérrez-Valero, María D.; Arranz-Mascarós, Paloma; López de la Torre, M. Dolores; Domingo-García, María; López-Garzón, F. Javier

2016-11-01

The main objective of this study is to prepare and characterize two functionalizated carbon materials with enhanced adsorptive properties for Cu(II). Thus, two novel hybrid materials have been prepared by a non-covalent functionalization method based on the adsorption of a pyrimidine-desferrioxamine-B conjugate compound (H4L) on two activated carbons, ACs (labelled Merck and F). The adsorption of H4L on the ACs is pH-dependent and highly irreversible. This is due to strong π-π interactions between the arene centers of the ACs and the pyrimidine moiety of H4L. The textural characterization of the AC/H4L hybrids shows large decreases of their surface areas. Thus the values of Merck and F are 1031 and 1426 m2/g respectively, while these of Merck/H4L and F/H4L hybrids are 200 and 322 m2/g. An important decrease in the micropore volumes is also found, due to the blockage of narrow porosity produced by the adsorption of H4L molecules. The ACs/H4L hybrids show larger adsorption capacities for Cu(II) (0.105(4) and 0.13(2) mmol/g, at pH 2.0, and 0.20(3) and 0.242(9) mmol/g, at pH 5.5, for Merck/H4L and F/H4L, respectively) than those of the ACs (0.024(6) and 0.096(9) mmol/g, at pH 2.0, and 0.10(2) and 0.177(8) mmol/g, at pH 5.5, for Merck and F respectively), which is explained on the basis of the complexing ability of the trihydroxamic acid functions. The desorption of Cu(II) from the ACs/H4L/Cu(II) materials in acid solution allows the regeneration of most active sites (78.5% in the case of Merck/H4L/Cu(II) and 83.0% in the case of F/H4L/Cu(II)).

Preparation, characterization, and luminescence of (SBA-15) immobilized pepsin

NASA Astrophysics Data System (ADS)

Zhai, Qing-Zhou; Sun, Si-Jia

2014-12-01

SBA-15 mesoporous silica was synthesized by hydrothermal method and its surface was methylated by treatment with methyltrimethoxysilane. Pepsin was immobilized on the obtained materials giving host-guest composite materials (SBA-15)-pepsin and (methylated SBA-15)-pepsin. The optimum conditions for preparation of these materials were established. Methylated SBA-15 (M-SBA-15) has improved immobilization efficiency of enzyme compared to initial SBA-15 silica. It was shown that with the gradual increase of NaCl solution ionic strength the immobilized amount of enzyme was reduced. Powder X-ray diffraction and Fourier transform infrared spectroscopy showed that the host frameworks in the prepared host-guest composite materials are intact and the ordered structure was retained. Scanning electron microscopic studies revealed fibrous morphologic characteristics of the SBA-15 and the immobilized pepsin composite materials. The average particle diameter of (SBA-15)-pepsin composite was 338 ± 10 and 343 ± 10 nm for (M-SBA-15)-pepsin. The low temperature N2 adsorption-desorption study at 77 K showed that the pore sizes and specific surface areas of the host-guest composite materials were smaller than those before the introduction of the enzyme, suggesting that the immobilized enzyme occupied a definite position in the host material pore channels. The UV-vis solid diffuse reflectance and luminescence studies showed that the enzyme was successfully immobilized on to the host material and that after the immobilization of enzyme on SBA-15 the conformation of pepsin macromolecule has not been changed.

Single droplet drying step characterization in microsphere preparation.

PubMed

Al Zaitone, Belal; Lamprecht, Alf

2013-05-01

Spray drying processes are difficult to characterize since process parameters are not directly accessible. Acoustic levitation was used to investigate microencapsulation by spray drying on one single droplet facilitating the analyses of droplet behavior upon drying. Process parameters were simulated on a poly(lactide-co-glycolide)/ethyl acetate combination for microencapsulation. The results allowed quantifying the influence of process parameters such as temperature (0-40°C), polymer concentration (5-400 mg/ml), and droplet size (0.5-1.37 μl) on the drying time and drying kinetics as well as the particle morphology. The drying of polymer solutions at temperature of 21°C and concentration of 5 mg/ml, shows that the dimensionless particle diameter (Dp/D0) approaches 0.25 and the particle needs 350 s to dry. At 400 mg/ml, Dp/D0=0.8 and the drying time increases to one order of magnitude and a hollow particle is formed. The study demonstrates the benefit of using the acoustic levitator as a lab scale method to characterize and study the microparticle formation. This method can be considered as a helpful tool to mimic the full scale spray drying process by providing identical operational parameters such as air velocity, temperature, and variable droplet sizes. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation, Characterization, and Selectivity Study of Mixed-Valence Sulfites

ERIC Educational Resources Information Center

Silva, Luciana A.; de Andrade, Jailson B.

2010-01-01

A project involving the synthesis of an isomorphic double sulfite series and characterization by classical inorganic chemical analyses is described. The project is performed by upper-level undergraduate students in the laboratory. This compound series is suitable for examining several chemical concepts and analytical techniques in inorganic…