Sample records for solid material phases

  1. Novel solidsolid phase change material based on polyethylene glycol and cellulose used for temperature stabilisation

    Wojda Marta


    Full Text Available Thermal management is one of crucial issues in the development of modern electronic devices. In the recent years interest in phase change materials (PCMs as alternative cooling possibility has increased significantly. Preliminary results concerning the research into possibility of the use of solid-solid phase change materials (S-S PCMs for stabilisation temperature of electronic devices has been presented in the paper. Novel solid-solid phase change material based on polyethylene glycol and cellulose has been synthesized. Attempt to improve its thermal conductivity has been taken. Material has been synthesized for the purpose of stabilisation of temperature of electronic devices.

  2. 40 CFR 227.32 - Liquid, suspended particulate, and solid phases of a material.


    ... MATERIALS Definitions § 227.32 Liquid, suspended particulate, and solid phases of a material. (a) For the... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Liquid, suspended particulate, and solid phases of a material. 227.32 Section 227.32 Protection of Environment ENVIRONMENTAL...

  3. Novel functionalized polymeric fabric and fiber material as solid support for solid-phase synthesis and biomedical applications

    Xiang, Bei

    The aim of the research is to develop novel polymer solid support by modifying or fabricating polymeric fibrous materials for peptide synthesis and biomedical applications. Originally chemical inert isotactic polypropylene (iPP) fabric was utilized and modified to serve as a functional flexible planar solid support for solid phase peptide synthesis. The modification was achieved through thermal initiated radical grafting polymerization using acrylic acid, poly (ethylene glycol) diacrylate as monomers, and benzoyl peroxide as radical initiator. The iPP fabric was successfully functionalized and possessing as high as 0.7mmol/g carboxylic acid groups. Peptide ligand LHPQF was successfully synthesized on the new functional planar support. Specific enzyme immobilization was fulfilled on the functional iPP fabric support. A commercially available ethylene-acrylic acid copolymer was made into ultrafine copolymer fiber bundles which are composed of nanofibers with diameters ranging from 200nm to 800nm. Various mixing ratios of copolymer/matrix materials were utilized to explore the effect on the final nanofiber physical properties including morphology and stability in solvents. The surface carboxylic acid groups were further converted to amino groups before the functional nanofibers can be applied in solid phase peptide synthesis. Two peptide ligands, LHPQF and HWRGWV, were also successfully synthesized on the nanofiber bundles. Streptavidin and human immunoglobulin G specific binding with the corresponding ligand which was anchored on the nanofibers was conducted successfully to illustrate the potential applications of the nanofiber materials in biomedical field. Further study on the dispersion of the ethylene-acrylic acid nanofiber bundles was pursued to take advantage of the super high active surface area of functional nanofibers. To manipulate the polymer nanofibers during synthesis and bio-assays, a technique was developed to controllably assemble and disperse the

  4. New methods and materials for solid phase extraction and high performance liquid chromatography

    Dumont, Philip John [Iowa State Univ., Ames, IA (United States)


    This paper describes methods for solid phase extraction and high performance liquid chromatography (HPLC). The following are described: Effects of Resin Sulfonation on the Retention of Polar Organic Compounds in Solid Phase Extraction; Ion-Chromatographic Separation of Alkali Metals In Non-Aqueous Solvents; Cation-Exchange Chromatography in Non-Aqueous Solvents; and Silicalite As a Stationary Phase For HPLC.

  5. Novel materials and methods for solid-phase extraction and liquid chromatography

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)


    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  6. Review of high-throughput techniques for detecting solid phase Transformation from material libraries produced by combinatorial methods

    Lee, Jonathan A.


    High-throughput measurement techniques are reviewed for solid phase transformation from materials produced by combinatorial methods, which are highly efficient concepts to fabricate large variety of material libraries with different compositional gradients on a single wafer. Combinatorial methods hold high potential for reducing the time and costs associated with the development of new materials, as compared to time-consuming and labor-intensive conventional methods that test large batches of material, one- composition at a time. These high-throughput techniques can be automated to rapidly capture and analyze data, using the entire material library on a single wafer, thereby accelerating the pace of materials discovery and knowledge generation for solid phase transformations. The review covers experimental techniques that are applicable to inorganic materials such as shape memory alloys, graded materials, metal hydrides, ferric materials, semiconductors and industrial alloys.

  7. Molecularly imprinted polymers: New molecular recognition materials for selective solid-phase extraction of organic compounds

    Martín Esteban, A.


    During the last few years molecularly imprinted polymers have appeared as new selective sorbents for solid-phase extraction of organic compounds in different samples. Molecular imprinting technology involves the preparation of a polymer with specific recognition sites for certain molecules. Once the polymer has been obtained, it can be used in solid-phase extraction protocols, where a careful selection of the most appropriate solvents to be used in the different steps (sample loading, washing...

  8. Solid phase transformations

    Čermák, J


    This special-topic book, devoted to ""Solid Phase Transformations"" , covers a broad range of phenomena which are of importance in a number of technological processes. Most commercial alloys undergo thermal treatment after casting, with the aim of imparting desired compositions and/or optimal morphologies to the component phases. In spite of the fact that the topic has lain at the center of physical metallurgy for a long time, there are numerous aspects which are wide open to potential investigative breakthroughs. Materials with new structures also stimulate research in the field, as well as n

  9. Preparation and characterization of cross-linking PEG/MDI/PE copolymer as solid-solid phase change heat storage material

    Li, Wei-Dong [Key Laboratory of Cellulose and Lignocellulosics Chemistry, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100039 (China); Ding, En-Yong [Key Laboratory of Cellulose and Lignocellulosics Chemistry, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou 510650 (China)


    Phase change materials (PCMs) are a series of functional materials with storing and releasing energy properties. PCMs can impact small environment around them through storing and releasing energy during phase change process. Phase change latent heat of PCMs has two main characters: one is high enthalpy and capacity of per unit volume and the other is that the temperature over phase change process keeps constant or changes slightly. PCMs have been widely used in lots of fields such as solar energy storing, smart housing, thermo-regulated fibers and agricultural greenhouse. In this article, a novel solid-solid phase change heat storage material was synthesized via the two-step condensation reaction of high molecule weight polyethylene glycol (PEG10000) with pentaerythritol (PE) and 4,4'-diphenylmethane diisocyanate (MDI). To characterize the resulting product in comparison with pristine PEG10000, Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), thermogravimetric analyses (TGA), polarization optical microscopy (POM) and wide-angle X-ray diffraction (WAXD) measurements were employed to investigate their ingredients, thermal properties and crystalline behaviors. The results indicated that the cross-linking PCM showed typical solid-solid phase transition property, and its phase change enthalpy and crystallinity reached 152.97 kJ/kg and 81.76%, respectively. (author)

  10. Experimental Method Development for Estimating Solid-phase Diffusion Coefficients and Material/Air Partition Coefficients of SVOCs

    The solid-phase diffusion coefficient (Dm) and material-air partition coefficient (Kma) are key parameters for characterizing the sources and transport of semivolatile organic compounds (SVOCs) in the indoor environment. In this work, a new experimental method was developed to es...

  11. Preparation and characterization of porous carbon material-coated solid-phase microextraction metal fibers.

    Zhu, Fang; Guo, Jiaming; Zeng, Feng; Fu, Ruowen; Wu, Dingcai; Luan, Tiangang; Tong, Yexiang; Lu, Tongbu; Ouyang, Gangfeng


    Two kinds of porous carbon materials, including carbon aerogels (CAs), wormhole-like mesoporous carbons (WMCs), were synthesized and used as the coatings of solid-phase microextraction (SPME) fibers. By using stainless steel wire as the supporting core, six types of fibers were prepared with sol-gel method, direct coating method and direct coating plus sol-gel method. Headspace SPME experiments indicated that the extraction efficiencies of the CA fibers are better than those of the WMC fibers, although the surface area of WMCs is much higher than that of CAs. The sol-gel-CA fiber (CA-A) exhibited excellent extraction properties for non-polar compounds (BTEX, benzene, toluene, ethylbenzene, o-xylene), while direct-coated CA fiber (CA-B) presented the best performance in extracting polar compounds (phenols). The two CA fibers showed wide linear ranges, low detection limits (0.008-0.047μgL(-1) for BTEX, 0.15-5.7μgL(-1) for phenols) and good repeatabilities (RSDs less than 4.6% for BTEX, and less than 9.5% for phenols) and satisfying reproducibilities between fibers (RSDs less than 5.2% for BTEX, and less than 9.9% for phenols). These fibers were successfully used for the analysis of water samples from the Pearl River, which demonstrated the applicability of the home-made CA fibers.

  12. Hydrophilic solid-phase extraction of melamine with ampholine-modified hybrid organic-inorganic silica material.

    Wang, Tingting; Zhu, Yiming; Ma, Junfeng; Xuan, Rongrong; Gao, Haoqi; Liang, Zhen; Zhang, Lihua; Zhang, Yukui


    In this work, an ampholine-functionalized hybrid organic-inorganic silica sorbent was successfully used to extract melamine from a milk formula sample by a hydrophilic interaction solid-phase extraction protocol. Primary factors affecting the extraction efficiency of the material such as extraction solvent, elution solvent, sample loading volume, and elution volume have been thoroughly optimized. Under the optimized hydrophilic solid-phase extraction conditions, the recoveries of melamine spiked in milk formula samples ranged from 86.2 to 101.8% with relative standard deviations of 4.1-9.4% (n = 3). The limit of detection (S/N = 3) was 0.32 μg/g. The adsorption capacity toward melamine was 30 μg of melamine per grams of sorbent. Due to its simplicity, rapidity and cost effectiveness, the newly developed hydrophilic solid-phase extraction method should provide a promising tool for daily monitoring of doped melamine in milk formula.

  13. Novel restricted access materials combined to molecularly imprinted polymers for selective solid-phase extraction of organophosphorus pesticides from honey.

    He, Juan; Song, Lixin; Chen, Si; Li, Yuanyuan; Wei, Hongliang; Zhao, Dongxin; Gu, Keren; Zhang, Shusheng


    A novel restricted access materials (RAM) combined to molecularly imprinted polymers (MIPs), using malathion as template molecule and glycidilmethacrylate (GMA) as pro-hydrophilic co-monomer, were prepared for the first time. RAM-MIPs with hydrophilic external layer were characterized by scanning electron microscopy and recognition and selectivity properties were compared with the restricted access materials-non-molecularly imprinted polymers (RAM-NIPs) and unmodified MIPs. RAM-MIPs were used as the adsorbent enclosed in solid phase extraction column and several important extraction parameters were comprehensively optimized to evaluate the extraction performance. Under the optimum extraction conditions, RAM-MIPs exhibited comparable or even higher selectivity with greater extraction capacity toward six kinds of organophosphorus pesticides (including malathion, ethoprophos, phorate, terbufos, dimethoate, and fenamiphos) compared with the MIPs and commercial solid phase extraction columns. The RAM-MIPs solid phase extraction coupled with gas chromatography was successfully applied to simultaneously determine six kinds of organophosphorus pesticides from honey sample. The new established method showed good linearity in the range of 0.01-1.0 μg mL(-1), low limits of detection (0.0005-0.0019 μg mL(-1)), acceptable reproducibility (RSD, 2.26-4.81%, n = 6), and satisfactory relative recoveries (90.9-97.6%). It was demonstrated that RAM-MIPs solid phase extraction with excellent selectivity and restricted access function was a simple, rapid, selective, and effective sample pretreatment method.

  14. Graphene-Based Materials as Solid Phase Extraction Sorbent for Trace Metal Ions, Organic Compounds, and Biological Sample Preparation.

    Ibrahim, Wan Aini Wan; Nodeh, Hamid Rashidi; Sanagi, Mohd Marsin


    Graphene is a new carbon-based material that is of interest in separation science. Graphene has extraordinary properties including nano size, high surface area, thermal and chemical stability, and excellent adsorption affinity to pollutants. Its adsorption mechanisms are through non-covalent interactions (π-π stacking, electrostatic interactions, and H-bonding) for organic compounds and covalent interactions for metal ions. These properties have led to graphene-based material becoming a desirable adsorbent in a popular sample preparation technique known as solid phase extraction (SPE). Numerous studies have been published on graphene applications in recent years, but few review papers have focused on its applications in analytical chemistry. This article focuses on recent preconcentration of trace elements, organic compounds, and biological species using SPE-based graphene, graphene oxide, and their modified forms. Solid phase microextraction and micro SPE (µSPE) methods based on graphene are discussed.

  15. Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography

    Freeze, Ronald [Iowa State Univ., Ames, IA (United States)


    Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can be injected directly into the liquid chromatographic system with no pretreatment. A new surfactant, a sulfonated form of Brij-30 (Brij-S) is shown to prevent the uptake of serum proteins on commercial HPLC columns by forming a thin coating on the silica C18 surface. Excellent separations of eight or more drugs with a wide range of retention times were obtained. The separations had sharper peaks and lower retention times than similar separations performed with the surfactant sodium dodecylsulfate (SDS). Quantitative recovery of a number of drugs with limits of detection near 1 ppm with a 5 μl injection volume were obtained. Finally, a method for solid-phase extraction in a syringe is introduced. The system greatly reduced the volume of solvent required to elute adsorbed analytes from the SPE bed while providing a semi-automated setup. SPE in a syringe consists of a very small bed of resin-loaded membrane packed into a GC or HPLC syringe. After extraction, elution was performed with just a few μl of solvent. This small elution volume allowed injection of the eluent directly from the syringe into the chromatographic system, eliminating the handling problems associated with such small volumes.

  16. Use of gas chromatography-mass spectrometry/solid phase microextraction for the identification of MVOCs from moldy building materials.

    Wady, Loay; Bunte, Annicka; Pehrson, Christina; Larsson, Lennart


    Gas chromatography-mass spectrometry/solid phase microextraction (GC-MS/SPME) was applied to identify microbial volatile organic compounds (MVOCs) in water-damaged, mold-infested building materials (gypsum board papers (n=2), mineral wool, and masonite) and in cultivated molds (Aspergillus penicillioides, Stachybotrys chartarum, and Chaetomium globosum). Three SPME fibers (65-microm PDMS-DVB, 75-microm Carboxen-PDMS, and 70-microm Carbowax-stableflex) designed for automated injection were used of which the latter showed best performance. A number of previously reported MVOCs were detected both in the building materials and the cultivated molds. In addition, methyl benzoate was identified both in the S. chartarum and A. penicillioides cultures and in the building materials. SPME combined with GC-MS may be a useful method for the determination of MVOCs emitted from mold-infested building materials.

  17. Solid phase transformations II

    Čermák, J


    This topical volume includes ten invited papers that cover selected areas of the field of solid phase transformations. The first two contributions represent a burgeoning branch; that of the computer simulation of physical phenomena. The following three articles deal with the thermodynamics of phase transformations as a basic theory for describing the phenomenology of phase changes in matter. The next paper describes the interconnections between structural stability and the electronic structure of phases. Two further articles are devoted to displacive transformations; a field where there are ma

  18. Solid-phase microextraction

    Nilsson, Torben

    The objective of this study has been to develop new analytical methods using the rapid, simple and solvent-free extraction technique solid-phase microextraction (SPME) for the quantitative analysis of organic pollutants at trace level in drinking water and environmental samples. The dynamics...

  19. Solid phases of tenoxicam.

    Cantera, Rodrigo G; Leza, María G; Bachiller, Carmen M


    In this report we describe the preparation and characterization of four polymorphic forms of tenoxicam; they are, three 1:1 stoichiometric solvates with acetonitrile, dioxane, and N,N-dimethylformamide, and an amorphous phase obtained by recrystallization in various solvents. Polymorph IV and solvates with dioxane and N,N-dimethylformamide are reported for the first time in this paper. In addition, three solvates were crystallized in acetone, ethyl acetate, and isopropyl alcohol. These solid forms were characterized by X-ray powder diffraction, differential scanning calorimetry, infrared spectroscopy, thermogravimetry, optical microscopy, and elemental analysis. Solid-state properties, intrinsic dissolution rate, and dissolution kinetics from formulated tablets are also provided.

  20. Sheared solid materials

    Akira Onuki; Akira Furukawa; Akihiko Minami


    We present a time-dependent Ginzburg–Landau model of nonlinear elasticity in solid materials. We assume that the elastic energy density is a periodic function of the shear and tetragonal strains owing to the underlying lattice structure. With this new ingredient, solving the equations yields formation of dislocation dipoles or slips. In plastic flow high-density dislocations emerge at large strains to accumulate and grow into shear bands where the strains are localized. In addition to the elastic displacement, we also introduce the local free volume . For very small the defect structures are metastable and long-lived where the dislocations are pinned by the Peierls potential barrier. However, if the shear modulus decreases with increasing , accumulation of around dislocation cores eventually breaks the Peierls potential leading to slow relaxations in the stress and the free energy (aging). As another application of our scheme, we also study dislocation formation in two-phase alloys (coherency loss) under shear strains, where dislocations glide preferentially in the softer regions and are trapped at the interfaces.

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

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


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

  2. Advanced functional materials in solid phase extraction for ICP-MS determination of trace elements and their species - A review.

    He, Man; Huang, Lijin; Zhao, Bingshan; Chen, Beibei; Hu, Bin


    For the determination of trace elements and their species in various real samples by inductively coupled plasma mass spectrometry (ICP-MS), solid phase extraction (SPE) is a commonly used sample pretreatment technique to remove complex matrix, pre-concentrate target analytes and make the samples suitable for subsequent sample introduction and measurements. The sensitivity, selectivity/anti-interference ability, sample throughput and application potential of the methodology of SPE-ICP-MS are greatly dependent on SPE adsorbents. This article presents a general overview of the use of advanced functional materials (AFMs) in SPE for ICP-MS determination of trace elements and their species in the past decade. Herein the AFMs refer to the materials featuring with high adsorption capacity, good selectivity, fast adsorption/desorption dynamics and satisfying special requirements in real sample analysis, including nanometer-sized materials, porous materials, ion imprinting polymers, restricted access materials and magnetic materials. Carbon/silica/metal/metal oxide nanometer-sized adsorbents with high surface area and plenty of adsorption sites exhibit high adsorption capacity, and porous adsorbents would provide more adsorption sites and faster adsorption dynamics. The selectivity of the materials for target elements/species can be improved by using physical/chemical modification, ion imprinting and restricted accessed technique. Magnetic adsorbents in conventional batch operation offer unique magnetic response and high surface area-volume ratio which provide a very easy phase separation, greater extraction capacity and efficiency over conventional adsorbents, and chip-based magnetic SPE provides a versatile platform for special requirement (e.g. cell analysis). The performance of these adsorbents for the determination of trace elements and their species in different matrices by ICP-MS is discussed in detail, along with perspectives and possible challenges in the future

  3. Determination of phthalates released from paper packaging materials by solid-phase extraction-high-performance liquid chromatography.

    Gao, Xin; Yang, Bofeng; Tang, Zhixu; Luo, Xin; Wang, Fengmei; Xu, Hui; Cai, Xue


    A solid phase extraction (SPE) high-performance liquid chromatography (HPLC) method was developed for the simultaneous determination of 10 phthalic acid esters (dimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzylbutyl phthalate, diisobutyl phthalate, dicyclohexyl phthalate, diamyl phthalate, di-n-hexyl phthalate, di-n-octyl phthalate and di-2-ethylhexyl phthalate) released from food paper packaging materials. The use of distilled water, 3% acetic acid (w/v), 10% ethanol (v/v) and 95% ethanol (v/v) instead of the different types of food simulated the migration of 10 phthalic acid esters from food paper packaging materials; the phthalic acid esters in four food simulants were enriched and purified by a C18 SPE column and nitrogen blowing, and quantified by HPLC with a diode array detector. The chromatographic conditions and extraction conditions were optimized and all 10 of the phthalate acid esters had a maximum absorbance at 224 nm. The method showed limitations of detection in the range of 6.0-23.8 ng/mL the correlation coefficients were greater than 0.9999 in all cases, recovery values ranged between 71.27 and 106.97% at spiking levels of 30, 60 and 90 ng/mL and relative standard deviation values ranged from 0.86 to 8.00%. The method was considered to be simple, fast and reliable for a study on the migration of these 10 phthalic acid esters from food paper packaging materials into food.

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

    Yamanaka, Stacey A.; Charych, Deborah H.; Loy, Douglas A.; Sasaki, Darryl Y.


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

  5. Tropical peat as a versatile material for solid-phase extraction of pesticides from medicinal plant Cordia salicifolia

    Carvalho,Pedro H. V. de; Amanda M. D. de Jesus; Prata,Vanessa M.; Bezerra,Débora S. S.; Romão, Luciane P. C.; Navickiene, Sandro


    Natural peat was tested for solid-phase extraction of acephate, chlorpropham, pirimicarb, bifenthrin, tetradifon and phosalone from the medicinal plant Cordia salicifolia, using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS, SIM). Considering that there are no Brazilian regulations concerning maximum permissible pesticide residue concentrations in medicinal herbs, recovery experiments were carried out (three replicates) at two arbitrary fortification levels (0.5 and...

  6. 特种功能材料中的固态相变及应用%Solid-State Phase Transformations and Their Applications in Special Functional Materials

    徐惠彬; 宫声凯; 蒋成保; 赵新青; 李岩; 郭洪波


    固态相变已经从传统结构材料的增强增韧延伸到新型功能材料研究领域,引发多种奇特的物理效应。目前已经形成一批基于固态相变的新型功能材料。这些新型功能材料蕴含着丰富的固态相变理论。固态相变现已成为新型功能材料设计与功能特性实现的重要手段之一。文章结合作者在固态相变及特种功能材料方面的研究工作,重点介绍高温形状记忆合金、高阻尼形状记忆合金、磁致伸缩材料和热障涂层材料中的固态相变特征及其在这些特种功能材料设计与功能实现和调控中应用的研究进展。%Solid-state phase transformations have been extended from toughening and strengthening of traditional structural materials to advanced functional materials, inducing many interesting physical phenomena. Varieties of functional materials have been developed based on the solid-state phase transformations. Studies on these functional materials have effectively enriches the theories of solid-state materials. The solid-state transformation have become one of the important approaches of functional materials designing and functionalities output. This paper briefly introduces the advances in solidstate phase transformations and their applications in high-temperature shape memory alloys, high damping shape memory alloys, magnetostrictive materials, and thermal barrier coatings.

  7. Solid materials for removing arsenic and method thereof

    Coronado, Paul R.; Coleman, Sabre J.; Sanner, Robert D.; Dias, Victoria L.; Reynolds, John G.


    Solid materials have been developed to remove arsenic compounds from aqueous media. The arsenic is removed by passing the aqueous phase through the solid materials which can be in molded, granular, or powder form. The solid materials adsorb the arsenic leaving a purified aqueous stream. The materials are aerogels or xerogels and aerogels or xerogels and solid support structure, e.g., granulated activated carbon (GAC), mixtures. The species-specific adsorption occurs through specific chemical modifications of the solids tailored towards arsenic.

  8. Solid-Phase Random Glycosylation

    Agoston, K.; Kröger, Lars; Dekany, Gyula


    Two different approaches were employed to study solid phase random glycosylations to obtain oligosaccharide libraries. In approach I, Wang resin esters were attached to the acceptors structures. Following their glycosylation and resin cleavage, the peracetylated components of the oligosaccharide ...

  9. Polymers in phase change materials

    Ferreira, M.C.; Brites, M.J.; Alexandre, J.H. [National Lab. for Energy and Geology, Lisbon (Portugal)


    Phase Change Materials (PCMs) which are the core of latent heat thermal energy storage systems are currently an area of investigation of increasing interest. Several substances differing in physical and chemical characteristics as well as in thermal behavior have been studied as PCMS{sup 1-3}. In order to meet the requisites of particular systems, auxiliary materials are often used with specific functions. This bibliographic survey shows that polymeric materials have been proposed either as the PCM itself in solid-liquid or solid-solid transitions or to perform auxiliary functions of shape stabilisation and microencapsulation for solid-liquid PCMs. The PCMs have an operating temperature ranging from around 0 C (for the system water/polyacrilamid) to around 127 C (for crosslinked HDPE). (orig.)

  10. Application of Deep Eutectic Solvents in Hybrid Molecularly Imprinted Polymers and Mesoporous Siliceous Material for Solid-Phase Extraction of Levofloxacin from Green Bean Extract.

    Li, Xiaoxia; Row, Kyung Ho


    Deep eutectic solvents (DES) are potential ecofriendly surfactants for the preparation of materials. In this study, both molecularly imprinted polymers (MIPs) and mesoporous siliceous materials (MSMs) were modified by betaine-based DES. Six materials were employed as solid phase extraction (SPE) adsorbents for the rapid purification of levofloxacin. The DES-based materials showed better selective adsorption than the conventional materials. The adsorption curves of DES-MIP showed superior molecular recognition ability and binding capability for levofloxacin compared to the other materials. The limit of detection and limit of quantitation of the method were 0.01 and 0.03 μg/mL for levofloxacin, respectively. The method recoveries at three spiked levels were 97.2 - 100.2% for DES-MIP, with an RSD <1.8%. DES-MIP showed the highest selective recovery (95.2%) for levofloxacin from the green bean extract, and could remove the interferent effectively.

  11. The adsorptive properties of powdered carbon materials with a strongly differentiated porosity and their applications in electroanalysis and solid phase microextraction.

    Kuśmierek, K; Sankowska, M; Skrzypczyńska, K; Świątkowski, A


    The adsorption of 4-chlorophenol from an aqueous solution on carbonaceous materials (one carbon black and two powdered activated carbons) with a strongly differentiated porosity was investigated. The kinetic data were fitted well to the pseudo-second order model. The amount of 4-chlorophenol adsorbed at equilibrium was increased with an increase in the specific surface area of the tested materials. The adsorption isotherms were analyzed using the Langmuir and Freundlich models. The Langmuir isotherm was slightly favorable (R(2)>0.99) rather than the Freundlich isotherm (R(2)>0.98). Carbon materials were also used for the modification of carbon paste electrodes as well as for the preparation of novel solid phase microextraction fibers. The peak current of the differential pulse voltammetry curves was increased along with the amount of added carbon paste electrode modifier. The signal response was closely related to the porosity of the materials used, and increased with the increase in the specific surface area. The amount of 4-chlorophenol extracted from the samples by the solid phase microextraction fiber's surface was also correlated with the specific surface area of the tested materials. All the novel fibers were better than the commercially available fibers prepared from polidimethylosiloxane.

  12. Solid-phase peptide synthesis

    Jensen, Knud Jørgen


    This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective.......This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective....

  13. Thermal properties and structural characterizations of new types of phase change material: Anhydrous and hydrated palmitic acid/camphene solid dispersions

    Lee, Tu, E-mail:; Chiu, Yu Hsiu; Lee, Yun; Lee, Hung Lin


    Highlights: • Solid dispersion is implemented on phase change materials. • Water is added as a tertiary component. • Specific heat of solid is increased by partially amorphous camphene. • Microstructures are characterized by LTDSC, PXRD and SAXS. • Thermal properties are linked to microstructures. - Abstract: Two new types of phase change material anhydrous and hydrated palmitic acid/camphene solid dispersions (PA1CA1) are prepared and characterized by low-temperature differential scanning calorimetry, powder X-ray diffraction, small-angle X-ray scattering and temperature–history method. Their microstructures contain nanometer-sized palmitic acid (PA) crystallites with lamellar periodicity dispersed in a partially amorphous plastic crystalline camphene (CA) matrix. The PA phase apparently possesses a relatively high latent heat value inherited from the pristine crystalline PA of 229.7 ± 0.1 kJ kg{sup −1}. The relatively high specific heat of solid, C{sub ps}, for anhydrous PA1CA1 of 2.17 ± 0.06 kJ kg{sup −1} K{sup −1} is originated from the presence of disordered CA matrix. Hydration of PA1CA1 can further increase the C{sub ps} to 2.61 ± 0.01 kJ kg{sup −1} K{sup −1}. The mixing of partially amorphous CA, some PA and the small amount of water may have turned the matrix into more disorder due to their different bonding natures, molecular weights, and various molecular shapes and sizes.

  14. Distilling solid carbonaceous materials

    Ainscow, J.W.H.


    Carbonaceous materials such as coal or oil shale are distilled by being passed in a continuous stream through a retort heated externally and at temperatures increasing from the inlet to the outlet end, the distillates being taken off through openings in the retort wall.



    The solid-phase synthesis of isoxazolines on 2-polystyrylsulfonamidoethanol resin isreported. 2-Polystyrylsuifonamidoethanol resin 1 was reacted with acryloyl chloride to afford2-polystyrylsulfonylamidoethyl acrylate resin 2, which was further reacted with brominatedaldoximes by [3+2] cycioaddition to give isoxazoline resin 4. Resin 4 was treated with aqueous 6mol/L HCI solution to obtain isoxazolines in good yield and purity.

  16. Multiple solid-phase microextraction

    Koster, EHM; de Jong, GJ


    Theoretical aspects of multiple solid-phase microextraction are described and the principle is illustrated with the extraction of lidocaine from aqueous solutions. With multiple extraction under non-equilibrium conditions considerably less time is required in order to obtain an extraction yield that

  17. PEG encapsulated by porous triamide-linked polymers as support for solid-liquid phase change materials for energy storage

    Andriamitantsoa, Radoelizo S.; Dong, Wenjun; Gao, Hongyi; Wang, Ge


    A series of porous triamide-linked polymers labeled as PTP were prepared by condensation of 1,3,5-benzenetricarbonyl trichloride with benzene-1,4-diamine (A), 4,4‧-methylenediamine (B) and 1,3,5-triazine-2,4,6-triamine (C) respectively. The as-synthesized polymers exhibit permanent porosity and high surface areas which guarantee to hold polyethylene glycol (PEG) molecules in their network for shape-stabilized phase change materials. They possess different effects on the phase change properties of the composite due to their different porosities. PTP-A have intrinsic well-ordered morphology, microstructure and good enough pores to keep the PCMs compared to PTP-B and PTP-C. PEG 2000 used as PCMs could be retained up to 85 wt% in PTP-A polymer materials and these composites were defined as form-stable composite PCMs without the leakage of melted PCM. The thermal study revealed a good storage effect of encapsulated polymer and the enthalpy of melting increases in the order PTP-C storage capacity. The latent heats for melting and freezing was found to be 155 and 141.7 kJ/kg with a peak appearing at around 53.13 and 29.67 °C respectively. The study suggests that pore size is important for the preparation of shape-stabilized PCMs.

  18. Comparison of different solid-phase extraction materials for the determination of fluoroquinolones in chicken plasma by LC-MS/MS.

    Janusch, Franziska; Scherz, Gesine; Mohring, Siegrun A I; Stahl, Jessica; Hamscher, Gerd


    Fluoroquinolones are synthetic antibiotics which are frequently used in veterinary medicine e.g. for the treatment of poultry. Their specific importance is based on the fact that they are regarded as antibiotics of last resort because of their broad spectrum of action against Gram-negative and -positive bacteria. Here, a new and sensitive method for the simultaneous determination of four fluoroquinolones (marbofloxacin, ciprofloxacin, enrofloxacin and difloxacin) in chicken plasma by LC-MS/MS was developed. Solid-phase extraction was chosen for sample preparation because a selective sample clean-up is combined with an effective extraction. Various solid-phase extraction materials including polymer-based reversed-phase, silica-based reversed-phase and mixed-mode sorbents were compared. Selection criteria were analyte recovery, sample extract purity and economical aspects (analysis time and elution solvent volume). Best recoveries and minimized elution solvent volumes were achieved using polymeric reversed-phase cartridges. However, post-column infusion experiments revealed that the analysis is influenced by co-eluting matrix components. Hence, a combination of a mixed-mode anion-exchange cartridge and a mixed-mode cation-exchange cartridge was used as final extraction method. This method yield slightly lower analyte recoveries compared to polymeric-reversed-phase cartridges but exhibit no matrix effects. Recoveries of spiked chicken plasma ranged from 61.9% to 84.8% with an inter-day precision of generally less than 12%. LODs are between 0.03 and 0.05μg/L; LOQs are between 0.08 and 0.16μg/L. Maximum plasma concentrations of chickens medicated with an enrofloxacin dosage of 3mg/kg bodyweight were 38.9μg/L for enrofloxacin and 3.3μg/L for its main metabolite ciprofloxacin. Copyright © 2014 Elsevier B.V. All rights reserved.


    SUNWeimin; LUOJuntao; 等


    The solid-phase synthesis of isoxazolines on 2-polystyrylsulfonamidoethanol resin is reported.2-Polystyrylsulfonamidoethanol resin 1 was reacted with acryloyl chloride to afford 2-polystyrylsulfonylamidoethyl acrylate resin 2,which was further reacted with brominated aldoximes by [3+2] cycloaddition to give isoxazoline resin 4.Resin 4 was treated with aqueous 6 mol/L HCl solution to obtain isoxazolines in good yield and purity.

  20. Simulation study of a chaotic cavity transducer based virtual phased array used for focusing in the bulk of a solid material.

    Delrue, Steven; Van Den Abeele, Koen; Matar, Olivier Bou


    In acoustic and ultrasonic non-destructive testing techniques, it is sometimes beneficial to concentrate sound energy at a chosen location in space and at a specific instance in time, for example to improve the signal-to-noise ratio or activate the nonlinearity of damage features. Time Reversal (TR) techniques, taking advantage of the reversible character of the wave equation, are particularly suited to focus ultrasonic waves in time and space. The characteristics of the energy focusing in solid media using principles of time reversed acoustics are highly influenced by the nature and dimensions of the medium, the number of transducers and the length of the received signals. Usually, a large number of transducers enclosing the domain of interest is needed to improve the quality of the focusing. However, in the case of highly reverberant media, the number of transducers can be reduced to only one (single-channel TR). For focusing in a non-reverberant medium, which is impossible when using only one source, an adaptation of the single-channel reciprocal TR procedure has been recently suggested by means of a Chaotic Cavity Transducer (CCT), a single element transducer glued on a cavity of chaotic shape. In this paper, a CCT is used to focus elastic energy, at different times, in different points along a predefined line on the upper surface of a thick solid sample. Doing so, all focusing points can act as a virtual phased array transducer, allowing to focus in any point along the depth direction of the sample. This is impossible using conventional reciprocal TR, as you need to have access to all points in the bulk of the material for detecting signals to be used in the TR process. To asses and provide a better understanding of this concept, a numerical study has been developed, allowing to verify the basic concepts of the virtual phased array and to illustrate multi-component time reversal focusing in the bulk of a solid material.

  1. Solid phase syntheses of oligoureas

    Burgess, K.; Linthicum, D.S.; Russell, D.H.; Shin, H.; Shitangkoon, A.; Totani, R.; Zhang, A.J.; Ibarzo, J. [Texas A& M Univ., College Station, TX (United States)


    Isocyanates 7 were formed from monoprotected diamines 3 or 6, which in turn can be easily prepared from commercially available N-BOC- or N-FMOC-protected amino acid derivatives. Isocyanates 7, formed in situ, could be coupled directly to a solid support functionalized with amine groups or to amino acids anchored on resins using CH{sub 2}Cl{sub 2} as solvent and an 11 h coupling time at 25 {degree}C. Such couplings afforded peptidomimetics with an N-phthaloyl group at the N-terminus. The optimal conditions identified for removal of the N-phthaloyl group were to use 60% hydrazine in DMF for 1-3 h. Several sequences of amino acids coupled to ureas (`peptidic ureas`) and of sequential urea units (`oligoureas`) were prepared via solid phase syntheses and isolated by HPLC. Partition coefficients were measured for two of these peptidomimetics, and their water solubilities were found to be similar to the corresponding peptides. A small library of 160 analogues of the YGGFL-amide sequence was prepared via Houghten`s tea bag methodology. This library was tested for binding to the anti-{beta}-endorphin monoclonal antibody. Overall, this paper describes methodology for solid phase syntheses of oligourea derivatives with side chains corresponding to some of the protein amino acids. The chemistry involved is ideal for high-throughput syntheses and screening operations. 51 refs., 3 figs., 2 tabs.

  2. Cyclodextrin-functionalized reduced graphene oxide as a fiber coating material for the solid-phase microextraction of some volatile aromatic compounds.

    Zhang, Shuaihua; Li, Zhi; Wang, Chun; Wang, Zhi


    A novel solid phase microextraction fiber was prepared for the first time by using a sol-gel technique with hydroxypropyl-β-cyclodextrin-functionalized reduced graphene oxide as the fiber coating material. The results verified that the β-cyclodextrin was successfully grafted onto the surface of reduced graphene oxide and the coating possessed a uniform folded and wrinkled structure. The performance of the solid phase microextraction fiber was evaluated by using it to extract nine volatile aromatic compounds from water samples before determination with gas chromatography and flame ionization detection. Some important experimental parameters that could affect the extraction efficiency such as the extraction time, extraction temperature, desorption temperature, desorption time, the volume of water sample solution, stirring rate, as well as ionic strength were optimized. The new method was validated to be effective for the trace analysis of some volatile aromatic compounds, with the limits of detection ranging from 2.0 to 8.0 ng/L. Single fiber repeatability and fiber-to-fiber reproducibility were in the range of 2.5-9.4 and 5.4-12.9%, respectively. The developed method was successfully applied to the analysis of three different water samples, and the recoveries of the method were in the range from 77.9 to 113.6% at spiking levels of 10, 100, and 1000 ng/L, respectively.

  3. A powerful methodological approach combining headspace solid phase microextraction, mass spectrometry and multivariate analysis for profiling the volatile metabolomic pattern of beer starting raw materials.

    Gonçalves, João L; Figueira, José A; Rodrigues, Fátima P; Ornelas, Laura P; Branco, Ricardo N; Silva, Catarina L; Câmara, José S


    The volatile metabolomic patterns from different raw materials commonly used in beer production, namely barley, corn and hop-derived products - such as hop pellets, hop essential oil from Saaz variety and tetra-hydro isomerized hop extract (tetra hop), were established using a suitable analytical procedure based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography-quadrupole mass spectrometry detection (GC-qMS). Some SPME extraction parameters were optimized. The best results, in terms of maximum signal recorded and number of isolated metabolites, were obtained with a 50/30 μm DVB/CAR/PDMS coating fiber at 40 °C for 30 min. A set of 152 volatile metabolites comprising ketones (27), sesquiterpenes (26), monoterpenes (19), aliphatic esters (19), higher alcohols (15), aldehydes (11), furan compounds (11), aliphatic fatty acids (9), aliphatic hydrocarbons (8), sulphur compounds (5) and nitrogen compounds (2) were positively identified. Each raw material showed a specific volatile metabolomic profile. Monoterpenes in hop essential oil and corn, sesquiterpenes in hop pellets, ketones in tetra hop and aldehydes and sulphur compounds in barley were the predominant chemical families in the targeted beer raw materials. β-Myrcene was the most dominant volatile metabolite in hop essential oil, hop pellets and corn samples while, in barley, the predominant volatile metabolites were dimethyl sulphide and 3-methylbutanal and, in tetra hop, 6-methyl-2-pentanone and 4-methyl-2-pentanone. Principal component analysis (PCA) showed natural sample grouping among beer raw materials.

  4. β-Cyclodextrin cross-linked polymer as solid-phase extraction material coupled with the spectrophotometric method for the analysis of serum albumin

    Wu, Min; Zhu, Xiashi


    The β-cyclodextrin cross-linked polymer (β-CDCP) was synthesized and used as solid-phase extraction material to preconcentrate/analysis bovine serum albumin (BSA) coupled with UV-vis spectroscopy. The method based on the complex (BSA-phenylfluorone (PF)) adsorbed on β-CDCP. Adsorption kinetics and various factors of the formation procedure of BSA-PF and its retention on β-CDCP were investigated. The linear range and detection limit (DL) was 20.0-200.0 and 0.03 mg/L, respectively. Moreover, the β-CDCP could be used repeatedly. The proposed method has been applied to analysis serum albumin with satisfactory results.

  5. Solid phase extraction-capillary electrophoresis determination of sulphonamide residues in milk samples by use of C18-carbon nanotubes as hybrid sorbent materials.

    Polo-Luque, M L; Simonet, B M; Valcárcel, M


    The exceptional sorption capabilities of carbon nanotubes were used to preconcentrate trace sulphonamides from milk samples. To this end, single walled carbon nanotubes (SWNTs) and multi-walled carbon nanotubes (MWNTs) dispersed in the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate were retained on a C18 stationary phase to obtain a hybrid material in a simple manner. In this approach ionic liquids are an excellent alternative to improve the dispersion of CNTs, without chemical modification or the use of solid substances or organic solvents. MWNTs provided better results than SWNTs. Carbon nanotubes retained in the C18 sorbent matrix were found to confer aromatic character, increasing its preconcentration capacity as a result. The conventional C18 stationary phase played a two-fold role: as a support to retain carbon nanotubes in the cartridge and as a medium to prevent their aggregation. The modified MWNT/C18 and SWNT/C18 materials were used to preconcentrate residual sulphonamides (SAs) in milk samples for their determination at concentrations as low as 0.03-0.069 mg L(-1) by capillary electrophoresis. Analyte recoveries from spiked samples ranged from 103.2 to 98.8% and precision, as RSD, from 8.2 to 5.4%.

  6. Nanoprobes, nanostructured materials and solid state materials

    Yin, Houping


    Novel templates have been developed to prepare nanostructured porous materials through nonsurfactant templated pathway. And new applications of these materials, such as drug delivery and molecular imprinting, have been explored. The relationship between template content and pore structure has been investigated. The composition and pore structures were studied in detail using IR, TGA, SEM, TEM, BET and XRD. The obtained mesoporous materials have tunable diameters in the range of 2--12 nm. Due to the many advantages of this nonsurfactant templated pathway, such as environment friendly and biocompatibility, controlled release of antibiotics in the nanoporous materials were studied. The in vitro release properties were found to depend on the silica structures which were well tuned by varying the template content. A controlled long-term release pattern of vancomycin was achieved when the template content was 30 wt% or lower. Nanoscale electrochemical probes with dimensions as small as 50 nm in diameter and 1--2 mum in length were fabricated using electron beam deposition on the apex of conventional micron size electrodes. The electroactive region was limited to the extreme tip of the nanoprobe by coating with an insulating polymer and re-opening of the coating at the extreme tip. The novel nanoelectrodes thus prepared were employed to probe neurons in mouse brain slice and the results suggest that the nanoprobes were capable of recording neuronal excitatory postsynaptic potential signals. Interesting solid state chemistry was found in oxygenated iron phthalocyanine. Their Mossbauer spectra show the formation of four oxygenated species apart from the unoxygenated parent compound. The oxygen-bridged compounds formed in the solid matrix bear no resemblance to the one formed by solution chemistry. Tentative assignment of species has been made with the help of Mossbauer and IR spectroscopy. An effort to modify aniline trimer for potential nanoelectronics applications and to

  7. A novel benzimidazole-functionalized 2-D COF material: synthesis and application as a selective solid-phase extractant for separation of uranium.

    Li, Juan; Yang, Xiaodan; Bai, Chiyao; Tian, Yin; Li, Bo; Zhang, Shuang; Yang, Xiaoyu; Ding, Songdong; Xia, Chuanqin; Tan, Xinyu; Ma, Lijian; Li, Shoujian


    A novel COF-based material (COF-COOH) containing large amounts of carboxylic groups was prepared for the first time by using a simple and effective one-step synthetic method, in which the cheap and commercially available raw materials, trimesoyl chloride and p-phenylenediamine, were used. The as-synthesized COF-COOH was modified with previously synthesized 2-(2,4-dihydroxyphenyl)-benzimidazole (HBI) by "grafting to" method, and a new solid-phase extractant (COF-HBI) with highly efficient sorption performance for uranium(VI) was consequently obtained. A series of characterizations demonstrated that COF-COOH and COF-HBI exhibited great thermostabilities and irradiation stabilities. Sorption behavior of the COF-based materials toward U(VI) was compared in simulated nuclear industrial effluent containing UO2(2+) and 11 undesired ions, and the UO2(2+) sorption amount of COF-HBI was 81 mg g(-1), accounting for approximately 58% of the total sorption amount, which was much higher than the sorption selectivity of COF-COOH to UO2(2+) (39%). Batch sorption experiment results indicated that the uranium(VI) sorption on COF-HBI was a pH dependent, rapid (sorption equilibrium was reached in 30 min), endothermic and spontaneous process. In the most favorable conditions, the equilibrium sorption capacity of the adsorbent for uranium could reach 211 mg g(-1).

  8. Bamboo charcoal as a novel solid-phase microextraction coating material for enrichment and determination of eleven phthalate esters in environmental water samples.

    Zhao, Ru-Song; Liu, Yan-Long; Zhou, Jia-Bin; Chen, Xiang-Feng; Wang, Xia


    This study demonstrates the potential of bamboo charcoal as a novel and inexpensive solid-phase microextraction (SPME) coating material for enrichment and determination of organic pollutants in water samples. Bamboo charcoal was prepared and used as a SPME coating material. Eleven phthalate esters (PAEs) were used as model analytes, and gas chromatography-mass spectrometry was used for separation and detection. Important extraction conditions (ionic strength, stirring rate, and extraction time) and desorption conditions (desorption temperature and time) were systematically investigated and optimized. Linearity of 0.1-100 μg L(-1) and correlation coefficients of 0.9992-0.9998 were obtained under optimum conditions. Inter-day and intra-day repeatability were 2.15-9.93 % and 1.89-9.85 %, respectively, and fiber-to-fiber reproducibility was 5.42-9.66 %. On the basis of a chromatographic signal-to-baseline noise ratio of three, the limits of detection reached 0.004-0.023 μg L(-1). Satisfactory results were achieved when the bamboo coating was used for determination of 11 PAEs in real water samples. The experimental results indicate that bamboo charcoal has significant potential as a SPME coating material for rapid enrichment and sensitive determination of organic pollutants in environmental samples.

  9. Solid Phase Characterization of Solids Recovered from Failed Sluicer Arm

    Cooke, Gary A. [Hanford Site (HNF), Richland, WA (United States)


    The Enclosure to this memo discusses the solid phase characterization of a solid sample that was retrieved from the single-shell Tank 241-C-111 extended reach sluicer #2. This sluicer, removed from riser #3 on September 25, 2014, was found to have approximately 0.4 gallons of solid tank waste adhering to the nozzle area.

  10. Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

    Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero, E-mail:


    The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption–elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L{sup −1}, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64–22.9 μg Pb L{sup −1}). - Highlights: • Lead determination in urine using a solid phase extraction procedure followed by ETAAS • Carbon nanotubes as SPE adsorbent for Pb in urine • Matrix elimination for the Pb determination in urine by using SPE based on carbon nanotubes • The detection limit was 0.08 μg Pb L{sup −1}.

  11. Multi-walled carbon nanotube modified dummy-template magnetic molecularly imprinted microspheres as solid-phase extraction material for the determination of polychlorinated biphenyls in fish.

    Du, Xiaowen; Lin, Saichai; Gan, Ning; Chen, Xidong; Cao, Yuting; Li, Tianhua; Zhan, Pan


    Novel multi-walled carbon nanotube modified dummy-template molecularly imprinted microspheres (MWCNTs@DMMIPs) were successfully synthesized as adsorbents for six kinds of polychlorinated biphenyls (PCBs). MWCNTs@DMMIPs were prepared by a surface molecular imprinting technique. Core-shell Fe3 O4 @SiO2 nanoparticles were employed as magnetic support. 3,4-Dichlorobenzene acetic acid was used as a dummy template instead of PCBs, methacrylic acid was used as functional monomer and ethylene glycol dimethacrylate was used as the cross-linker. The resulting absorbent was characterized by various methods. The adsorbent was employed for extracting PCBs and exhibited good selectivity and high adsorption efficiency. Furthermore, it was reusable and capable of magnetic separation. Adsorption kinetics fit well with a pseudo-second-order kinetic equation and also exhibited a three-stage intra-particle diffusion model. The Freundlich model was used to describe the adsorption isotherms. The materials were successfully applied to the magnetic dispersive solid-phase extraction of six kinds of PCBs followed by gas chromatography with mass spectrometry determination in fish samples, the limit of detection of six kinds of PCBs were 0.0028-0.0068 μg/L and spiked recoveries ranged between 73.41 and 114.21%. The prepared adsorbent was expected to be a new material for the removal and recovery of PCBs from contaminated foods.

  12. A comparison of observables for solid-solid phase transitions

    Smilowitz, Laura B [Los Alamos National Laboratory; Henson, Bryan F [Los Alamos National Laboratory; Romero, Jerry J [Los Alamos National Laboratory


    The study of solid-solid phase transformations is hindered by the difficulty of finding a volumetric probe to use as a progress variable. Solids are typically optically opaque and heterogeneous. Over the past several years, second harmonic generation (SHG) has been used as a kinetic probe for a solid-solid phase transition in which the initial and final phases have different symmetries. Bulk generation of SHG is allowed by symmetry only in noncentrosymmetric crystallographic space groups. For the organic energetic nitramine octahydro-1,3 ,5,7 -tetranitro-1,3 ,5,7 -tatrazocine (HMX), the beta phase is centro symmetric (space group P2{sub 1}/c) and the delta phase iS noncentrosymmetric (space group P6{sub 1}22) making SHG an extremely sensitive, essentially zero background probe of the phase change progress. We have used SHG as a tool to follow the progress of the transformation from beta to delta phase during the solid-solid transformation. However, kinetic models of the transformation derived using different observables from several other groups have differed, showing later onset for the phase change and faster progression to completion. In this work, we have intercompared several techniques to understand these differences. The three techniques discussed are second harmonic generation, Raman spectroscopy, and differential scanning calorimetry (DSC). The progress of the beta to delta phase transition in HMX observed with each of these different probes will be discussed and advantages and disadvantages of each technique described. This paper compares several different observables for use in measuring the kinetics of solid-solid phase transitions. Relative advantages and disadvantages for each technique are described and a direct comparison of results is made for the beta to delta polymorphic phase transition of the energetic nitramine, octahydro-1,3,5,7-tetranitro-1,3,5,7-tatrazocine.

  13. Structural control of Fe-based alloys through diffusional solid/solid phase transformations in a high magnetic field.

    Ohtsuka, Hideyuki


    A magnetic field has a remarkable influence on solid/solid phase transformations and it can be used to control the structure and function of materials during phase transformations. The effects of magnetic fields on diffusional solid/solid phase transformations, mainly from austenite to ferrite, in Fe-based alloys are reviewed. The effects of magnetic fields on the transformation temperature and phase diagram are explained thermodynamically, and the transformation behavior and transformed structures in magnetic fields are discussed.

  14. Research on microcapsules of phase change materials

    DAI Xia; SHEN Xiaodong


    Microcapsule technology is a kind of technology wrapping the solid or liquid into minute-sized particles within the field of micrometer or millimeter with film forming materials. This thesis introduces microcapsule technology of phase change materials and its main functions and the structural composition, preparation methods and characterization technology of microcapsule of phase change materials. The microcapsule of phase change materials is small in size and its temperature remains unchanged during the process of heat absorption and heat release. It is of great value in research and application prospect due to these characteristics.

  15. Heat transfer in multi-phase materials

    Öchsner, Andreas


    This book provides a profound understanding, which physical processes and mechanisms cause the heat transfer in composite and cellular materials. It shows models for all important classes of composite materials and introduces into the latest advances. In three parts, the book covers Composite Materials (Part A), Porous and Cellular Materials (Part B) and the appearance of a conjoint solid phase and fluid aggregate (Part C).

  16. Analysis of solid-liquid phase change heat transfer enhancement

    张寅平; 王馨


    Solid-liquid phase change processes have two important features: the process is an approximately isothermal process and the heat of fusion of phase change material tends to be much greater than its specific heat. Therefore, if any phase change material adjacent to a hot or cold surface undergoes phase change, the heat transfer rate on the surface will be noticeably enhanced. This paper presents a novel insight into the mechanisms of heat transfer enhancement induced by solid-liquid phase change based on the analogy analysis for heat conduction with an internal heat source and solid-liquid phase change heat transfer. Three degrees of surface heat transfer enhancement for different conditions are explored, and corresponding formulae are written to describe them. The factors influencing the degrees of heat transfer enhancement are clarified and their effects quantitatively analyzed. Both the novel insight and the analysis contribute to effective application of phase change heat transfer enhancement technique.

  17. Behaviors of a MGPM/Opal Solid-Solid Phase-Change Storage Material%一种MGPM/Opal固-固相变储能材料的相变及结晶行为

    顾晓华; 西鹏; 段玉情; 高芬; 刘剑虹


    A solid-solid phase change energy storage composite material with polyethylene glycol single methyl ether(MPEG) chain structure,which chould be abbreviated as MGPM/opal,was synthesized by the way of monomer polycondensation with phase change.Wide-angle X-ray diffraction(WAXD),differential thermal scanning calorimeter(DSC) and hot stage polarizing microscope(POM),thermogravimetry(TG) and other testing methods were performed to investigate the crystal structure,crystallization behaviors,crystalline morphology and thermal stability of the composite materials.The results indicate that the addition of natural nano-phase materials opal improves the crystallization behavior and increases the crystallization speed of MPEG.When the mass fraction of opal is 0.7%,the crystallinity of the copolymer is the highest,when the phase change enthalpy comes to 109.07 kJ/g.Compared to the pure MPEG,the melting enthalpy and the crystallization enthalpy of the copolymer increase by 10.578 J/g and 8 J/g,respectively.The thermal stability of the copolymer is good,and it increases with the increase of opal.%采用含有相变单元的单体缩聚法合成了侧链含有聚乙二醇单甲醚(MPEG)的新型固-固相变储能复合材料(相变共聚物缩写名称为(MGPM)/蛋白石(opal)),通过广角X射线衍射(WAXD)、差热扫描量热仪(DSC)和热台偏光显微镜(POM)、热重(TG)等测试手段对其结晶结构、结晶行为、结晶形态和热稳定性进行了研究,结果表明,天然纳米材料蛋白石的加入改善了MPEG的结晶行为,提高了聚合物的结晶速率。蛋白石的添加量为0.7%时可以最大程度提高聚合物的结晶度,相变焓值最高达到109.07 kJ/g,比纯MPEG的熔融焓值提高了10.578 J/g,结晶焓值提高了8 J/g,热稳定性良好。

  18. Synthesis and Properties of Polymer Solid-Solid Phase Change Material Used for Fibers%一种纤维用高分子型固-固相变材料的合成及性能

    费鹏飞; 西鹏; 付鹏; 程博闻


    利用设计合成的八羟基化合物为支化单元,通过两步法合成出了一种相变储能材料.通过红外光谱(FT-IR)、偏光显微镜(POM)、X射线衍射(XRD)、差示扫描量热分析(DSC)对所制备的样品进行了测试表征.POM测试结果表明,所制备的相变材料的相变类型为固-固相变,具有与聚乙二醇(PEG)类似的球晶结构;DSC测试结果表明,该相变材料的相变焓值较高,吸放热焓值均达到了100J/g以上.而且由于八羟基化合物的特殊分子结构使得所制备的高分子相变材料的调温区间从PEG的65.90℃~34.20℃调整到55.20℃~25.10℃,更趋近相变纤维及其服饰面料的最佳使用温度区间.%In this paper,using the designed and synthesized eight hydroxyl compound as branched units,a phase change material was synthesized through the two-step method.The as-sample was characterized through FT-IR,POM,XRD,and DSC.The results of POM imply that the as-sample and polyethylene glycol (PEG) own similar micro-morphologies,their crystal structures are both spherulites.The results of DSC show that,this material has high phase transition enthalpy value,and its endothermic and exothermic enthalpy value both reach more than 100J/ g.Furthermore,owing to the special molecular structure of eight hydroxyl compound,the temperature adjusting zone of the polymer solid-solid phase change material is changed from 65.90 ℃ ~34.20 ℃ of PEG to 55.20 ℃ ~ 25.10 ℃,which is more close to the applied temperature of phase change energy storage fibers and its clothing fabrics.

  19. Effect of graphene layer thickness and mechanical compliance on interfacial heat flow and thermal conduction in solid-liquid phase change materials.

    Warzoha, Ronald J; Fleischer, Amy S


    Solid-liquid phase change materials (PCMs) are attractive candidates for thermal energy storage and electronics cooling applications but have limited applicability in state-of-the-art technologies due to their low intrinsic thermal conductivities. Recent efforts to incorporate graphene and multilayer graphene into PCMs have led to the development of thermal energy storage materials with remarkable values of bulk thermal conductivity. However, the full potential of graphene as a filler material for the thermal enhancement of PCMs remains unrealized, largely due to an incomplete understanding of the physical mechanisms that govern thermal transport within graphene-based nanocomposites. In this work, we show that the number of graphene layers (n) within an individual graphene nanoparticle has a significant effect on the bulk thermal conductivity of an organic PCM. Results indicate that the bulk thermal conductivity of PCMs can be tuned by over an order of magnitude simply by adjusting the number of graphene layers (n) from n = 3 to 44. Using scanning electron microscopy in tandem with nanoscale analytical techniques, the physical mechanisms that govern heat flow within a graphene nanocomposite PCM are found to be nearly independent of the intrinsic thermal conductivity of the graphene nanoparticle itself and are instead found to be dependent on the mechanical compliance of the graphene nanoparticles. These findings are critical for the design and development of PCMs that are capable of cooling next-generation electronics and storing heat effectively in medium-to-large-scale energy systems, including solar-thermal power plants and building heating and cooling systems.

  20. A new graphene oxide/polypyrrole foam material with pipette-tip solid-phase extraction for determination of three auxins in papaya juice.

    Wang, Lihui; Wang, Mingyu; Yan, Hongyuan; Yuan, Yanan; Tian, Jing


    A new material, graphene oxide/polypyrrole (GO/Ppy), was synthesized by mixing graphene oxide and polypyrrole in a specific proportion. It possesses a unique structure similar to that of foam. A homemade pipette-tip solid-phase extraction (PT-SPE) device, which is more simple and convenient than traditional devices, was used for saving reagents and operation time. When GO/Ppy was used as the adsorbent of PT-SPE for determining three auxins (indole-3-propionic acid, indole-3-butyric acid, and 1-naphthaleneacetic acid) present in trace amounts in papaya juice, it showed high affinity and adsorption capacity for all the three auxins. GO/Ppy-PT-SPE also had a significant capacity for eliminating the interferences from the papaya juice matrix. Under optimized conditions, a good linearity of auxins was obtained in the range 16.3-812.5 ng g(-1); the average recoveries at the three spiked levels of the three auxins ranged from 89.4% to 105.6% with the relative standard deviations ≤ 3.0%. Meanwhile, six papaya juice samples with different growth stages were analyzed under optimum conditions, and trace auxins in the range 18.3-100.6 ng g(-1) were observed. Because of its high selectivity, simplicity, and reliability, the GO/Ppy-PT-SPE method developed herein can be potentially applied for determining trace auxins in complex biological samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

    Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero


    The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption-elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L- 1, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64-22.9 μg Pb L- 1).

  2. Electrospun nanostructured polystyrene as a new coating material for solid-phase microextraction: Application to separation of multipesticides from honey samples.

    Zali, Sara; Jalali, Fahimeh; Es-Haghi, Ali; Shamsipur, Mojtaba


    For the first time, electrospun polystyrene nanostructure was used as coating material on a stainless steel wire for solid-phase microextraction. Surface morphology of the coating was studied by scanning electron microscopy which showed the formation of nanofibers on the wire. The coating was stable after conditioning at 250°C for 2h. The efficiency of the polystyrene coating was approved by extracting a mixture of seven pesticides (polar and apolar) from head space of honey samples followed by gas chromatography-mass spectrometry. The important parameters affecting extraction efficiency such as, extraction time and temperature, desorption conditions, agitation rate and ionic strength were investigated. Under optimized experimental conditions, detection limits for the investigated pesticides ranged from 0.1-2μgL(-1). The intra- and inter-day precisions of the developed method were 3.5-17.6% and 10.0-25.0%, respectively. Finally, all the investigated pesticides were spiked to honey samples and extracted by the proposed method. The accuracies of determination of all the species were found to be in the range of 81-125%.

  3. Application of solid phase extraction with the use of silica modified with polyaniline film for pretreatment of samples from plant material before HPLC determination of triterpenic acids.

    Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Rokicka, Kamila; Kocjan, Ryszard; Szymczak, Grażyna


    The new sorbent based on silica gel coated with a film of polyaniline (Si-PANI) was obtained in a process of in situ polymerization directly on carrier particles and its potential application for pretreatment of plant material samples with the use of solid phase extraction (SPE) was investigated. Parameters such as cartridge conditioning, the volume and concentration of the sample, the type and volume of the elution solvent were optimized and compared with parameters obtained for RP-18 and aminopropyl silica cartridges. The high recovery values above 97% after the SPE procedure with the use of Si-PANI cartridges proves their utility for analysis of triterpenic acids. The sorbent tested was successfully used for clean-up of extracts from Salvia officinalis L., Syzygium aromaticum (L.) Merrill., and Origanum vulgare L. prior to HPLC-DAD determination of oleanolic, ursolic and betulinic acid. The efficiency of sample purification was verified by monitoring of chromatograms in the region between 190 nm and 400 nm during the gradient elution. The fewest components or their lowest concentrations were observed for all the investigated samples after the SPE procedures.

  4. Ampholine-functionalized hybrid organic-inorganic silica material as sorbent for solid-phase extraction of acidic and basic compounds.

    Wang, Tingting; Chen, Yihui; Ma, Junfeng; Chen, Mingliang; Nie, Chenggang; Hu, Minjie; Li, Ying; Jia, Zhijian; Fang, Jianghua; Gao, Haoqi


    A novel sorbent for solid-phase extraction (SPE) was synthesized by chemical immobilization of ampholine on hybrid organic-inorganic silica material. The ampholine-functionalized hybrid organic-inorganic silica sorbent is consisted of aliphatic amine groups, carboxyl groups and long carbon chains, allowing for extraction of both acidic and basic compounds. The retention properties of the developed sorbent were evaluated for 1-hydroxy-2-naphthoic acid (HNA), 1-naphthoic acid (NA), 3-hydroxybenzoic acid (HBA), benzoic acid (BA), sorbic acid (SA), vanillic aldehyde (VA), butyl 4-hydroxybenzoate (BHB), propyl 4-hydroxybenzoate (PHB), ethyl 4-hydroxybenzoate (EHB), and methyl 4-hydroxybenzoate (MHB). The results show that such a sorbent has three types of interaction, i.e., electrostatic interaction, hydrophobic interaction, and hydrogen bonding, exhibiting high extraction efficiency towards the compounds tested. The adsorption capacities of the analytes ranged from 0.61 to 6.54μgmg(-1). The reproducibility of the sorbent preparation was evaluated at three spiking concentration levels, with relative standard deviations (RSDs) of 1.0-10.5%. The recoveries of ten acidic and basic compounds spiked in beverage Coca-Cola(®) sample ranged from 82.5% to 98.2% with RSDs less than 5.8%. Under optimum conditions, the ampholine-functionalized hybrid organic-inorganic silica sorbent rendered higher extraction efficiency for acidic compounds than that of the commercially available ampholine-functionalized silica particles, and was comparable to that of the commercial Oasis WAX and Oasis WCX.

  5. Nuclear Concrete Materials Database Phase I Development

    Ren, Weiju [ORNL; Naus, Dan J [ORNL


    The FY 2011 accomplishments in Phase I development of the Nuclear Concrete Materials Database to support the Light Water Reactor Sustainability Program are summarized. The database has been developed using the ORNL materials database infrastructure established for the Gen IV Materials Handbook to achieve cost reduction and development efficiency. In this Phase I development, the database has been successfully designed and constructed to manage documents in the Portable Document Format generated from the Structural Materials Handbook that contains nuclear concrete materials data and related information. The completion of the Phase I database has established a solid foundation for Phase II development, in which a digital database will be designed and constructed to manage nuclear concrete materials data in various digitized formats to facilitate electronic and mathematical processing for analysis, modeling, and design applications.

  6. Solid-solid phase transitions via melting in metals

    Pogatscher, S.; Leutenegger, D.; Schawe, J. E. K.; Uggowitzer, P. J.; Löffler, J. F.


    Observing solid-solid phase transitions in-situ with sufficient temporal and spatial resolution is a great challenge, and is often only possible via computer simulations or in model systems. Recently, a study of polymeric colloidal particles, where the particles mimic atoms, revealed an intermediate liquid state in the transition from one solid to another. While not yet observed there, this finding suggests that such phenomena may also occur in metals and alloys. Here we present experimental evidence for a solid-solid transition via the formation of a metastable liquid in a `real' atomic system. We observe this transition in a bulk glass-forming metallic system in-situ using fast differential scanning calorimetry. We investigate the corresponding transformation kinetics and discuss the underlying thermodynamics. The mechanism is likely to be a feature of many metallic glasses and metals in general, and may provide further insight into phase transition theory.

  7. Solid electrolytes general principles, characterization, materials, applications

    Hagenmuller, Paul


    Solid Electrolytes: General Principles, Characterization, Materials, Applications presents specific theories and experimental methods in the field of superionic conductors. It discusses that high ionic conductivity in solids requires specific structural and energetic conditions. It addresses the problems involved in the study and use of solid electrolytes. Some of the topics covered in the book are the introduction to the theory of solid electrolytes; macroscopic evidence for liquid nature; structural models; kinetic models; crystal structures and fast ionic conduction; interstitial motion in

  8. A porous carbon derived from amino-functionalized material of Institut Lavoisier as a solid-phase microextraction fiber coating for the extraction of phthalate esters from tea.

    Liang, Weiqian; Wang, Juntao; Zang, Xiaohuan; Wang, Chun; Wang, Zhi


    In this work, a porous carbon derived from amino-functionalized material of Institut Lavoisier (C-NH2 -MIL-125) was prepared and coated onto a stainless-steel wire through sol-gel technique. The coated fiber was used for the solid-phase microextraction of trace levels of phthalate esters (diallyl phthalate, di-iso-butyl ortho-phthalate, di-n-butyl ortho-phthalate, benzyl-n-butyl ortho-phthalate, and bis(2-ethylhexy) ortho-phthalate) from tea beverage samples before gas chromatography with mass spectrometric analysis. Several experimental parameters that could influence the extraction efficiency such as extraction time, extraction temperature, sample pH, sample salinity, stirring rate, desorption temperature and desorption time, were investigated. Under the optimal conditions, the linearity existed in the range of 0.05-30.00 μg/L for green jasmine tea beverage samples, and 0.10-30.00 μg/L for honey jasmine tea beverage samples, with the correlation coefficients (r) ranging from 0.9939 to 0.9981. The limits of detection of the analytes for the method were 2.0-3.0 ng/L for green jasmine tea beverage sample, and 4.0-5.0 ng/L for honey jasmine tea beverage sample, depending on the compounds. The recoveries of the analytes for the spiked samples were in the range of 82.0-106.0%, and the precision, expressed as the relative standard deviations, was less than 11.1%.

  9. Solid phase microextraction device using aerogel

    Miller, Fred S.; Andresen, Brian D.


    A sample collection substrate of aerogel and/or xerogel materials bound to a support structure is used as a solid phase microextraction (SPME) device. The xerogels and aerogels may be organic or inorganic and doped with metals or other compounds to target specific chemical analytes. The support structure is typically formed of a glass fiber or a metal wire (stainless steel or kovar). The devices are made by applying gel solution to the support structures and drying the solution to form aerogel or xerogel. Aerogel particles may be attached to the wet layer before drying to increase sample collection surface area. These devices are robust, stable in fields of high radiation, and highly effective at collecting gas and liquid samples while maintaining superior mechanical and thermal stability during routine use. Aerogel SPME devices are advantageous for use in GC/MS analyses due to their lack of interfering background and tolerance of GC thermal cycling.

  10. Sulfur Release from Cement Raw Materials during Solid Fuel Combustion

    Nielsen, Anders Rooma; Larsen, Morten B.; Glarborg, Peter


    During combustion of solid fuels in the material inlet end of cement rotary kilns, local reducing conditions can occur and cause decomposition of sulfates from cement raw materials. Decomposition of sulfates is problematic because it increases the gas-phase SO2 concentration, which may cause...... deposit formation in the kiln system. SO2 release from cement raw materials during combustion of solid fuels has been studied experimentally in a high temperature rotary drum. The fuels were tire rubber, pine wood, petcoke, sewage sludge, and polypropylene. The SO2 release from the raw materials...

  11. Molecular Modeling of Solid Fluid Phase Behavior

    Peter A. Monson


    This report gives a summary of the achievements under DOE contract No. DOE/ER/14150 during the period September 1, 1990 to December 31, 2007. This project was concerned with the molecular modeling of solid-fluid equilibrium. The focus was on understanding how solid-fluid and solid-solid phase behavior are related to molecular structure, and the research program made a seminal contribution in this area. The project led to 34 journal articles, including a comprehensive review article published in Advances in Chemical Physics. The DOE funding supported the work of 5 Ph.D. students, 2 M.S. students and 5 postdoctoral researchers.

  12. Binary Solid-Liquid Phase Equilibria

    Ellison, Herbert R.


    Indicates some of the information that may be obtained from a binary solid-liquid phase equilibria experiment and a method to write a computer program that will plot an ideal phase diagram to which the experimental results may be compared. (Author/CP)

  13. Nanoscale phase change memory materials.

    Caldwell, Marissa A; Jeyasingh, Rakesh Gnana David; Wong, H-S Philip; Milliron, Delia J


    Phase change memory materials store information through their reversible transitions between crystalline and amorphous states. For typical metal chalcogenide compounds, their phase transition properties directly impact critical memory characteristics and the manipulation of these is a major focus in the field. Here, we discuss recent work that explores the tuning of such properties by scaling the materials to nanoscale dimensions, including fabrication and synthetic strategies used to produce nanoscale phase change memory materials. The trends that emerge are relevant to understanding how such memory technologies will function as they scale to ever smaller dimensions and also suggest new approaches to designing materials for phase change applications. Finally, the challenges and opportunities raised by integrating nanoscale phase change materials into switching devices are discussed.

  14. Solid phase sequencing of biopolymers

    Cantor, Charles R.; Hubert, Koster


    This invention relates to methods for detecting and sequencing target nucleic acid sequences, to mass modified nucleic acid probes and arrays of probes useful in these methods, and to kits and systems which contain these probes. Useful methods involve hybridizing the nucleic acids or nucleic acids which represent complementary or homologous sequences of the target to an array of nucleic acid probes. These probes comprise a single-stranded portion, an optional double-stranded portion and a variable sequence within the single-stranded portion. The molecular weights of the hybridized nucleic acids of the set can be determined by mass spectroscopy, and the sequence of the target determined from the molecular weights of the fragments. Probes may be affixed to a solid support such as a hybridization chip to facilitate automated molecular weight analysis and identification of the target sequence.

  15. Solid phase sequencing of biopolymers

    Cantor, Charles (Del Mar, CA); Koster, Hubert (La Jolla, CA)


    This invention relates to methods for detecting and sequencing target nucleic acid sequences, to mass modified nucleic acid probes and arrays of probes useful in these methods, and to kits and systems which contain these probes. Useful methods involve hybridizing the nucleic acids or nucleic acids which represent complementary or homologous sequences of the target to an array of nucleic acid probes. These probes comprise a single-stranded portion, an optional double-stranded portion and a variable sequence within the single-stranded portion. The molecular weights of the hybridized nucleic acids of the set can be determined by mass spectroscopy, and the sequence of the target determined from the molecular weights of the fragments. Nucleic acids whose sequences can be determined include DNA or RNA in biological samples such as patient biopsies and environmental samples. Probes may be fixed to a solid support such as a hybridization chip to facilitate automated molecular weight analysis and identification of the target sequence.

  16. Heterogeneous Ferroelectric Solid Solutions Phases and Domain States

    Topolov, Vitaly


    The book deals with perovskite-type ferroelectric solid solutions for modern materials science and applications, solving problems of complicated heterophase/domain structures near the morphotropic phase boundary and applications to various systems with morphotropic phases. In this book domain state–interface diagrams are presented for the interpretation of heterophase states in perovskite-type ferroelectric solid solutions. It allows to describe the stress relief in the presence of polydomain phases, the behavior of unit-cell parameters of coexisting phases and the effect of external electric fields. The novelty of the book consists in (i) the first systematization of data about heterophase states and their evolution in ferroelectric solid solutions (ii) the general interpretation of heterophase and domain structures at changing temperature, composition or electric field (iii) the complete analysis of interconnection domain structures, unit-cell parameters changes, heterophase structures and stress relief.

  17. Preparation and evaluation of a molecularly imprinted sol-gel material as the solid-phase extraction adsorbents for the specific recognition of cloxacilloic acid in cloxacillin.

    Du, Kangli; Luo, Zhimin; Guo, Pengqi; Tang, Weili; Wu, Ningli; Zheng, Penglei; Du, Wei; Zeng, Aiguo; Jing, Wanghui; Chang, Chun; Fu, Qiang


    Highly selective molecularly imprinted polymers on the surface of silica gels were prepared by a sol-gel process and used as solid-phase extraction adsorbents for the specific recognition, enrichment and detection of cloxacilloic acid in cloxacillin. The obtained polymers were characterized by scanning electron microscopy, FTIR spectroscopy, nitrogen adsorption and desorption, elemental analysis and thermogravimetric analysis. The imprinted polymers not only possessed high adsorption capacity (6.5 μg/mg), but also exhibited fast adsorption kinetics (they adsorb 80% of the maximum amount within 20 min) and excellent selectivity (the imprinted factor was 3.6). A method using the imprinted polymers as solid-phase extraction adsorbents coupled with high-performance liquid chromatography was established with good specificity, linearity (r = 0.9962), precision (ranging from 0.5 to 6.7%), accuracy (ranging from 93.9 to 97.7%) and extraction recoveries (ranging from 78.8 to 89.8%). The limits of detection and quantification were 0.07 and 0.25 mg/g, respectively. This work could provide a promising method in the enrichment, extraction and detection of allergenic impurities in the manufacture, storage and application of cloxacillin.

  18. Inorganic-organic hybrid coating material for the online in-tube solid-phase microextraction of monohydroxy polycyclic aromatic hydrocarbons in urine.

    Wang, ShuLing; Xu, Hui


    An inorganic-organic hybrid nanocomposite (zinc oxide/polypyrrole) that represents a novel kind of coating for in-tube solid-phase microextraction is reported. The composite coating was prepared by a facile electrochemical polymerization strategy on the inner surface of a stainless-steel tube. Based on the coated tube, a novel online in-tube solid-phase microextraction with liquid chromatography and mass spectrometry method was developed and applied for the extraction of three monohydroxy polycyclic aromatic hydrocarbons in human urine. The coating displayed good extraction ability toward monohydroxy polycyclic aromatic hydrocarbons. In addition, long lifespan, excellent stability, and good compression resistance were also obtained for the coating. The experimental conditions affecting the extraction were optimized systematically. Under the optimal conditions, the limits of detection and quantification were in the range of 0.039-0.050 and 0.130-0.167 ng/mL, respectively. Good linearity (0.2-100 ng/mL) was obtained with correlation coefficients larger than 0.9967. The repeatability, expressed as relative standard deviation, ranged between 2.5% and 9.4%. The method offered the advantage of process simplicity, rapidity, automation, and sensitivity in the analysis of human urinary monohydroxy polycyclic aromatic hydrocarbons in two different cities of Hubei province. An acceptable recovery of monohydroxy polycyclic aromatic hydrocarbons (64-122%) represented the additional attractive features of the method in real urine analysis.

  19. Measurements of solids concentration and axial solids velocity in gas-solid two-phase flows.

    Nieuwland, J.J.; Meijer, R.; Kuipers, J.A.M.; Swaaij, van W.P.M.


    Several techniques reported in the literature for measuring solids concentration and solids velocity in (dense) gas-solid two-phase flow have been briefly reviewed. An optical measuring system, based on detection of light reflected by the suspended particles, has been developed to measure local soli

  20. Obtaining cementitious material from municipal solid waste

    Macías, A.


    Full Text Available The primary purpose of the present study was to determine the viability of using incinerator ash and slag from municipal solid waste as a secondary source of cementitious materials. The combustion products used were taken from two types of Spanish MSW incinerators, one located at Valdemingómez, in Madrid, and the other in Melilla, with different incineration systems: one with fluidised bed combustion and other with mass burn waterwall. The effect of temperature (from 800 to 1,200 ºC on washed and unwashed incinerator residue was studied, in particular with regard to phase formation in washed products with a high NaCl and KCl content. The solid phases obtained were characterized by X-ray diffraction and BET-N2 specific surface procedures.El principal objetivo del trabajo ha sido determinar la viabilidad del uso de las cenizas y escorias procedentes de la incineración de residuos sólidos urbanos, como materia prima secundaria para la obtención de fases cementantes. Para ello se han empleado los residuos generados en dos tipos de incineradoras españolas de residuos sólidos urbanos: la incineradora de Valdemingómez y la incineradora de Melilla. Se ha estudiado la transformación de los residuos, sin tratamiento previo, en función de la temperatura de calentamiento (desde 800 ºC hasta 1.200 ºC, así como la influencia del lavado de los residuos con alto contenido en NaCl y KCl en la formación de fases obtenidas a las diferentes temperaturas de calcinación. Las fases obtenidas fueron caracterizadas por difracción de rayos X y área superficial por el método BET-N2.

  1. Transitional Phenomena on Phase Change Materials

    Wójcik Tadeusz M.


    Full Text Available One of the most significant problem with technology development is transferring of large heat fluxes, which requires constant heat transfer temperature (in the specified temperature range. This problem concern mainly the nuclear energetics, space technologies, military technologies and most of all electronics containing integrated circuits with very large scale of integrations. Intensive heat transfer and thermal energy storage are possible by the use of phase change materials (PCMs. In the paper there are presented preliminary results of research on the use of liquid-gas (L-G PCMs and solid-solid phase change materials (S-S PCMs. For L-G PCMs the boiling characteristics were determined by increasing and decreasing the heat flux, which for certain sets of structural parameters of the heating surface and the physical properties of the liquid induce a variety of forms of transitional phenomena. Thermal energy storage is much more effective when using PCMs than sensible heat.

  2. Solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the direct determination of Hg in different materials using isotope dilution with a gaseous phase for calibration

    Resano, M.; Gelaude, I.; Dams, R.; Vanhaecke, F.


    This paper evaluates the potential of electrothermal vaporization-inductively coupled plasma mass spectrometry (ETV-ICPMS) for the direct determination of Hg in solid samples, using a 200Hg-enriched gaseous phase for calibration based on isotope dilution. Three different samples were studied, BCR CRM 320 River sediment, IAEA-086 Hair and a real (wet) freshwater fish sample (M1). The samples selected show important differences in their matrix composition, and especially the fish sample constitutes a challenge as a result of its high water content (≈80%). The main conclusion of the work is that the calibration approach investigated succesfully corrects for all the matrix effects (suppression) observed during Hg vaporization, allowing accurate values to be obtained in all cases. Moreover, practically the same operating conditions could be used for all sample types. The method finally proposed presents interesting features for the direct determination of this challenging element in solid samples, such as: a low sample consumption (a few milligrams), a high sample throughput (10 min/sample), a low limit of detection (6 ng g -1) and a reduced risk of analyte losses or contamination. Precision values depend on the homogeneity of the sample studied, and are typically in the vicinity of 10% RSD, except for the more inhomogenous river sediment (18% RSD).

  3. Multiplexed Colorimetric Solid-Phase Extraction

    Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.


    Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

  4. Synthesis of nano B{sub 2}O{sub 3}/TiO{sub 2} composite material as a new solid phase extractor and its application to preconcentration and separation of cadmium

    Kalfa, Orhan Murat; Yalcinkaya, Ozcan [Gazi University, Science and Art Faculty, Department of Chemistry, 06500, Ankara (Turkey); Tuerker, Ali Rehber, E-mail: [Gazi University, Science and Art Faculty, Department of Chemistry, 06500, Ankara (Turkey)


    A new solid phase extractor, nano-scale diboron trioxide/titanium dioxide composite material, was synthesized and used for separation and/or preconcentration of trace cadmium ion from various samples. The characterization of the synthesized material was performed by scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray diffractometer methods (XRD). The specific surface area of the material was also determined and found as 3.4 m{sup 2}/g. Analytical parameters including pH of sample solution, sample volume, flow rate of sample solution, volume and concentration of eluent for the column solid phase extraction (SPE) procedure were examined. The effect of common matrix ions on the recovery of the cadmium has also been investigated and found that they did not interfere on cadmium preconcentration. Under the optimum experimental conditions, preconcentration factor and analytical detection limit were determined as 50 and 1.44 {mu}g/L, respectively. The reusability (stabile up to 100 run) and adsorption capacity (49 mg/g) of the sorbent were excellent. The accuracy of the method was confirmed by analyzing certified reference materials (Tea leaves GBW-07605). The results demonstrated good agreement with the certified values (relative error <10%). The precision of the method was also satisfactory. The recovery of cadmium under the optimum conditions was found to be 96 {+-} 3% at 95% confidence level. The method was applied for the determination of cadmium in tap water and tea leaves.

  5. Phase 2, Solid waste retrieval strategy

    Johnson, D.M.


    Solid TRU retrieval, Phase 1 is scheduled to commence operation in 1998 at 218W-4C-T01 and complete recovery of the waste containers in 2001. Phase 2 Retrieval will recover the remaining buried TRU waste to be retrieved and provide the preliminary characterization by non-destructive means to allow interim storage until processing for disposal. This document reports on researching the characterization documents to determine the types of wastes to be retrieved and where located, waste configurations, conditions, and required methods for retrieval. Also included are discussions of wastes encompassed by Phase 2 for which there are valid reasons to not retrieve.

  6. Nanophase materials in solid freeform fabrication

    Manthiram, A.; Bourell, D. L.; Marcus, H. L.


    Solid freeform fabrication (SFF) is a manufacturing technology that produces parts directly from computer-aided design databases. Examples of the SFF approach are selective laser sintering (SLS) and selective laser reactive sintering (SLRS), both of which have the potential to directly produce structurally sound metallic or ceramic parts. The development of suitable materials systems that can optimize the SLS or SLRS processes are critical to this technology. For instance, nanocomposites, in which the constituents are mixed on a nanometer scale, have the potential to provide important advantages in the SLS and SLRS processes. One strategy is to design and develop nanocomposites in which one nanosize component has a lower melting point than the other nanosize component, either of which can serve as the matrix phase. The nanoscale dispersion of the low-melting component can aid the sintering process during SLS or SLRS. In this article, the philosophical basis for SLS and SLRS of nanocomposites is discussed. Conceptual design of nanocomposite systems and the SLS/SLRS results of a few exploratory systems are presented.

  7. Megabar pressure phases of solid hydrogen

    Chen, Nancy Hueling

    The behavior of solid Hsb2, Dsb2, and HD at low temperatures high pressures was investigated. The experimental data were obtained by combining high pressure diamond anvil cell apparatus with cryogenic and spectroscopic techniques. Megabar pressures (1 bar = 10sp5 Pa) and liquid helium temperatures were accessible. The observed phases and phase lines are discussed with respect to orientational order, crystal structure, and electronic properties. The orientational order-disorder phase transition in HD was studied by Raman spectroscopy. Due to the distinguishability of the nuclei in an HD molecule, the observed phase line exhibits surprising behavior relative to that expected for the homonuclear molecules Hsb2 and Dsb2. The megabar pressure phase diagram of solid Dsb2 was investigated by infrared and Raman spectroscopy. The broken symmetry phase (BSP) transition line and the D-A phase line were observed to meet at a triple point. The relative arrangement of phase lines in P-T space, combined with group theoretical analysis of observed infrared and Raman spectra within the phases, sets symmetry restrictions on the allowed crystal structures. The electronic properties of the high pressure H-A and D-A phases were examined, since these recently discovered phases were suspected of being metallic. Acquired broadband infrared absorption spectra extending to 10 mum were analyzed in terms of the Drude model for metals. No evidence indicating metallic behavior was found. Refinements in high pressure techniques were explored, in order to increase the maximum pressures attainable. A method of extending ruby fluorescence pressure measurements to multimegabar pressures was developed, which involved excitation of ruby fluorescence with red, rather than blue or green laser light.


    Dmitrenko D. V.


    Full Text Available The article is dedicated to the determination of conditions for solid bodies’ fragmentation, providing minimal size of particles by means of their mechanical dispersion through the example of powders of titanium carbide (TiC, cubic boron nitride – borazon (CBN and boron carbide (B4C. The theoretical and practical aspects of the process of mechanical fragmentation of particles of solid powder materials in ball mill for their further utilization in furnace charge for high-speed gas-flame sputtering of wear-resistant composite materials are examined in the article. Methods of preliminary calculation of minimum allowable size of solid particles of powder materials during mechanical fragmentation, based upon Griffiths’ mechanical theory of rapture using experimental data for hardness of material and its yield are proposed and theoretically substantiated. There we have the results of experiments on mechanical fragmentation of titanium carbide in attritor, boron carbide and cubic boron nitride in centrifugal planetary mill, confirming correctness of theoretical propositions and calculations are set out. Recommendations on mechanical fragmentation of solid powder materials in ball mills are formulated as well

  9. Stability of solid oxide fuel cell materials

    Armstrong, T.R.; Bates, J.L.; Coffey, G.W.; Pederson, L.R. [Pacific Northwest National Lab., Richland, WA (United States)] [and others


    Chromite interconnection materials in an SOFC are exposed to both highly oxidizing conditions at the cathode and to highly reducing conditions at the anode. Because such conditions could lead to component failure, the authors have evaluated thermal, electrical, chemical, and structural stabilities of these materials as a function of temperature and oxygen partial pressure. The crystal lattice of the chromites was shown to expand for oxygen partial pressures smaller than 10{sup {minus}10} atm, which could lead to cracking and debonding in an SOFC. Highly substituted lanthanum chromite compositions were the most susceptible to lattice expansion; yttrium chromites showed better dimensional stability by more than a factor of two. New chromite compositions were developed that showed little tendency for lattice expansion under strongly reducing conditions, yet provided a good thermal expansion match to other fuel cell components. Use of these new chromite interconnect compositions should improve long-term SOFC performance, particularly for planar cell configurations. Thermodynamic properties of substituted lanthanum manganite cathode compositions have been determined through measurement of electromotive force as a function of temperature. Critical oxygen decomposition pressures for Sr and Ca-substituted lanthanum manganites were established using cells based on a zirconia electrolyte. Strontium oxide and calcium oxide activities in a lanthanum manganite matrix were determined using cells based on strontium fluoride and calcium fluoride electrolytes, respectively. The compositional range of single-phase behavior of these ABO{sub 3}-type perovskites was established as a function of A/B cation ratios and the extent of acceptor doping. Before this work, very little thermodynamic information was in existence for substituted manganite compositions. Such information is needed to predict the long-term stability of solid oxide fuel cell assemblies.

  10. Cyclodextrin polymer/Fe3O4 nanocomposites as solid phase extraction material coupled with UV-vis spectrometry for the analysis of rutin.

    Gong, Aiqin; Ping, Wenhui; Wang, Jue; Zhu, Xiashi


    In this paper, carboxymethyl-hydroxypropyl-β-cyclodextrin polymer modified magnetic particles Fe3O4 (CM-HP-β-CDCP-MNPs) were prepared and applied to magnetic solid phase extraction of rutin combined with UV-visible spectrometry detection. The synthesized magnetic particles were characterized by element analysis, Fourier transform infrared spectra, thermal gravimetric analysis, and transmission electron microscopy. Several variables affecting the extraction and desorption of rutin such as pH, the amount of adsorbent, the type and volume of eluent, extraction and desorption time, and temperature were investigated. The maximum adsorption capacity was 67.0 mg g(-1) for rutin with the equilibrium time of 30 min at room temperature, and the adsorbent could be reused for 10 times. A calibration curve was linear in the range of 0.05-8.00 μg mL(-1) with a relative standard deviation of 2.9% (n=5, c=4.0 μg mL(-1)). The limit of detection was 7.0 ng mL(-1). The interaction mechanism between the adsorbent and rutin was also studied. Feasibility of this method was validated by the analysis of rutin tablets and lotus plumule. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Comparison of Three Solid Phase Materials for the Extraction of Carboxylic Acids from River Water Followed by 2D GC × GC-TOFMS Determination.

    Bosire, G O; Ngila, J C; Parshotam, H


    The extraction and determination of aliphatic and aromatic carboxylic acids as well as their influence on the aromaticity and molecularity relationship of natural organic matter (NOM) in water are reported in this study. Three solid phase extraction (SPE) sorbents were used and their extraction efficiencies evaluated after chromatographic determinations (using gas chromatography with a time of flight mass spectrometer (GC × GC-TOFMS) and liquid chromatography with organic carbon detector (LC-OCD)). More than 42 carboxylic acids were identified in raw water from the Vaal River, which feeds the Lethabo Power Generation Station, South Africa, with cooling water. The aromatic carboxylic acid efficiency (28%) was achieved by using Strata™ X SPE while the highest aliphatic carboxylic acid efficiency (92.08%) was achieved by silica SPE. The hydrophobic nature of NOM in water depends on the nature of organic compounds in water, whether aromatic or aliphatic. The LC-OCD was used to assess the hydrophobicity levels of NOM as a function of these carboxylic acids in cooling water. The LC-OCD results showed that the aromatic nature of NOM in SPE filtered water followed the order Silica>Strata X>C-18. From the results, the hydrophobicity degree of the samples depended on the type and number of carboxylic acids that were removed by the SPE cartridges.

  12. Cyclodextrin polymer/Fe3O4 nanocomposites as solid phase extraction material coupled with UV-vis spectrometry for the analysis of rutin

    Gong, Aiqin; Ping, Wenhui; Wang, Jue; Zhu, Xiashi


    In this paper, carboxymethyl-hydroxypropyl-β-cyclodextrin polymer modified magnetic particles Fe3O4 (CM-HP-β-CDCP-MNPs) were prepared and applied to magnetic solid phase extraction of rutin combined with UV-visible spectrometry detection. The synthesized magnetic particles were characterized by element analysis, Fourier transform infrared spectra, thermal gravimetric analysis, and transmission electron microscopy. Several variables affecting the extraction and desorption of rutin such as pH, the amount of adsorbent, the type and volume of eluent, extraction and desorption time, and temperature were investigated. The maximum adsorption capacity was 67.0 mg g-1 for rutin with the equilibrium time of 30 min at room temperature, and the adsorbent could be reused for 10 times. A calibration curve was linear in the range of 0.05-8.00 μg mL-1 with a relative standard deviation of 2.9% (n = 5, c = 4.0 μg mL-1). The limit of detection was 7.0 ng mL-1. The interaction mechanism between the adsorbent and rutin was also studied. Feasibility of this method was validated by the analysis of rutin tablets and lotus plumule.

  13. Modeling the Capillary Pressure for the Migration of the Liquid Phase in Granular Solid-Liquid-Vapor Systems: Application to the Control of the Composition Profile in W-Cu FGM Materials

    Missiaen, Jean-Michel; Raharijaona, Jean-Joël; Delannay, Francis


    A model is developed to compute the capillary pressure for the migration of the liquid phase out or into a uniform solid-liquid-vapor system. The capillary pressure is defined as the reduction of the overall interface energy per volume increment of the transferred fluid phase. The model takes into account the particle size of the solid particle aggregate, the packing configuration (coordination number, porosity), the volume fractions of the different phases, and the values of the interface energies in the system. The model is used for analyzing the stability of the composition profile during processing of W-Cu functionally graded materials combining a composition gradient with a particle size gradient. The migration pressure is computed with the model in two stages: (1) just after the melting of copper, i.e., when sintering and shape accommodation of the W particle aggregate can still be neglected and (2) at high temperature, when the system is close to full density with equilibrium particle shape. The model predicts well the different stages of liquid-phase migration observed experimentally.

  14. All solid-state SBS phase conjugate mirror

    Dane, C.B.; Hackel, L.A.


    A stimulated Brillouin scattering (SBS) phase conjugate laser mirror uses a solid-state nonlinear gain medium instead of the conventional liquid or high pressure gas medium. The concept has been effectively demonstrated using common optical-grade fused silica. An energy threshold of 2.5 mJ and a slope efficiency of over 90% were achieved, resulting in an overall energy reflectivity of >80% for 15 ns, 1 um laser pulses. The use of solid-state materials is enabled by a multi-pass resonant architecture which suppresses transient fluctuations that would otherwise result in damage to the SBS medium. This all solid state phase conjugator is safer, more reliable, and more easily manufactured than prior art designs. It allows nonlinear wavefront correction to be implemented in industrial and defense laser systems whose operating environments would preclude the introduction of potentially hazardous liquids or high pressure gases. 8 figs.

  15. Stability of solid oxide fuel cell materials

    Armstrong, T.R.; Bates, J.L.; Chick, L.A. [Pacific Northwest Lab., Richland, WA (United States)


    Interconnection materials in a solid oxide fuel cell are exposed to both highly oxidizing conditions at the cathode and to highly reducing conditions at the anode. The thermal expansion characteristics of substituted lanthanum and yttrium chromite interconnect materials were evaluated by dilatometry as a function of oxygen partial pressures from 1 atm to 10{sup -18} atm, controlled using a carbon dioxide/hydrogen buffer.

  16. Solid phase synthesis of bifunctional antibodies.

    DeSilva, B S; Wilson, G S


    Bifunctional antibodies were prepared using the principle of solid-phase synthesis. The two Fab' fragments were chemically linked together via a bismaleimide crosslinking reagent. The F(ab')2 fragments from intact IgG were prepared using an immobilized pepsin column. Goat, mouse and human antibodies were digested completely within 4 h. The F(ab')2 fragments thus produced did not contain any IgG impurities. The Fab' fragments were produced by reducing the inter-heavy chain disulfide bonds using 2-mercaptoethylamine. The use of the solid-phase reactor in the preparation of the bifunctional antibodies eliminated many of the time-consuming separation steps between the fragmentation and conjugation steps. This procedure facilitates the automation of the bifunctional antibody preparation and the rapid optimization of reaction conditions.

  17. [Solid phase techniques in blood group serology].

    Uthemann, H; Sturmfels, L; Lenhard, V


    As alternatives to hemagglutination, solid-phase red blood cell adherence assays are of increasing importance. The adaptation of the new techniques to microplates offers several advantages over hemagglutination. Using microplates the assays may be processed semiautomatically, and the results can be read spectrophotometrically and interpreted by a personal computer. In this paper, different red blood cell adherence assays for AB0 grouping, Rh typing, Rh phenotyping, antibody screening and identification, as well as crossmatching will be described.

  18. Recent advances in solid phase peptide synthesis

    White, P.D.


    Since its introduction by Merrifield half a century ago, solid phase peptide synthesis has evolved to become the enabling technology for the development of peptide therapeutics. Using modern methods, 100 - 1000s of peptides can be routinely synthesised in parallel for screening as leads for drug development and peptide APIs are produced in ton scale. In this talk I consider the state of art and report on recent advances to overcome remaining issues such as aspartimide formation, racemisation ...

  19. Cellular Automata Model for Elastic Solid Material

    DONG Yin-Feng; ZHANG Guang-Cai; XU Ai-Guo; GAN Yan-Biao


    The Cellular Automaton (CA) modeling and simulation of solid dynamics is a long-standing difficult problem.In this paper we present a new two-dimensional CA model for solid dynamics.In this model the solid body is represented by a set of white and black particles alternatively positioned in the x-and y-directions.The force acting on each particle is represented by the linear summation of relative displacements of the nearest-neighboring particles.The key technique in this new model is the construction of eight coefficient matrices.Theoretical and numerical analyses show that the present model can be mathematically described by a conservative system.So,it works for elastic material.In the continuum limit the CA model recovers the well-known Navier equation.The coefficient matrices are related to the shear module and Poisson ratio of the material body.Compared with previous CA model for solid body,this model realizes the natural coupling of deformations in the x-and y-directions.Consequently,the wave phenomena related to the Poisson ratio effects are successfully recovered.This work advances significantly the CA modeling and simulation in the field of computational solid dynamics.

  20. Fundamental Material Properties Underlying Solid Oxide Electrochemistry

    Mogensen, Mogens Bjerg; Hansen, Karin Vels; Holtappels, Peter


    and electronic conductor (MIEC) the electrode is. Selected examples of literature studies of specific electrodes in solid oxide cells (SOC) are discussed. The reported effects of impurities - both impurities in the electrode materials and in the gases – point to high reactivity and mobility of materials...... in the TPB region. Also, segregations to the surfaces and interfaces of the electrode materials, which may affect the electrode reaction mechanism, are very dependent on the exact history of fabrication and operation. The positive effects of even small concentrations of nanoparticles in the electrodes may...

  1. ITER solid breeder blanket materials database

    Billone, M.C. [Argonne National Lab., IL (United States); Dienst, W. [Kernforschungszentrum Karlsruhe GmbH (Germany). Inst. fuer Material- und Festkoerperforschung; Flament, T. [CEA Centre d`Etudes de Fontenay-aux-Roses (France). Commissariat A L`Energie Atomique; Lorenzetto, P. [NET Team, Garching (Germany); Noda, K. [Japan Atomic Energy Research Inst., Takai, Ibaraki, (Japan); Roux, N. [CEA Centre d`Etudes et de Recherches Les Materiaux (France). Commissariat a L`Energie Atomique


    The databases for solid breeder ceramics (Li{sub 2},O, Li{sub 4}SiO{sub 4}, Li{sub 2}ZrO{sub 3} and LiAlO{sub 2}) and beryllium multiplier material are critically reviewed and evaluated. Emphasis is placed on physical, thermal, mechanical, chemical stability/compatibility, tritium, and radiation stability properties which are needed to assess the performance of these materials in a fusion reactor environment. Correlations are selected for design analysis and compared to the database. Areas for future research and development in blanket materials technology are highlighted and prioritized.

  2. Thermal Energy Storage with Phase Change Material

    Lavinia Gabriela SOCACIU


    Full Text Available Thermal energy storage (TES systems provide several alternatives for efficient energy use and conservation. Phase change materials (PCMs for TES are materials supplying thermal regulation at particular phase change temperatures by absorbing and emitting the heat of the medium. TES in general and PCMs in particular, have been a main topic in research for the last 30 years, but although the information is quantitatively enormous, it is also spread widely in the literature, and difficult to find. PCMs absorb energy during the heating process as phase change takes place and release energy to the environment in the phase change range during a reverse cooling process. PCMs possesses the ability of latent thermal energy change their state with a certain temperature. PCMs for TES are generally solid-liquid phase change materials and therefore they need encapsulation. TES systems using PCMs as a storage medium offers advantages such as high TES capacity, small unit size and isothermal behaviour during charging and discharging when compared to the sensible TES.

  3. PCM Concrete. [Phase Change Materials

    Juul Andersen, T. [Danish Technological Institute, Taastrup (Denmark); Poulsen, H.-H. [BASF A/S, Roedekro (Denmark); Passov, F. [Spaencom A/S, Hedehusene (Denmark); Heiselberg, P. [Aalborg Univ..Aalborg (Denmark)


    PCM-Concrete was a research and development project launched in 2009 and finished in 2012. The project, which was funded by The Danish National Advanced Technology Foundation, had a total budget of 1.7 million Euros and included 4 partners: Danish Technological Institute (project manager), Aalborg University, BASF A/S and Spaencom A/S. The overall vision of the project was to reduce energy consumption for heating and cooling in buildings by developing high-performance concrete structures microencapsulated Phase Change Materials (PCM). The PCM used in the project was Micronal produced by BASF A/S. Micronal is small capsules with an acrylic shell and inside a wax with a melting point at approx. 23 deg. C equal to a comfortable indoor temperature. During the melting process thermal energy is transferred to chemical reaction (melting/solidification) depending on PCM being heated up or cooled down. Adding Micronal to concrete would theoretically increase the thermal mass of the concrete and improve the diurnal heat capacity which is the amount of energy that can be stored and released during 24 hours. Nevertheless, it is a relatively new technology that has not received much attention, yet. In the PCM-Concrete project 5 main investigations were carried out: 1) Development of concrete mix design with PCM. 2) Investigation of thermal properties of the PCM concrete: thermal conductivity, specific heat capacity, density. 3) Up-scaling the research to industrial production of PCM-concrete structures. 4) Testing energy efficiency in full scale. 5) Confronting aesthetic and acoustic barriers to full exploitation of the potential of PCM-concrete structures. The results from the test program showed: 1) That the diurnal heat storage capacity is higher for all 4 hollow core decks with tiles attached compared to the reference hollow core deck. 2) The hollow core decks with concrete tiles without PCM performs slightly better than the tiles with PCM. 3) That is was impossible to

  4. A solid-phase microextraction fiber with carbon nanoparticles as sorbent material prepared by a simple flame-based preparation process.

    Sun, Min; Feng, Juanjuan; Qiu, Huamin; Fan, Lulu; Li, Leilei; Luo, Chuannan


    A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500μgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300μgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150μgL(-1). Limits of detection were 0.005μgL(-1) for three PAEs and 0.001-0.003μgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples.

  5. β-CD/ATP composite materials for use in dispersive solid-phase extraction to measure (fluoro)quinolone antibiotics in honey samples.

    Cui, Xiangqian; Zhang, Panjie; Yang, Xiaoling; Yang, Miyi; Zhou, Wenfeng; Zhang, Sanbin; Gao, Haixiang; Lu, Runhua


    A novel sorbent (β-CD/ATP composite) for dispersive solid-phase extraction (d-SPE) prepared by bonding β-cyclodextrin to modified attapulgite via silane coupling was used to determine the concentrations of four (fluoro)quinolones (Qs) in honey samples. The subsequent quantification of the Qs (ciprofloxacin, norfloxacin, ofloxacin, and gatifloxacin) was accomplished using high-performance liquid chromatography (HPLC) with ultraviolet detection after the d-SPE procedure. Parameters that may influence the extraction efficiency, such as type and volume of the eluent, type and amount of the sorbent, times of the vortex and sonication process, and pH of the sample, were investigated using batch and column procedures. The optimal experimental conditions (5 mL sample at pH 3, 4 mg of β-CD/ATP composite as the sorbent, 200 μL of 40% ammonia in methanol as the eluent, with vortex time 60s and sonication time 6 min, and no addition of salt) were obtained from this statistical evaluation. The limits of detection (LODs) were determined to the range from 0.30 to 3.95 μg L(-1). Good recoveries (83.6-88.6%) were obtained under the optimum conditions, and the relative standard deviations (RSDs), which are used to indicate reproducibility, were less than 7.4%. The method was validated with three real honey samples, and the results demonstrated that β-CD/ATP composite possessed a high adsorption capacity for Qs. Although the LODs were slightly higher than expected, this study confirmed the possibility of using cyclodextrin grafted palygorskite in analytical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Hyperdoping silicon with selenium: solid vs. liquid phase epitaxy

    Zhou, Shengqiang; Liu, Fang; Prucnal, S.; Gao, Kun; Khalid, M.; Baehtz, C.; Posselt, M.; Skorupa, W.; Helm, M


    Chalcogen-hyperdoped silicon shows potential applications in silicon-based infrared photodetectors and intermediate band solar cells. Due to the low solid solubility limits of chalcogen elements in silicon, these materials were previously realized by femtosecond or nanosecond laser annealing of implanted silicon or bare silicon in certain background gases. The high energy density deposited on the silicon surface leads to a liquid phase and the fast recrystallization velocity allows trapping o...

  7. Development of headspace solid-phase microextraction method for ...

    ... solid-phase microextraction method for the analysis of pesticide residues in fruit and ... Journal of Applied Sciences and Environmental Management ... interface temperature) and solid phase microextraction parameters (fiber coating type, ...

  8. Size Dependence of a Temperature-Induced Solid-Solid Phase Transition in Copper(I) Sulfide

    Rivest, Jessy B; Fong, Lam-Kiu; Jain, Prashant K; Toney, Michael F; Alivisatos, A Paul


    Determination of the phase diagrams for the nanocrystalline forms of materials is crucial for our understanding of nanostructures and the design of functional materials using nanoscale building blocks. The ability to study such transformations in nanomaterials with controlled shape offers further insight into transition mechanisms and the influence of particular facets. Here we present an investigation of the size-dependent, temperature-induced solid-solid phase transition in copper sulfide nanorods from low- to high-chalcocite. We find the transition temperature to be substantially reduced, with the high chalcocite phase appearing in the smallest nanocrystals at temperatures so low that they are typical of photovoltaic operation. Size dependence in phase trans- formations suggests the possibility of accessing morphologies that are not found in bulk solids at ambient conditions. These other- wise-inaccessible crystal phases could enable higher-performing materials in a range of applications, including sensing, switching, lighting, and photovoltaics.

  9. Wax Precipitation Modeled with Many Mixed Solid Phases

    Heidemann, Robert A.; Madsen, Jesper; Stenby, Erling Halfdan


    The behavior of the Coutinho UNIQUAC model for solid wax phases has been examined. The model can produce as many mixed solid phases as the number of waxy components. In binary mixtures, the solid rich in the lighter component contains little of the heavier component but the second phase shows sub...


    Douglas C. Hittle


    Passive solar systems integrated into residential structures significantly reduce heating energy consumption. Taking advantage of latent heat storage has further increased energy savings. This is accomplished by the incorporation of phase change materials into building materials used in passive applications. Trombe walls, ceilings and floors can all be enhanced with phase change materials. Increasing the thermal storage of floor tile by the addition of encapsulated paraffin wax is the proposed topic of research. Latent heat storage of a phase change material (PCM) is obtained during a change in phase. Typical materials use the latent heat released when the material changes from a liquid to a solid. Paraffin wax and salt hydrates are examples of such materials. Other PCMs that have been recently investigated undergo a phase transition from one solid form to another. During this process they will release heat. These are known as solid-state phase change materials. All have large latent heats, which makes them ideal for passive solar applications. Easy incorporation into various building materials is must for these materials. This proposal will address the advantages and disadvantages of using these materials in floor tile. Prototype tile will be made from a mixture of quartz, binder and phase change material. The thermal and structural properties of the prototype tiles will be tested fully. It is expected that with the addition of the phase change material the structural properties will be compromised to some extent. The ratio of phase change material in the tile will have to be varied to determine the best mixture to provide significant thermal storage, while maintaining structural properties that meet the industry standards for floor tile.

  11. Releasing metal catalysts via phase transition: (NiO)0.05-(SrTi0.8Nb0.2O3)0.95 as a redox stable anode material for solid oxide fuel cells.

    Xiao, Guoliang; Wang, Siwei; Lin, Ye; Zhang, Yanxiang; An, Ke; Chen, Fanglin


    Donor-doped perovskite-type SrTiO3 experiences stoichiometric changes at high temperatures in different Po2 involving the formation of Sr or Ti-rich impurities. NiO is incorporated into the stoichiometric strontium titanate, SrTi0.8Nb0.2O3-δ (STN), to form an A-site deficient perovskite material, (NiO)0.05-(SrTi0.8Nb0.2O3)0.95 (Ni-STN), for balancing the phase transition. Metallic Ni nanoparticles can be released upon reduction instead of forming undesired secondary phases. This material design introduces a simple catalytic modification method with good compositional control of the ceramic backbones, by which transport property and durability of solid oxide fuel cell anodes are largely determined. Using Ni-STN as anodes for solid oxide fuel cells, enhanced catalytic activity and remarkable stability in redox cycling have been achieved. Electrolyte-supported cells with the cell configuration of Ni-STN-SDC anode, La0.8Sr0.2Ga0.87Mg0.13O3 (LSGM) electrolyte, and La0.6Sr0.4Co0.2Fe0.8O3 (LSCF) cathode produce peak power densities of 612, 794, and 922 mW cm(-2) at 800, 850, and 900 °C, respectively, using H2 as the fuel and air as the oxidant. Minor degradation in fuel cell performance resulted from redox cycling can be recovered upon operating the fuel cells in H2. Such property makes Ni-STN a promising regenerative anode candidate for solid oxide fuel cells.

  12. Stability of solid oxide fuel cell materials

    Armstrong, T.R.; Pederson, L.R.; Stevenson, J.W.; Raney, P.E. [Pacific Northwest Lab., Richland, WA (United States)


    The phase stability and sintering behavior of materials used in SOFCs has been evaluated. The sintering behavior of Ca and Sr doped lanthanum. manganite (the preferred SOFC cathode material) is highly dependent on the relative proportion of A and B site cations in the material. Ca and Sr doped lanthanum chromite (the preferred interconnect material) have been shown to rapidly expand in reducing atmospheres at temperatures as low as 700{degrees}C. This expansion is due to the reduction of Cr{sup 4+} to Cr{sup 3+} in reducing environments.

  13. Fundamental Material Properties Underlying Solid Oxide Electrochemistry

    Mogensen, Mogens Bjerg; Hansen, Karin Vels; Holtappels, Peter


    and electronic conductor (MIEC) the electrode is. Selected examples of literature studies of specific electrodes in solid oxide cells (SOC) are discussed. The reported effects of impurities - both impurities in the electrode materials and in the gases – point to high reactivity and mobility of materials...... place. The length of the TPB is a key factor even though the width and depth of the zone, in which the rate limiting reactions take place, may vary depending of the degree of the electrode materials ability to conduct both electrons and ions, i.e. the TPB zone volume depends on how good a mixed ionic...... in the TPB region. Also, segregations to the surfaces and interfaces of the electrode materials, which may affect the electrode reaction mechanism, are very dependent on the exact history of fabrication and operation. The positive effects of even small concentrations of nanoparticles in the electrodes may...

  14. Parallel solid-phase synthesis of diaryltriazoles

    Matthias Wrobel


    Full Text Available A series of substituted diaryltriazoles was prepared by a solid-phase-synthesis protocol using a modified Wang resin. The copper(I- or ruthenium(II-catalyzed 1,3-cycloaddition on the polymer bead allowed a rapid synthesis of the target compounds in a parallel fashion with in many cases good to excellent yields. Substituted diaryltriazoles resemble a molecular structure similar to established terphenyl-alpha-helix peptide mimics and have therefore the potential to act as selective inhibitors for protein–protein interactions.

  15. Solid-phase synthesis of molecularly imprinted nanoparticles.

    Canfarotta, Francesco; Poma, Alessandro; Guerreiro, Antonio; Piletsky, Sergey


    Molecularly imprinted polymers (MIPs) are synthetic materials, generally based on acrylic or methacrylic monomers, that are polymerized in the presence of a specific target molecule called the 'template' and capable of rebinding selectively to this target molecule. They have the potential to be low-cost and robust alternatives to biomolecules such as antibodies and receptors. When prepared by traditional synthetic methods (i.e., with free template in solution), their usefulness has been limited by high binding site heterogeneity, the presence of residual template and the fact that the production methods are complex and difficult to standardize. To overcome some of these limitations, we developed a method for the synthesis of MIP nanoparticles (nanoMIPs) using an innovative solid-phase approach, which relies on the covalent immobilization of the template molecules onto the surface of a solid support (glass beads). The obtained nanoMIPs are virtually free of template and demonstrate high affinity for the target molecule (e.g., melamine and trypsin in our published work). Because of an affinity separation step performed on the solid phase after polymerization, poor binders and unproductive polymer are removed, so the final product has more uniform binding characteristics. The overall protocol, starting from the immobilization of the template onto the solid phase and including the purification and characterization of the nanoparticles, takes up to 1 week.

  16. Hot-water and solid-phase extraction of fluorescent whitening agents in paper materials and infant clothes followed by unequivocal determination with ion-pair chromatography-tandem mass spectrometry.

    Chen, Hsin-Chang; Ding, Wang-Hsien


    A comprehensive method for the determination of four stilbene-type disulfonate and one distyrylbiphenyl-type fluorescent whitening agents (FWAs) in paper materials (napkin and paper tissue) and infant clothes was developed. FWAs were extracted from paper material and cloth samples using a hot-water extraction, and the aqueous extracts were then preconcentrated with the newly developed Oasis WAX (mixed-mode of weak anion exchange and reversed-phase sorbent) solid-phase extraction cartridge. The analytes were unequivocal determined by ion pair chromatography coupled with negative electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS-MS), applying a di-n-hexyl-ammonium acetate (DHAA) as the ion-pairing reagent in mobile phase. Limits of quantitation (LOQ) were established between 0.2 and 0.9 ng/g in 2 g of samples. Recovery of five FWAs in spiked commercial samples was between 42 and 95% and RSD (n = 3) ranging from 2 to 11%. The method was finally applied to commercial samples, showing that two stilbene-type disulfonates were predominant FWAs detected in napkin and infant cloth samples.

  17. Numerical simulation of mechanical deformation of semi-solid material using a level-set based finite element method

    Sun, Zhidan; Bernacki, Marc; Logé, Roland; Gu, Guochao


    In this work, a level-set based finite element method was used to numerically evaluate the mechanical behavior in a small deformation range of semi-solid materials with different microstructure configurations. For this purpose, a finite element model of the semi-solid phase was built based on Voronoï diagram. Interfaces between the solid and the liquid phases were implicitly described by level-set functions coupled to an anisotropic meshing technique. The liquid phase was considered as a Newtonian fluid, whereas the behavior of the solid phase was described by a viscoplastic law. Simulations were performed to study the effect of different parameters such as solid phase fraction and solid bridging. Results show that the macroscopic mechanical behavior of semi-solid material strongly depends on the solid fraction and the local microstructure which play important roles in the formation of hot tearing. These results could provide valuable information for the processing of semi-solid materials.

  18. Solid-Phase Organic Synthesis and Catalysis: Some Recent Strategies Using Alumina, Silica, and Polyionic Resins

    Basudeb Basu; Susmita Paul


    Solid-phase organic synthesis (SPOS) and catalysis have gained impetus after the seminal discovery of Merrifield’s solid-phase peptide synthesis and also because of wide applicability in combinatorial and high throughput chemistry. A large number of organic, inorganic, or organic-inorganic hybrid materials have been employed as polymeric solid supports to promote or catalyze various organic reactions. This review article provides a concise account on our approaches involving the use of (i) al...

  19. Comparison of solid highlighter materials for thermography

    Genest, M.; Forsyth, D.S. [National Research Council of Canada, Inst. for Aerospace Research, Ottawa, Ontario (Canada)]. E-mail:; Maldague, X. [Univ. Laval, Electrical and Computing Engienering Dept., Quebec, Quebec (Canada)


    Bare metal surfaces are difficult to inspect with flash thermography due to the high reflectivity and low emissivity of metal surfaces. Often black paint is used to prepare these surfaces for inspection. The additional time required to apply, dry, and then remove paint after inspection can be a significant barrier to using thermographic inspection techniques in these applications. This paper examines the use of solid 'highlighter' materials instead of paint to provide desirable surface characteristics and ease of use. Both positive pressure and vacuum methods were used to apply a variety of materials to metal test specimens, which were then inspected with a commercial pulsed flash thermography system. A vacuum-applied black latex material provided surface performance close to that of black paint without the extra burden of paint application and removal. (author)

  20. Density-functional theory for fluid-solid and solid-solid phase transitions

    Bharadwaj, Atul S.; Singh, Yashwant


    We develop a theory to describe solid-solid phase transitions. The density functional formalism of classical statistical mechanics is used to find an exact expression for the difference in the grand thermodynamic potentials of the two coexisting phases. The expression involves both the symmetry conserving and the symmetry broken parts of the direct pair correlation function. The theory is used to calculate phase diagram of systems of soft spheres interacting via inverse power potentials u (r ) =ɛ "close="1 /n )">σ /r n , where parameter n measures softness of the potential. We find that for 1 /n ≥0.154 the body-centred-cubic (bcc) structure is preferred. The bcc structure transforms into the fcc structure upon increasing the density. The calculated phase diagram is in good agreement with the one found from molecular simulations.

  1. Studies on solid-solid phase transitions of polyols by infrared spectroscopy

    Feng, H.; Liu, X.; He, S.; Wu, K.; Zhang, J. [Department of Chemistry, Hebei Normal University, Shijiazhuang (China)


    This paper chiefly deals with the properties of polyols - a kind of energy storage material, by IR spectra. A series of infrared spectra at various temperatures were obtained for pentaerythritol (PE), pentaglycerine (PG), neopentylglycol (NPG) and their mixture NPG/PG. The experimental results (the shifts of -OH absorption band in IR spectra) support the solid-solid phase transition mechanism, which involves the reversible breaking of nearest-neighbor hydrogen bonds in the molecular crystals at transformation temperature. The correlation between the wave number shifts and the temperatures of phase transition is proposed in this paper. Finally, by means of infrared spectroscopy experiments, it is shown that aging has a great influence on the thermal properties of polyol mixtures.

  2. Accretion of solid materials onto circumplanetary disks from protoplanetary disks

    Tanigawa, Takayuki [Institute of Low Temperature Science, Hokkaido University, Sapporo 060-0819 (Japan); Maruta, Akito; Machida, Masahiro N., E-mail: [Department of Earth and Planetary Sciences, Kyushu University, Fukuoka 812-8581 (Japan)


    We investigate the accretion of solid materials onto circumplanetary disks from heliocentric orbits rotating in protoplanetary disks, which is a key process for the formation of regular satellite systems. In the late stage of the gas-capturing phase of giant planet formation, the accreting gas from protoplanetary disks forms circumplanetary disks. Since the accretion flow toward the circumplanetary disks affects the particle motion through gas drag force, we use hydrodynamic simulation data for the gas drag term to calculate the motion of solid materials. We consider a wide range of size for the solid particles (10{sup –2}-10{sup 6} m), and find that the accretion efficiency of the solid particles peaks around 10 m sized particles because energy dissipation of drag with circum-planetary disk gas in this size regime is most effective. The efficiency for particles larger than 10 m becomes lower because gas drag becomes less effective. For particles smaller than 10 m, the efficiency is lower because the particles are strongly coupled with the background gas flow, which prevents particles from accretion. We also find that the distance from the planet where the particles are captured by the circumplanetary disks is in a narrow range and well described as a function of the particle size.

  3. Solid Phase Synthesis of Polymacromer and Copolymacromer Brushes


    REPORT Solid Phase Synthesis of Polymacromer and Copolymacromer Brushes 14. ABSTRACT 16. SECURITY CLASSIFICATION OF: We report a novel solid phase...form poly-macromer brushes wherein macromonomers are linked via triazole groups. After each addition step, the terminal alkyne group can be deprotected...Research Triangle Park, NC 27709-2211 15. SUBJECT TERMS Solid Phase Synthesis , polymers and copolymers Hernán R. Rengifo, Cristian Grigoras, Benjamin I

  4. Solid freeform fabrication of biological materials

    Wang, Jiwen

    This thesis investigates solid freeform fabrication of biological materials for dental restoration and orthopedic implant applications. The basic approach in this study for solid freeform fabrication of biological materials is micro-extrusion of single or multiple slurries for 3D components and inkjet color printing of multiple suspensions for functionally graded materials (FGMs). Common issues associated with micro-extrusion and inkjet color printing are investigated. These common issues include (i) formulation of stable slurries with a pseudoplastic property, (ii) cross-sectional geometry of the extrudate as a function of the extrusion parameters, (iii) fabrication path optimization for extrusion process, (iv) extrusion optimization for multi-layer components, (v) composition control in functionally graded materials, and (vi) sintering optimization to convert the freeform fabricated powder compact to a dense body for biological applications. The present study clearly shows that the rheological and extrusion behavior of dental porcelain slurries depend strongly on the pH value of the slurry and extrusion conditions. A slurry with pseudoplastic properties is a basic requirement for obtaining extruded lines with rectangular cross-sections. The cross-sectional geometry of the extrudate is also strongly affected by extrusion parameters including the extrusion nozzle height, nozzle moving speed, extrusion rate, and critical nozzle height. Proper combinations of these extrusion parameters are necessary in order to obtain single line extrudates with near rectangular cross-sections and 3D objects with dimensional accuracy, uniform wall thickness, good wall uprightness, and no wall slumping. Based on these understandings, single-wall, multi-wall, and solid teeth have been fabricated via micro-extrusion of the dental slurry directly from a CAD digital model in 30 min. Inkjet color printing using stable Al2O3 and ZrO 2 aqueous suspensions has been developed to fabricate

  5. Two phase continuous digestion of solid manure on-farm

    Schaefer, W.; Lehto, M. [MTT Agrifood Research Finland, Vihti (Finland). Animal Production Research; Evers, L.; Granstedt, A. [Biodynamic Research Inst., Jaerna (Sweden)


    Present commercially available biogas plants are mainly suitable for slurry and co-substrates. Cattle, horse and poultry farms using a solid manure chain experience a crucial competitive disadvantage, because conversion to slurry technology requires additional investments. Based on the technological progress of anaerobic digestion of municipal solid waste, so called 'dry fermentation' prototype plants were developed for anaerobic digestion of organic material containing 15-50% total solids (Hoffman, 2001). These plants show added advantages compared to slurry digestion plants: Less reactor volume, less process energy, less transport capacity, less odour emissions. On-farm research (Gronauer and Aschmann, 2004; Kusch and Oechsner, 2004) and prototype research (Linke, 2004) on dry fermentation in batch reactors show that loading and discharging of batch reactors remains difficult and/or time-consuming compared to slurry reactors. Additionally a constant level of gas generation requires offset operation of several batch reactors. Baserga et al. (1994) developed a pilot plant of 9.6 m{sup 3} capacity for continuous digestion of solid beef cattle manure on-farm. However, on-farm dry fermentation plants are not common and rarely commercially available. We assume that lack of tested technical solutions and scarceness of on-farm research results are the main reason for low acceptance of dry fermentation technology on-farm. We report about an innovative two phase farm-scale biogas plant. The plant continuously digests dairy cattle manure and organic residues of the farm and the surrounding food processing units. The two phase reactor technology was chosen for two reasons: first it offers the separation of a liquid fraction and a solid fraction for composting after hydrolysis and secondly the methanation of the liquid fraction using fixed film technology results in a very short hydraulic retention time, reduction in reactor volume, and higher methane content of the

  6. Sealing materials for solid oxide fuel cells

    Larsen, P.H.


    A major obstacle in the achievement of high electrical efficiency for planar solid oxide fuel cell stacks (SOFC) is the need for long term stable seals at the operational temperature between 850 and 1000 deg. C. In the present work the formation and properties of sealing materials for SOFC stacks that fulfil the necessary requirements were investigated. The work comprises analysis of sealing material properties independently, in simple systems as well as tests in real SOFC stacks. The analysed sealing materials were based on pure glasses or glass-ceramic composites having B{sub 2}O{sub 3}, P{sub 2}O{sub 5} or siO{sub 2} as glass formers, and the following four glass systems were investigated: MgO/caO/Cr{sub 2}O{sub 3}-Al{sub 2}O{sub 3}B{sub 2}O{sub 3}-P{sub 2}O{sub 5}, MgO-Al{sub 2}O{sub 3}-P{sub 2}O{sub 5}, MgO-Al{sub 2}O{sub 3}-P{sub 2}O{sub 5}-SiO{sub 2} and BaO/Na{sub 2}O-Al{sub 2}O{sub 3}-SiO{sub 2}. (au) 32 tabs., 106 ills., 107 refs.

  7. Applied solid state science advances in materials and device research

    Wolfe, Raymond


    Applied Solid State Science: Advances in Materials and Device Research, Volume 4 covers articles on single crystal compound semiconductors and complex polycrystalline materials. The book discusses narrow gap semiconductors and solid state batteries. The text then describes the advantages of hot-pressed microcrystalline compacts of oxygen-octahedra ferroelectrics over single crystal materials, as well as heterostructure junction lasers. Solid state physicists, materials scientists, electrical engineers, and graduate students studying the subjects being discussed will find the book invaluable.

  8. Phase Change Material Thermal Power Generator

    Jones, Jack A.


    An innovative modification has been made to a previously patented design for the Phase Change Material (PCM) Thermal Generator, which works in water where ocean temperature alternatively melts wax in canisters, or allows the wax to re-solidify, causing high-pressure oil to flow through a hydraulic generator, thus creating electricity to charge a battery that powers the vehicle. In this modification, a similar thermal PCM device has been created that is heated and cooled by the air and solar radiation instead of using ocean temperature differences to change the PCM from solid to liquid. This innovation allows the device to use thermal energy to generate electricity on land, instead of just in the ocean.

  9. Thermodynamic phase behavior of API/polymer solid dispersions.

    Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele


    To improve the bioavailability of poorly soluble active pharmaceutical ingredients (APIs), these materials are often integrated into a polymer matrix that acts as a carrier. The resulting mixture is called a solid dispersion. In this work, the phase behaviors of solid dispersions were investigated as a function of the API as well as of the type and molecular weight of the carrier polymer. Specifically, the solubility of artemisinin and indomethacin was measured in different poly(ethylene glycol)s (PEG 400, PEG 6000, and PEG 35000). The measured solubility data and the solubility of sulfonamides in poly(vinylpyrrolidone) (PVP) K10 and PEG 35000 were modeled using the perturbed-chain statistical associating fluid theory (PC-SAFT). The results show that PC-SAFT predictions are in a good accordance with the experimental data, and PC-SAFT can be used to predict the whole phase diagram of an API/polymer solid dispersion as a function of the kind of API and polymer and of the polymer's molecular weight. This remarkably simplifies the screening process for suitable API/polymer combinations.

  10. Restricted accessed material-copper(II) ion imprinted polymer solid phase extraction combined with inductively coupled plasma-optical emission spectrometry for the determination of free Cu(II) in urine and serum samples.

    Cui, Chao; He, Man; Chen, Beibei; Hu, Bin


    A novel restricted accessed material (RAM)-Cu(II) ion imprinted polymer (IIP) was synthesized by the surface imprinted-emulsion method, and possessed a high selectivity to Cu(II) and good macromolecules exclusion property. And a novel method of RAM-IIP packed microcolumn solid phase extraction (SPE) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the determination of trace free Cu(II) in human body fluids. Under the optimized conditions, the adsorption capacity of RAM-IIP for Cu(II) was 15.9 mg g(-1). With a preconcentration factor of 30, the limit of detection was 0.17 µg L(-1), and the relative standard deviation was 2.2% (n=7, c=1 µg L(-1)). The developed method was validated by the analysis of two Certified Reference Materials, and the determined values were in good agreement with the certified values. This method was also successfully applied for the direct analysis of free Cu(II) in human urine and serum samples. While the total Cu can be determined by the proposed method after microwave digestion. The concentrations of free Cu(II) were much lower than that of total Cu, indicating that Cu is mainly coordinated with macromolecules in these biological samples. From this point of view, the developed method exhibits application potential in speciation of free metal ions and metallic complex molecules in biological samples. © 2013 Elsevier B.V. All rights reserved.

  11. Phase change materials science and applications

    Raoux, Simone


    ""Phase Change Materials: Science and Applications"" provides a unique introduction of this rapidly developing field. This clearly written volume describes the material science of these fascinating materials from a theoretical and experimental perspective.

  12. Advanced Materials and Solids Analysis Research Core (AMSARC)

    The Advanced Materials and Solids Analysis Research Core (AMSARC), centered at the U.S. Environmental Protection Agency's (EPA) Andrew W. Breidenbach Environmental Research Center in Cincinnati, Ohio, is the foundation for the Agency's solids and surfaces analysis capabilities. ...

  13. Advanced Materials and Solids Analysis Research Core (AMSARC)

    The Advanced Materials and Solids Analysis Research Core (AMSARC), centered at the U.S. Environmental Protection Agency's (EPA) Andrew W. Breidenbach Environmental Research Center in Cincinnati, Ohio, is the foundation for the Agency's solids and surfaces analysis capabilities. ...

  14. Chelating agent free-solid phase extraction (CAF-SPE) of Co(II), Cu(II) and Cd(II) by new nano hybrid material (ZrO{sub 2}/B{sub 2}O{sub 3})

    Yalcinkaya, Ozcan [Gazi University, Science Faculty, Department of Chemistry, 06500, Ankara (Turkey); Kalfa, Orhan Murat [Dumlupinar University, Science and Art Faculty, Department of Chemistry, 43100, Kuetahya (Turkey); Tuerker, Ali Rehber, E-mail: [Gazi University, Science Faculty, Department of Chemistry, 06500, Ankara (Turkey)


    Highlights: {yields} A novel sorbent for solid phase extraction for the preconcentration of metal ions. {yields} Hybrid nano-scale ZrO{sub 2}/B{sub 2}O{sub 3} as a new SPE material. {yields} There is a no need for using any chelating agents before the preconcentration procedure. - Abstract: New nano hybrid material (ZrO{sub 2}/B{sub 2}O{sub 3}) was synthesized and applied as a sorbent for the separation and/or preconcentration of Co(II), Cu(II) and Cd(II) in water and tea leaves prior to their determination by flame atomic absorption spectrometry. Synthesized nano material was characterized by scanning electron microscope, transmission electron microscope and X-ray diffraction. The optimum conditions for the quantitative recovery of the analytes, including pH, eluent type and volume, flow rate of sample solution were examined. The effect of interfering ions was also investigated. Under the optimum conditions, adsorption isotherms and adsorption capacities have been examined. The recoveries of Co(II), Cu(II) and Cd(II) were 96 {+-} 3%, 95 {+-} 3%, 98 {+-} 4% at 95% confidence level, respectively. The analytical detection limits for Co(II), Cu(II), and Cd(II) were 3.8, 3.3, and 3.1 {mu}g L{sup -1}, respectively. The reusability and adsorption capacities (32.2 mg g{sup -1} for Co, 46.5 mg g{sup -1} for Cu and 109.9 mg g{sup -1} for Cd) of the sorbent were found as satisfactory. The accuracy of the method was confirmed by analyzing certified reference material (GBW-07605 Tea leaves) and spiked real samples. The method was applied for the determination of analytes in tap water and tea leaves.

  15. Stable solid-phase Rh antigen.

    Yared, M A; Moise, K J; Rodkey, L S


    Numerous investigators have attempted to isolate the Rh antigens in a stable, immunologically reactive form since the discovery of the Rh system over 56 years ago. We report here a successful and reproducible approach to solubilizing and adsorbing the human Rh antigen(s) to a solid-phase matrix in an antigenically active form. Similar results were obtained with rabbit A/D/F red blood cell antigens. The antigen preparation was made by dissolution of the red blood cell membrane lipid followed by fragmentation of the residual cytoskeleton in an EDTA solution at low ionic strength. The antigenic activity of the soluble preparations was labile in standard buffers but was stable in zwitterionic buffers for extended periods of time. Further studies showed that the antigenic activity of these preparations was enhanced, as was their affinity for plastic surfaces, in the presence of acidic zwitterionic buffers. Adherence to plastic surfaces at low pH maintained antigenic reactivity and specificity for antibody was retained. The data show that this approach yields a stable form of antigenically active human Rh D antigen that could be used in a red blood cell-free assay for quantitative analysis of Rh D antibody and for Rh D antibody immunoadsorption and purification.

  16. Macrocyclic polyamine-functionalized silica as a solid-phase extraction material coupled with ionic liquid dispersive liquid-liquid extraction for the enrichment of polycyclic aromatic hydrocarbons.

    Liu, Longhui; He, Lijun; Jiang, Xiuming; Zhao, Wenjie; Xiang, Guoqiang; Anderson, Jared L


    In this study, silica modified with a 30-membered macrocyclic polyamine was synthesized and first used as an adsorbent material in SPE. The SPE was further combined with ionic liquid (IL) dispersive liquid-liquid microextraction (DLLME). Five polycyclic aromatic hydrocarbons were employed as model analytes to evaluate the extraction procedure and were determined by HPLC combined with UV/Vis detection. Acetone was used as the elution solvent in SPE as well as the dispersive solvent in DLLME. The enrichment of analytes was achieved using the 1,3-dibutylimidazolium bis[(trifluoromethyl)sulfonyl]imide IL/acetone/water system. Experimental conditions for the overall macrocycle-SPE-IL-DLLME method, such as the amount of adsorbent, sample solution volume, sample solution pH, type of elution solvent as well as addition of salt, were studied and optimized. The developed method could be successfully applied to the analysis of four real water samples. The macrocyclic polyamine offered higher extraction efficiency for analytes compared with commercially available C18 cartridge, and the developed method provided higher enrichment factors (2768-5409) for model analytes compared with the single DLLME. Good linearity with the correlation coefficients ranging from 0.9983 to 0.9999 and LODs as low as 0.002 μg/L were obtained in the proposed method.

  17. Metallic materials in solid oxide fuel cells

    Willem Joseph Quadakkers


    Full Text Available Fe-Cr alloys with variations in chromium content and additions of different elements were studied for potential application in intermediate temperature Solid Oxide Fuel Cell (SOFC. Recently, a new type of FeCrMn(Ti/La based ferritic steels has been developed to be used as construction material for SOFC interconnects. In the present paper, the long term oxidation resistance of this class of steels in both air and simulated anode gas will be discussed and compared with the behaviour of a number of commercial available ferritic steels. Besides, in-situ studies were carried out to characterize the high temperature conductivity of the oxide scales formed under these conditions. Main emphasis will be put on the growth and adherence of the oxide scales formed during exposure, their contact resistance at service temperature as well as their interaction with various perovskite type contact materials. Additionally, parameters and protection methods in respect to the volatilization of chromia based oxide scales will be illustrated.

  18. Preparation of Ion Exchange Films for Solid-Phase Spectrophotometry and Solid-Phase Fluorometry

    Hill, Carol M.; Street, Kenneth W.; Tanner, Stephen P.; Philipp, Warren H.


    Atomic spectroscopy has dominated the field of trace inorganic analysis because of its high sensitivity and selectivity. The advantages gained by the atomic spectroscopies come with the disadvantage of expensive and often complicated instrumentation. Solid-phase spectroscopy, in which the analyte is preconcentrated on a solid medium followed by conventional spectrophotometry or fluorometry, requires less expensive instrumentation and has considerable sensitivity and selectivity. The sensitivity gains come from preconcentration and the use of chromophore (or fluorophore) developers and the selectivity is achieved by use of ion exchange conditions that favor the analyte in combination with speciative chromophores. Little work has been done to optimize the ion exchange medium (IEM) associated with these techniques. In this report we present a method for making ion exchange polymer films, which considerably simplify the solid-phase spectroscopic techniques. The polymer consists of formaldehyde-crosslinked polyvinyl alcohol with polyacrylic acid entrapped therein. The films are a carboxylate weak cation exchanger in the calcium form. They are mechanically sturdy and optically transparent in the ultraviolet and visible portion of the spectrum, which makes them suitable for spectrophotometry and fluorometry.

  19. Investigation of binary solid phases by calorimetry and kinetic modelling

    Matovic, M.


    The traditional methods for the determination of liquid-solid phase diagrams are based on the assumption that the overall equilibrium is established between the phases. However, the result of the crystallization of a liquid mixture will typically be a non-equilibrium or metastable state of the solid

  20. Electrical transport in crystalline phase change materials

    Woda, Michael


    In this thesis, the electrical transport properties of crystalline phase change materials are discussed. Phase change materials (PCM) are a special class of semiconducting and metallic thin film alloys, typically with a high amount of the group five element antimony or the group six element tellurium, such as Ge{sub 2}Sb{sub 2}Te{sub 5}. The unique property portfolio of this material class makes it suitable for memory applications. PCMs reveal fast switching between two stable room-temperature phases (amorphous and crystalline) realized by optical laser or electrical current pulses in memory devices. Additionally, a pronounced property contrast in form of optical reflectivity and electrical conductivity between the amorphous and crystalline phase is the characteristic fingerprint of PCMs. The emerging electrical solid state memory PCRAM is a very promising candidate to replace Flash memory in the near future or to even become a universal memory, which is non-volatile and shows the speed and cyclability of DRAM. One of the main technological challenges is the switching process into the amorphous state, which is the most power demanding step. In order to reduce the switching power, the crystalline resistivity needs to be increased at a given voltage. Thus understanding and tayloring of this property is mandatory. In this work, first the technological relevance, i.e. optical and electrical memory concepts based on PCMs are introduced. Subsequently a description of the physical properties of PCMs in four categories is given. Namely, structure, kinetics, optical properties and electrical properties are discussed. Then important recent developments such as the identification of resonant bonding in crystalline PCMs and a property predicting coordination scheme are briefly reviewed. The following chapter deals with the theoretical background of electrical transport, while the next chapter introduces the experimental techniques: Sputtering, XRR, XRD, DSC, thermal annealing

  1. Isotope effects in dense solid hydrogen - Phase transition in deuterium at 190 + or - 20 GPa

    Hemley, R. J.; Mao, H. K.


    Raman measurements of solid normal deuterium compressed in a diamond-anvil cell indicate that the material undergoes a structural phase transformation at 190 + or - 20 GPa and 77 K. Spectroscopically, the transition appears analogous to that observed in hydrogen at 145 + or - 5 GPa. The large isotope effect on the transition pressure suggests there is a significant vibrational contribution to the relative stability of the solid phases of hydrogen at very high densities.

  2. Solid-solid phase transitions determined by differential scanning calorimetry.

    Murrill, E.; Whitehead, M. E.; Breed, L.


    Data are presented to show that tris(hydroxymethyl)acetic acid, monochloropentaerythritol, monofluoropentaerythritol, difluoropentaerythritol, monoaminopentaerythritol, and diaminopentaerythritol exhibit solid-state transitions to a plastic crystalline state. Transitional enthalpies in many of these substances are lower than might be expected by analogy with related structures, suggesting that some configurational contributions to their entropy increments have been inhibited.

  3. Solid-solid phase transitions determined by differential scanning calorimetry.

    Murrill, E.; Whitehead, M. E.; Breed, L.


    Data are presented to show that tris(hydroxymethyl)acetic acid, monochloropentaerythritol, monofluoropentaerythritol, difluoropentaerythritol, monoaminopentaerythritol, and diaminopentaerythritol exhibit solid-state transitions to a plastic crystalline state. Transitional enthalpies in many of these substances are lower than might be expected by analogy with related structures, suggesting that some configurational contributions to their entropy increments have been inhibited.

  4. Studies on solid phase synthesis,characterization and fluorescent property of the new rare earth complexes

    Shi, Jianwei; Xiaoxu TENG; Wang, Linling; Long, Rong


    Rare earth-β-diketone ligand complex luminescent material has stable chemical properties and excellent luminous property. Using europium oxide and (γ-NTA) as raw materials, novel rare earth-β-dione complexes are synthesized by solid state coordination chemistry. The synthesis temperature and milling time are discussed for optimization. Experimental results show that the suitable reaction situation is at 50 ℃ and 20 h for solid-phase synthesis. The compositions and structures of the complexes...

  5. Resilient Sealing Materials for Solid Oxide Fuel Cells

    Signo T. Reis; Richard K. Brow


    This report describes the development of ''invert'' glass compositions designed for hermetic seals in solid oxide fuel cells (SOFC). Upon sealing at temperatures compatible with other SOFC materials (generally {le}900 C), these glasses transform to glass-ceramics with desirable thermo-mechanical properties, including coefficients of thermal expansion (CTE) over 11 x 10{sup -6}/C. The long-term (>four months) stability of CTE under SOFC operational conditions (e.g., 800 C in wet forming gas or in air) has been evaluated, as have weight losses under similar conditions. The dependence of sealant properties on glass composition are described in this report, as are experiments to develop glass-matrix composites by adding second phases, including Ni and YSZ. This information provides design-guidance to produce desirable sealing materials.

  6. Synthesis and application of multi-walled carbon nanotubes-molecularly imprinted sol-gel composite material for on-line solid-phase extraction and high-performance liquid chromatography determination of trace Sudan IV

    Zhang Zhaohui, E-mail: [College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000 (China); State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University, Changsha 410082 (China); Zhang Huabin; Hu Yufang [College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000 (China); Yao Shouzhuo [State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University, Changsha 410082 (China)


    A novel composite material of multi-walled carbon nanotubes (MWNTs)-Sudan IV molecularly imprinted polymers (MIPs) was prepared by surface molecular imprinting technique in combination with sol-gel technology. The MWNTs-MIPs were evaluated by scanning electron micrograph (SEM), Fourier transform infrared spectroscopy (FT-IR), and adsorption experiments. The results showed that the MWNTs-MIPs exhibited good selective recognition to Sudan IV. The maximum saturated binding capacity (Q{sub max}) is 63.2 {mu}mol g{sup -1}. Applied as sorbent, the MWNTs-MIPs were used for the determination of trace Sudan IV in chilli powder by on-line solid-phase extraction-high-performance liquid chromatography (SPE-HPLC). The results showed that an enrichment factor of 741 was achieved with a loading flow rate of 1.0 mL min{sup -1} for sampling 50 mL. The MWNTs-MIPs provided a fast and convenience determination platform for Sudan IV in real samples.

  7. Sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as a new dispersive solid-phase extraction material for acrylamide determination in food with direct gas chromatography-mass spectrometry analysis.

    Omar, Mei Musa Ali; Wan Ibrahim, Wan Aini; Elbashir, Abdalla Ahmed


    A sol-gel hybrid sorbent, methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was successfully used as new dispersive solid phase extraction (dSPE) sorbent material in the determination of acrylamide in several Sudanese foods and analysis using GC-MS. Several important dSPE parameters were optimised. Under the optimised conditions, excellent linearity (r(2)>0.9998) was achieved using matrix matched standard calibration in the concentration range 50-1000 μg kg(-1). The limits of detection (LOD) and limit of quantification ranged from 9.1 to 12.8 μg/kg and 27.8-38.9 μg/kg, respectively. The precision (RSD%) of the method was ⩽6.6% and recoveries of acrylamide obtained were in the range of 88-103%, (n=3). The LOD obtained is comparable with the LODs of primary secondary amine dSPE. The proposed MTMOS-TEOS dSPE method is direct and safe for acrylamide analysis, showed reliable method validation performances and good cleanup effects. It was successfully applied to the analysis of acrylamide in real food samples.

  8. Synthesis and application of molecularly imprinted poly(methacrylic acid)-silica hybrid composite material for selective solid-phase extraction and high-performance liquid chromatography determination of oxytetracycline residues in milk.

    Lv, Yun-Kai; Wang, Li-Min; Yang, Lei; Zhao, Chen-Xi; Sun, Han-Wen


    A novel molecularly imprinted organic-inorganic hybrid composite material (MIP-HCM) was developed based on molecular imprinting technique in combination with hybrid composite synthesis and sol-gel technology for selective solid-phase extraction (SPE) of tetracyclines residues in milk. The MIP-HCM was prepared using oxytetracycline as the template, methacrylic acid as organic functional monomer, tetraethoxysilane as inorganic precursor and methacryloxypropyltrimethoxysilane as the coupling agent. Synthesis conditions are optimized by changing some factors to obtain sorbent with the controllable adsorption capacity, selectivity, hardness and toughness. Binding study demonstrated that the imprinted hybrid composites showed excellent affinity and high selectivity to oxytetracycline. An enrichment factor of 18.8 along with a good sample clean-up was obtained under the optimized SPE conditions. The average recoveries of three tetracyclines antibiotics spiked milk at 0.1, 0.2 and 0.5 mg kg⁻¹ were in the range of 80.9-104.3% with the precision of 1.5-5.0%. The limits of detection and quantitation of the proposed method were in a range of 4.8-12.7 μg kg⁻¹ and 16.0-42.3 μg kg⁻¹, respectively.

  9. Multi-residue determination of 171 pesticides in cowpea using modified QuEChERS method with multi-walled carbon nanotubes as reversed-dispersive solid-phase extraction materials.

    Han, Yongtao; Song, Le; Zou, Nan; Chen, Ronghua; Qin, Yuhong; Pan, Canping


    A rapid and sensitive method for the determination of 171 pesticides in cowpea was developed using multi-walled carbon nanotubes (MWCNTs) as reversed-dispersive solid-phase (r-DSPE) extraction materials. The clean-up performance of MWCNTs was proved to be obviously superior to PSA and GCB. This method was validated on cowpea spiked at 0.01 and 0.1mgkg(-1) with five replicates. The mean recoveries for 169 pesticides ranged from 74% to 129% with relative standard deviations (RSDs) (n=5) lower than 16.4%, except diflufenican and quizalofop-ethyl. Good linearity for all pesticides was obtained with the calibration curve coefficients (R(2)) larger than 0.9970. The limit of detection (LODs) and limit of quantification (LOQs) for the 171 pesticides ranged from 0.001 to 0.003mgkg(-1) and from 0.002 to 0.009mgkg(-1), respectively. The method was demonstrated to be reliable and sensitive for the routine monitoring of the 171 pesticides in cowpea samples.

  10. Tuning of the vinyl groups' spacing at surface of modified silica in preparation of high density imprinted layer-coated silica nanoparticles: a dispersive solid-phase extraction materials for chlorpyrifos.

    Lu, Qing; Chen, Xuemei; Nie, Li; Luo, Jing; Jiang, Huijun; Chen, Lina; Hu, Qin; Du, Shuhu; Zhang, Zhongping


    This paper reports the preparation of high density imprinted layer-coated silica nanoparticles toward selective recognition and fast enrichment of chlorpyrifos (CP) from complicated matrices. The molecularly imprinted polymers (MIPs) were successfully coated at the surface of modified silica through using the chemical immovable vinyl groups at the nanoparticles' surface, followed by the graft copolymerization of methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) in the presence of templates CP. It has been demonstrated that the space of end vinyl groups at the surface of silica can be controlled by changing the condition of chemical modification, regulating the thickness of imprinted shells and the density of efficient imprinted sites. After removal of templates by solvent extraction, the recognition sites of CP were created in the polymer coating layer. The CP-imprinted nanoparticles exhibited high recognition selectivity and binding affinity to CP analyte. When the CP-imprinted nanoparticles were used as dispersive solid-phase extraction (dSPE) materials, the high recovery yields of 76.1-93.5% from various spiked samples with only 1microg/mL analyte were achieved by one-step extraction. These results reported herein provide the possibility for the separation and enrichment of CP from complicated matrices by the molecular imprinting modification at the surface of common silica nanoparticles.



    Velocities of solid phase and liquid phase in debris flow are one key problem to research on impact and abrasion mechanism of banks and control structures under action of debris flow. Debris flow was simplified as two-phase liquid composed of solid phase with the same diameter particles and liquid phase with the same mechanical features. Assume debris flow was one-dimension two-phase liquid moving to one direction,then general equations of velocities of solid phase and liquid phase were founded in twophase theory. Methods to calculate average pressures, volume forces and surface forces of debris flow control volume were established. Specially, surface forces were ascertained using Bingham's rheology equation of liquid phase and Bagnold's testing results about interaction between particles of solid phase. Proportional coefficient of velocities between liquid phase and solid phase was put forward, meanwhile, divergent coefficient between theoretical velocity and real velocity of solid phase was provided too. To state succinctly before, method to calculate velocities of solid phase and liquid phase was obtained through solution to general equations. The method is suitable for both viscous debris flow and thin debris flow. Additionally, velocities every phase can be identified through analyzing deposits in-situ after occurring of debris flow. It is obvious from engineering case the result in the method is consistent to that in real-time field observation.

  12. Diffusion in Solids Fundamentals, Methods, Materials, Diffusion-Controlled Processes

    Mehrer, Helmut


    Diffusion is a vital topic in solid-state physics and chemistry, physical metallurgy and materials science. Diffusion processes are ubiquitous in solids at elevated temperatures. A thorough understanding of diffusion in materials is crucial for materials development and engineering. This book first gives an account of the central aspects of diffusion in solids, for which the necessary background is a course in solid state physics. It then provides easy access to important information about diffuson in metals, alloys, semiconductors, ion-conducting materials, glasses and nanomaterials. Several diffusion-controlled phenomena, including ionic conduction, grain-boundary and dislocation pipe diffusion, are considered as well. Graduate students in solid-state physics, physical metallurgy, materials science, physical and inorganic chemistry or geophysics will benefit from this book as will physicists, chemists, metallurgists, materials engineers in academic and industrial research laboratories.

  13. Hyperdoping silicon with selenium: solid vs. liquid phase epitaxy.

    Zhou, Shengqiang; Liu, Fang; Prucnal, S; Gao, Kun; Khalid, M; Baehtz, C; Posselt, M; Skorupa, W; Helm, M


    Chalcogen-hyperdoped silicon shows potential applications in silicon-based infrared photodetectors and intermediate band solar cells. Due to the low solid solubility limits of chalcogen elements in silicon, these materials were previously realized by femtosecond or nanosecond laser annealing of implanted silicon or bare silicon in certain background gases. The high energy density deposited on the silicon surface leads to a liquid phase and the fast recrystallization velocity allows trapping of chalcogen into the silicon matrix. However, this method encounters the problem of surface segregation. In this paper, we propose a solid phase processing by flash-lamp annealing in the millisecond range, which is in between the conventional rapid thermal annealing and pulsed laser annealing. Flash lamp annealed selenium-implanted silicon shows a substitutional fraction of ~ 70% with an implanted concentration up to 2.3%. The resistivity is lower and the carrier mobility is higher than those of nanosecond pulsed laser annealed samples. Our results show that flash-lamp annealing is superior to laser annealing in preventing surface segregation and in allowing scalability.

  14. Solid State Ionic Materials - Proceedings of the 4th Asian Conference on Solid State Ionics

    Chowdari, B. V. R.; Yahaya, M.; Talib, I. A.; Salleh, M. M.


    The Table of Contents for the full book PDF is as follows: * Preface * I. INVITED PAPERS * Diffusion of Cations and Anions in Solid Electrolytes * Silver Ion Conductors in the Crystalline State * NMR Studies of Superionic Conductors * Hall Effect and Thermoelectric Power in High Tc Hg-Ba-Ca-Cu-O Ceramics * Solid Electrolyte Materials Prepared by Sol-Gel Chemistry * Preparation of Proton-Conducting Gel Films and their Application to Electrochromic Devices * Thin Film Fuel Cells * Zirconia based Solid Oxide Ion Conductors in Solid Oxide Fuel Cells * The Influence of Anion Substitution on Some Phosphate-based Ion Conducting Glasses * Lithium Intercalation in Carbon Electrodes and its Relevance in Rocking Chair Batteries * Chemical Sensors using Proton Conducting Ceramics * NMR/NQR Studies of Y-Ba-Cu-O Superconductors * Silver Molybdate Glasses and Battery Systems * New Highly Conducting Polymer Ionics and their Application in Electrochemical Devices * Study of Li Electrokinetics on Oligomeric Electrolytes using Microelectrodes * Calculation of Conductivity for Mixed-Phase Electrolytes PEO-MX-Immiscible Additive by Means of Effective Medium Theory * II. CONTRIBUTED PAPERS * Phase Relationship and Electrical Conductivity of Sr-V-O System with Vanadium Suboxide * Amorphous Li+ Ionic Conductors in Li2SO4-Li2O-P2O5 System * Fast Ion Transport in KCl-Al2O3 Composites * The Effect of the Second Phase Precipitation on the Ionic Conductivity of Zr0.85Mg0.15O1.85 * Conductivity Measurements and Phase Relationships in CaCl2-CaHCl Solid Electrolyte * Relationships Between Crystal Structure and Sodium Ion Conductivity in Na7Fe4(AsO4)6 and Na3Al2(AsO4)3 * Electrical Conductivity and Solubility Limit of Ti4+ Ion in Na1+x TiyZr2-ySixP3-xO12 System * Study on Sodium Fast Ion Conductors of Na1+3xAlxTi2-xSi2xP3-2xO12 System * Influences of Zirconia on the Properties of β''-Alumina Ceramics * Decay of Luminescence from Cr3+ Ions in β-Alumina * Lithium Ion Conductivity in the Li4XO4-Li2

  15. Materials for diode pumped solid state lasers

    Chase, L. L.; Davis, L. E.; Krupke, W. F.; Payne, S. A.


    The advantages of semiconductor diode lasers and laser arrays as pump sources for solid state lasers are reviewed. The properties that are desirable in solid state laser media for various diode pumping applications are discussed, and the characteristics of several promising media are summarized.

  16. Youth Solid Waste Educational Materials List, November 1991.

    Cornell Univ., Ithaca, NY. Cooperative Extension Service.

    This guide provides a brief description and ordering information for approximately 300 educational materials for grades K-12 on the subject of solid waste. The materials cover a variety of environmental issues and actions related to solid waste management. Entries are divided into five sections including audiovisual programs, books, magazines,…

  17. Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

    Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao


    An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. The role of solid-solid phase transitions in mantle convection

    Faccenda, Manuele; Dal Zilio, Luca


    With changing pressure and temperature conditions, downwelling and upwelling crustal and mantle rocks experience several solid-solid phase transitions that affect the mineral physical properties owing to structural changes in the crystal lattice and to the absorption or release of latent heat. Variations in density, together with phase boundary deflections related to the non-null reaction slope, generate important buoyancy forces that add to those induced by thermal perturbations. These buoyancy forces are proportional to the density contrast between reactant and product phases, their volume fraction, the slope and the sharpness of the reaction, and affect the style of mantle convection depending on the system composition. In a homogeneous pyrolitic mantle there is little tendency for layered convection, with slabs that may stagnate in the transition zone because of the positive buoyancy caused by post-spinel and post-ilmenite reactions, and hot plumes that are accelerated by phase transformations in the 600-800 km depth range. By adding chemical and mineralogical heterogeneities as on Earth, phase transitions introduce bulk rock and volatiles filtering effects that generate a compositional gradient throughout the entire mantle, with levels that are enriched or depleted in one or more of these components. Phase transitions often lead to mechanical softening or hardening that can be related to a different intrinsic mechanical behaviour and volatile solubility of the product phases, the heating or cooling associated with latent heat, and the transient grain size reduction in downwelling cold material. Strong variations in viscosity would enhance layered mantle convection, causing slab stagnation and plume ponding. At low temperatures and relatively dry conditions, reactions are delayed due to the sluggish kinetics, so that non-equilibrium phase aggregates can persist metastably beyond the equilibrium phase boundary. Survival of low-density metastable olivine

  19. Molybdate Based Ceramic Negative-Electrode Materials for Solid Oxide Cells

    Graves, Christopher R.; Reddy Sudireddy, Bhaskar; Mogensen, Mogens Bjerg


    Novel molybdate materials with varying Mo valence were synthesized as possible negative-electrode materials for solid oxide cells. The phase, stability, microstructure and electrical conductivity were characterized. The electrochemical activity for H2O and CO2 reduction and H2 and CO oxidation wa...

  20. Electrostatic levitation studies of supercooled liquids and metastable solid phases

    Rustan, Gustav Errol

    A new laboratory has been developed at Iowa State University (ISU) to be used for the study of high temperature liquids and solids, with particular focus on the supercooling of liquids and their metastable solidification products. This new laboratory employs the electrostatic levitation (ESL) technique, in which a charged sample is suspended between a set of electrodes to achieve non-contact handling. Owing to the elimination of a crucible, high temperature processing of samples can be achieved with reduced levels of contamination and heterogeneous nucleation. Because of the reduction in heterogeneous nucleation, samples can be supercooled well below their equilibrium melting temperature, opening the door to a wide range of measurements on supercooled liquids. Measurements methods have been implemented for the characterization of thermophysical properties such as: volume/density, ratio of specific heat to total hemispherical emissivity, surface tension, viscosity, electrical resistivity, and magnetic susceptibility. For measurements of electrical resistivity and magnetic susceptibility, a new method has been developed at ISU based on the tunnel diode oscillator (TDO) technique. The TDO technique uses the negative differential resistance of a tunnel diode to drive an LC tank circuit into self-sustained oscillation at the resonant LC frequency. The LC tank is inductively coupled to the samples under study, and changes in the electrical resistivity or magnetic susceptibility of the sample are manifested as changes in the resonant frequency. By measuring the frequency shifts of the TDO, insights can be made into changes in the material's electrical and magnetic properties. This method has been validated by performing resistivity measurements on a sample of high purity Zr, and by performing measurements on the ferromagnetic transition in a low-carbon steel ball bearing. In addition to the development of the laboratory and its supporting instrumentation, an effort has

  1. The solid lubricating material experiment device for Shenzhou-7 Spaceship


    A solid lubricating material exposure experiment in space is one of the missions during the seventh manned spaceflight of China,and the key is to develop a device which can be fixed reliably outside of the orbital module and can be fetched conveniently by an astronaut during space walk.The solid lubricating material experiment device needs to be locked reliably in a vibrating and impacting environment during the launch phase,and should meet the requirement that it can be unlocked and fetched reliably by the astronaut wearing an extravehicular spacesuit via simple operations in orbit in an environment of high and low temperature.As for the device we developed,the environmental characteristic of the mission was analyzed,the mechanical analysis and thermal analysis were carried out,and then a mechanism with functions of mechanical locking,structural self-locking and manual unlocking was designed.The device was verified by a sequence of experiments and was fetched by the astronaut during the flight of the Shenzhou-7 Spaceship.

  2. Automated solid-phase synthesis of oligosaccharides containing sialic acids

    Chian-Hui Lai


    Full Text Available A sialic acid glycosyl phosphate building block was designed and synthesized. This building block was used to prepare α-sialylated oligosaccharides by automated solid-phase synthesis selectively.


    B. S. Chandravanshi

    cation exchange-solid phase extraction (SCX-SPE) was investigated as an .... Stock solutions, with a concentration of 1.00 mg/mL were prepared ... Johannesburg, South Africa) connected to a vacuum pump (Vacuubrand, GMBH, Germany).

  4. Combinatorial Solid-Phase Synthesis of Balanol Analogues

    Nielsen, John; Lyngsø, Lars Ole


    The natural product balanol has served as a template for the design and synthesis of a combinatorial library using solid-phase chemistry. Using a retrosynthetic analysis, the structural analogues have been assembled from three relatively accessible building blocks. The solid-phase chemistry inclu...... including MSNT-mediated esterification of both support-bound alcohols and carboxylic acids has been implemented successfully. Copyright (C) 1996 Elsevier Science Ltd....

  5. Combinatorial Solid-Phase Synthesis of Balanol Analogues

    Nielsen, John; Lyngsø, Lars Ole


    The natural product balanol has served as a template for the design and synthesis of a combinatorial library using solid-phase chemistry. Using a retrosynthetic analysis, the structural analogues have been assembled from three relatively accessible building blocks. The solid-phase chemistry inclu...... including MSNT-mediated esterification of both support-bound alcohols and carboxylic acids has been implemented successfully. Copyright (C) 1996 Elsevier Science Ltd....

  6. Vapour phase synthesis of salol over solid acids via transesterification

    S Z Mohamed Shamshuddin; N Nagaraju


    The transesterification of methyl salicylate with phenol has been studied in vapour phase over solid acid catalysts such as ZrO2, MoO3 and SO$^{2-}_{4}$ or Mo(VI) ions modified zirconia. The catalytic materials were prepared and characterized for their total surface acidity, BET surface area and powder XRD patterns. The effect of mole-ratio of the reactants, catalyst bed temperature, catalyst weight, flowrate of reactants, WHSV and time-on-stream on the conversion (%) of phenol and selectivity (%) of salol has been investigated. A good yield (up to 70%) of salol with 90% selectivity was observed when the reactions were carried out at a catalyst bed temperature of 200°C and flow-rate of 10 mL/h in presence of Mo(VI)/ZrO2 as catalyst. The results have been interpreted based on the variation of acidic properties and powder XRD phases of zirconia on incorporation of SO$^{2-}_{4}$ or Mo(VI) ions. The effect of poisoning of acid sites of SO$^{2-}_{4}$ or Mo(VI) ions modified zirconia on total surface acidity, powder XRD phases and catalytic activity was also studied. Possible reaction mechanisms for the formation of salol and diphenyl ether over acid sites are proposed.

  7. The Structural Phase Transition in Solid DCN

    Dietrich, O. W.; Mackenzie, Gordon A.; Pawley, G. S.


    Neutron scattering measurements on deuterated hydrogen cyanide have shown that the structural phase change from a tetragonal to an orthorhombic form at 160K is a first-order transition. A transverse acoustic phonon mode, which has the symmetry of the phase change, was observed at very low energies...... and showed 'softening' as the transition temperature was approached from above....

  8. Magnetic Solid Phase Extraction Applied to Food Analysis

    Israel S. Ibarra


    Full Text Available Magnetic solid phase extraction has been used as pretreatment technique for the analysis of several compounds because of its advantages when it is compared with classic methods. This methodology is based on the use of magnetic solids as adsorbents for preconcentration of different analytes from complex matrices. Magnetic solid phase extraction minimizes the use of additional steps such as precipitation, centrifugation, and filtration which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique which were applied in food analysis.

  9. Fuel spill identification using solid-phase extraction and solid-phase microextraction. 1. Aviation turbine fuels.

    Lavine, B K; Brzozowski, D M; Ritter, J; Moores, A J; Mayfield, H T


    The water-soluble fraction of aviation jet fuels is examined using solid-phase extraction and solid-phase microextraction. Gas chromatographic profiles of solid-phase extracts and solid-phase microextracts of the water-soluble fraction of kerosene- and nonkerosene-based jet fuels reveal that each jet fuel possesses a unique profile. Pattern recognition analysis reveals fingerprint patterns within the data characteristic of fuel type. By using a novel genetic algorithm (GA) that emulates human pattern recognition through machine learning, it is possible to identify features characteristic of the chromatographic profile of each fuel class. The pattern recognition GA identifies a set of features that optimize the separation of the fuel classes in a plot of the two largest principal components of the data. Because principal components maximize variance, the bulk of the information encoded by the selected features is primarily about the differences between the fuel classes.

  10. Traveling waves for models of phase transitions of solids driven by configurational forces

    Kawashima, Shuichi


    This article is concerned with the existence of traveling wave solutions, including standing waves, to some models based on configurational forces, describing respectively the diffusionless phase transformations of solid materials, e.g., Steel, and phase transitions due to interface motion by interface diffusion, e.g., Sintering. These models are recently proposed by Alber and Zhu. We consider both the order-parameter-conserved case and the non-conserved one, under suitable assumptions. Also we compare our results with the corresponding ones for the Allen-Cahn and the Cahn-Hilliard equations coupled with linear elasticity, which are models for diffusion-dominated phase transformations in elastic solids.

  11. Research of solid-solid phase change heat storage material applied in solar collector to produce high temperature air%固-固相变蓄热材料在太阳能高温空气集热系统中的应用研究

    胡仁林; 刘振华; 赵峰; 肖红升


    为利用太阳能获得稳定持续的高温空气工质,除了有效集热外,还需要解决因太阳辐射强度变化导致输出工质温度波动的问题.在性能优良的太阳能集热系统中采用蓄热技术是解决此问题的有效途径.根据给定的设计目标,研究将固-固相变蓄热材料季戊四醇应用到太阳能集热蓄热一体化的实验装置中.实验结果表明:按集热蓄热一体化思路设计的实验装置,集热单元能够输出最高温度超过220℃的高温空气,蓄热单元能够将高温空气的温度稳定在蓄热材料的相变温度附近.并且随着蓄热管级数的增加,空气出口温度稳定的时间就越长,为利用太阳能获得稳定持续的高温热媒工质奠定了基础.%In order to get high temperature air constantly through the utilization of solar energy,the fluctuation of the air outlet temperature caused by the changing solar radiation must also be taken into consideration besides the effective collection of solar energy. Therefore,the adoption of heat storage technology in a solar energy collector of high efficiency is a feasible approach to diminish the temperature fluctuation. The solid-solid phase change material-Pentaerythritol was used as heat storage material in the solar energy collector/storage designed by an integrated method. The experimental results indicate that the maximum air outlet temperature of heating units exceeds 220 ℃ and the heat storage units can stabilize the air temperature around the phase-transition temperature of Pentaerythritol for a short time,which tends to be longer with the increase of the number of heat storage units. The results provide a foundation for the utilization of solar energy collector to get stable and high temperature air constantly through the application of phase change material.

  12. N-Acyliminium Intermediates in Solid-Phase Synthesis

    Quement, Sebastian Thordal le; Petersen, Rico; Meldal, M.


    N-Acyliminium ions are powerful intermediates in synthetic organic chemistry. Examples of their use are numerous in solution-phase synthesis, but there are unmerited few reports on these highly reactive electrophiles in solid-phase synthesis. The present review covers the literature to date and i...

  13. Solid phase extraction method for determination of mitragynine in ...

    mitragynine in urine and its application to mitragynine excretion ... Purpose: To develop a solid phase extraction (SPE) method that utilizes reverse-phase high performance .... solution of MG (1 mg/mL) which was further ... Facility, Prince of Songkla University and carried ..... d), which permit unrestricted use, distribution,.

  14. Ultrafast laser spectroscopy in complex solid state materials

    Li, Tianqi [Iowa State Univ., Ames, IA (United States)


    This thesis summarizes my work on applying the ultrafast laser spectroscopy to the complex solid state materials. It shows that the ultrafast laser pulse can coherently control the material properties in the femtosecond time scale. And the ultrafast laser spectroscopy can be employed as a dynamical method for revealing the fundamental physical problems in the complex material systems.

  15. Anisotropic kinetics of solid phase transition from first principles: alpha-omega phase transformation of Zr.

    Guan, Shu-Hui; Liu, Zhi-Pan


    Structural inhomogeneity is ubiquitous in solid crystals and plays critical roles in phase nucleation and propagation. Here, we develop a heterogeneous solid-solid phase transition theory for predicting the prevailing heterophase junctions, the metastable states governing microstructure evolution in solids. Using this theory and first-principles pathway sampling simulation, we determine two types of heterophase junctions pertaining to metal α-ω phase transition at different pressures and predict the reversibility of transformation only at low pressures, i.e. below 7 GPa. The low-pressure transformation is dominated by displacive Martensitic mechanism, while the high-pressure one is controlled by the reconstructive mechanism. The mechanism of α-ω phase transition is thus highly pressure-sensitive, for which the traditional homogeneous model fails to explain the experimental observations. The results provide the first atomic-level evidence on the coexistence of two different solid phase transition mechanisms in one system.

  16. The Structural Phase Transition in Solid DCN

    Dietrich, O. W.; Mackenzie, Gordon A.; Pawley, G. S.


    Neutron scattering measurements on deuterated hydrogen cyanide have shown that the structural phase transition from a tetragonal to an orthorhombic form at 160 K is a first order transition. A transverse acoustic phonon mode, which has the symmetry of the transition was observed at very low energ...... energies and showed “softening” as the transition was approached from above.......Neutron scattering measurements on deuterated hydrogen cyanide have shown that the structural phase transition from a tetragonal to an orthorhombic form at 160 K is a first order transition. A transverse acoustic phonon mode, which has the symmetry of the transition was observed at very low...

  17. Temperature reduction due to the application of phase change materials

    Voelker, Conrad; Kornadt, Oliver [Department of Building Physics, Bauhaus-University Weimar, Coudraystrasse 11a, 99423 Weimar (Germany); Ostry, Milan [Faculty of Civil Engineering, Brno University of Technology, Department of Building Structures, Veveri 95, 602 00 Brno (Czech Republic)


    Overheating is a major problem in many modern buildings due to the utilization of lightweight constructions with low heat storing capacity. A possible answer to this problem is the emplacement of phase change materials (PCM), thereby increasing the thermal mass of a building. These materials change their state of aggregation within a defined temperature range. Useful PCM for buildings show a phase transition from solid to liquid and vice versa. The thermal mass of the materials is increased by the latent heat. A modified gypsum plaster and a salt mixture were chosen as two materials for the study of their impact on room temperature reduction. For realistic investigations, test rooms were erected where measurements were carried out under different conditions such as temporary air change, alternate internal heat gains or clouding. The experimental data was finally reproduced by dint of a mathematical model. (author)

  18. Electrical conduction in solid materials physicochemical bases and possible applications

    Suchet, J P


    Electrical Conduction in Solid Materials (Physicochemical Bases and Possible Applications) investigates the physicochemical bases and possible applications of electrical conduction in solid materials, with emphasis on conductors, semiconductors, and insulators. Topics range from the interatomic bonds of conductors to the effective atomic charge in conventional semiconductors and magnetic transitions in switching semiconductors. Comprised of 10 chapters, this volume begins with a description of electrical conduction in conductors and semiconductors, metals and alloys, as well as interatomic bon

  19. Solid phase characterization and gas transfers through unsaturated porous media: experimental study and modeling applied diffusion of hydrogen through cement-based materials; Caracterisation de la phase solide et transferts de gaz dans les milieux poreux insatures: etude experimentale et modelisation appliquees a la diffusion de l'hydrogene dans les materiaux cimentaires

    Vu, T.H.


    This thesis documents the relationship between the porous microstructure of cement based materials and theirs gaseous diffusivity properties relative to the aqueous phase location and the global saturation level of the material. The materials studied are cement pastes and mortars. To meet the thesis objective, the materials are characterized in detail by means of several experimental methods: mercury intrusion porosimetry, water porosimetry, thermo-poro-metry, nitrogen sorption and water desorption. In addition, diffusion tests realized on materials maintained in controlled humidity chambers allow obtaining the effective hydrogen diffusivity as function of the microstructure and the saturation state of material with a gas chromatography. The experimental results are then used as a data base that is compared to a modeling approach. The model developed consists of a combination of ordinary diffusion (Fick regime) and Knudsen diffusion of hydrogen. The model also accounts for the effects of the liquid curtains, the impact of tortuosity on gas diffusion, and the saturation level of the porous system. (author)

  20. Ionic liquids in solid-phase microextraction: a review.

    Ho, Tien D; Canestraro, Anthony J; Anderson, Jared L


    Solid-phase microextraction (SPME) has undergone a surge in popularity within the field of analytical chemistry in the past two decades since its introduction. Owing to its nature of extraction, SPME has become widely known as a quick and cost-effective sample preparation technique. Although SPME has demonstrated extraordinary versatility in sampling capabilities, the technique continues to experience a tremendous growth in innovation. Presently, increasing efforts have been directed towards the engineering of novel sorbent material in order to expand the applicability of SPME for a wider range of analytes and matrices. This review highlights the application of ionic liquids (ILs) and polymeric ionic liquids (PILs) as innovative sorbent materials for SPME. Characterized by their unique physico-chemical properties, these compounds can be structurally-designed to selectively extract target analytes based on unique molecular interactions. To examine the advantages of IL and PIL-based sorbent coatings in SPME, the field is reviewed by gathering available experimental data and exploring the sensitivity, linear calibration range, as well as detection limits for a variety of target analytes in the methods that have been developed.

  1. Materials System for Intermediate Temperature Solid Oxide Fuel Cell

    Uday B. Pal; Srikanth Gopalan


    AC complex impedance spectroscopy studies were conducted between 600-800 C on symmetrical cells that employed strontium-and-magnesium-doped lanthanum gallate electrolyte, La{sub 0.9}Sr{sub 0.1}Ga{sub 0.8}Mg{sub 0.2}O{sub 3} (LSGM). The objective of the study was to identify the materials system for fabrication and evaluation of intermediate temperature (600-800 C) solid oxide fuel cells (SOFCs). The slurry-coated electrode materials had fine porosity to enhance catalytic activity. Cathode materials investigated include La{sub 1-x}Sr{sub x}MnO{sub 3} (LSM), LSCF (La{sub 1-x}Sr{sub x}Co{sub y}Fe{sub 1-y}O{sub 3}), a two-phase particulate composite consisting of LSM-doped-lanthanum gallate (LSGM), and LSCF-LSGM. The anode materials were Ni-Ce{sub 0.85}Gd{sub 0.15}O{sub 2} (Ni-GDC) and Ni-Ce{sub 0.6}La{sub 0.4}O{sub 2} (Ni-LDC) composites. Experiments conducted with the anode materials investigated the effect of having a barrier layer of GDC or LDC in between the LSGM electrolyte and the Ni-composite anode to prevent adverse reaction of the Ni with lanthanum in LSGM. For proper interpretation of the beneficial effects of the barrier layer, similar measurements were performed without the barrier layer. The ohmic and the polarization resistances of the system were obtained over time as a function of temperature (600-800 C), firing temperature, thickness, and the composition of the electrodes. The study revealed important details pertaining to the ohmic and the polarization resistances of the electrode as they relate to stability and the charge-transfer reactions that occur in such electrode structures.

  2. Nanocrystalline cerium oxide materials for solid fuel cell systems

    Brinkman, Kyle S


    Disclosed are solid fuel cells, including solid oxide fuel cells and PEM fuel cells that include nanocrystalline cerium oxide materials as a component of the fuel cells. A solid oxide fuel cell can include nanocrystalline cerium oxide as a cathode component and microcrystalline cerium oxide as an electrolyte component, which can prevent mechanical failure and interdiffusion common in other fuel cells. A solid oxide fuel cell can also include nanocrystalline cerium oxide in the anode. A PEM fuel cell can include cerium oxide as a catalyst support in the cathode and optionally also in the anode.

  3. Phase coexistence in ferroelectric solid solutions: Formation of monoclinic phase with enhanced piezoelectricity

    Xiaoyan Lu


    Full Text Available Phase morphology and corresponding piezoelectricity in ferroelectric solid solutions were studied by using a phenomenological theory with the consideration of phase coexistence. Results have shown that phases with similar energy potentials can coexist, thus induce interfacial stresses which lead to the formation of adaptive monoclinic phases. A new tetragonal-like monoclinic to rhombohedral-like monoclinic phase transition was predicted in a shear stress state. Enhanced piezoelectricity can be achieved by manipulating the stress state close to a critical stress field. Phase coexistence is universal in ferroelectric solid solutions and may provide a way to optimize ultra-fine structures and proper stress states to achieve ultrahigh piezoelectricity.

  4. Solid electrolyte material manufacturable by polymer processing methods

    Singh, Mohit; Gur, Ilan; Eitouni, Hany Basam; Balsara, Nitash Pervez


    The present invention relates generally to electrolyte materials. According to an embodiment, the present invention provides for a solid polymer electrolyte material that is ionically conductive, mechanically robust, and can be formed into desirable shapes using conventional polymer processing methods. An exemplary polymer electrolyte material has an elastic modulus in excess of 1.times.10.sup.6 Pa at 90 degrees C. and is characterized by an ionic conductivity of at least 1.times.10.sup.-5 Scm-1 at 90 degrees C. An exemplary material can be characterized by a two domain or three domain material system. An exemplary material can include material components made of diblock polymers or triblock polymers. Many uses are contemplated for the solid polymer electrolyte materials. For example, the present invention can be applied to improve Li-based batteries by means of enabling higher energy density, better thermal and environmental stability, lower rates of self-discharge, enhanced safety, lower manufacturing costs, and novel form factors.

  5. Phase transformations, stability, and materials interactions

    Morris, J.W. Jr.; Brewer, L.; Cost, J.R.; Shewmon, P.


    The proceedings of the Materials Sciences Workshop on Phase Transformations, Stability, and Materials Interactions are divided into sections according to the following topics: (I) workshop scope and priorities; (II) study group reports--ERDA mission needs; (III) study group reports--technical area research priorities. (SDF)

  6. Solid-phase techniques in blood transfusion serology.

    Beck, M L; Plapp, F V; Sinor, L T; Rachel, J M


    For nearly a century, erythrocyte agglutination has persisted as the most widely used method for the demonstration of antigen-antibody reaction in immunohematology. So far, no other system has been developed which can match its simplicity, versatility, and general reliability. The major disadvantage of agglutination reactions is the lack of an objective endpoint, which has severely hindered attempts to automate routine pretransfusion tests. To overcome this problem, we have designed a series of solid-phase assays for ABO and Rh grouping, antibody screening, compatibility, and hepatitis tests. Each of these solid-phase assays shares a common endpoint of red cell adherence, which is easily interpreted visually or spectrophotometrically. Computer interface permits the automatic interpretation and recording of results. We believe this solid-phase system should finally bring the blood bank laboratory into the age of automation.

  7. Kinetic Processes Crystal Growth, Diffusion, and Phase Transformations in Materials

    Jackson, Kenneth A


    The formation of solids is governed by kinetic processes, which are closely related to the macroscopic behaviour of the resulting materials. With the main focus on ease of understanding, the author begins with the basic processes at the atomic level to illustrate their connections to material properties. Diffusion processes during crystal growth and phase transformations are examined in detail. Since the underlying mathematics are very complex, approximation methods typically used in practice are the prime choice of approach. Apart from metals and alloys, the book places special emphasis on th

  8. Preparation of Firefighting Hood for Cooling for Phase Change Materials

    Shu Hwa Lin


    Full Text Available There are two types of Phase Change Materials (PCMs which have been developed and adopted in textiles: heat (energy released and cool (energy absorbed. This paper discusses current PCM applications and explores future applications in firefighting gear. Phase change materials are considered latent heat storage units because as they change phase from solid to liquid, liquid to gas and vice versa, energy in the form of heat is absorbed or released. The goal of PCM textiles is to create reusable energy to maintain body temperature, as well as to optimize the performance of protective wear such as hoods. When the wearer’s body temperature increases or decreases, the PCMs applied to the fabric will change state helping to regulate the wearer’s body temperature by providing warmth or cooling. Maintaining a stable body temperature can improve working conditions and comfort.

  9. Preparation of Firefighting Hood for Cooling For Phase Change Materials

    Shu Hwa Lin


    Full Text Available There are two types of Phase Change Materials (PCMs which have been developed and adopted in textiles: heat (energy released and cool (energy absorbed. This paper discusses current PCM applications and explores future applications in firefighting gear. Phase change materials are considered latent heat storage units because as they change phase from solid to liquid, liquid to gas and vice versa, energy in the form of heat is absorbed or released. The goal of PCM textiles is to create reusable energy to maintain body temperature, as well as to optimize the performance of protective wear such as hoods. When the wearer’s body temperature increases or decreases, the PCMs applied to the fabric will change state helping to regulate the wearer’s body temperature by providing warmth or cooling. Maintaining a stable body temperature can improve working conditions and comfort.

  10. Solid State Ionics Advanced Materials for Emerging Technologies

    Chowdari, B. V. R.; Careem, M. A.; Dissanayake, M. A. K. L.; Rajapakse, R. M. G.; Seneviratne, V. A.


    Keynote lecture. Challenges and opportunities of solid state ionic devices / W. Weppner -- pt. I. Ionically conducting inorganic solids. Invited papers. Multinuclear NMR studies of mass transport of phosphoric acid in water / J. R. P. Jayakody ... [et al.]. Crystalline glassy and polymeric electrolytes: similarities and differences in ionic transport mechanisms / J.-L. Souquet. 30 years of NMR/NQR experiments in solid electrolytes / D. Brinkmann. Analysis of conductivity and NMR measurements in Li[symbol]La[symbol]TiO[symbol] fast Li[symbol] ionic conductor: evidence for correlated Li[symbol] motion / O. Bohnké ... [et al.]. Transport pathways for ions in disordered solids from bond valence mismatch landscapes / S. Adams. Proton conductivity in condensed phases of water: implications on linear and ball lightning / K. Tennakone -- Contributed papers. Proton transport in nanocrystalline bioceramic materials: an investigative study of synthetic bone with that of natural bone / H. Jena, B. Rambabu. Synthesis and properties of the nanostructured fast ionic conductor Li[symbol]La[symbol]TiO[symbol] / Q. N. Pham ... [et al.]. Hydrogen production: ceramic materials for high temperature water electrolysis / A. Hammou. Influence of the sintering temperature on pH sensor ability of Li[symbol]La[symbol]TiO[symbol]. Relationship between potentiometric and impedance spectroscopy measurements / Q. N. Pham ... [et al.]. Microstructure chracterization and ionic conductivity of nano-sized CeO[symbol]-Sm[symbol]O[symbol] system (x=0.05 - 0.2) prepared by combustion route / K. Singh, S. A. Acharya, S. S. Bhoga. Red soil in Northern Sri Lanka is a natural magnetic ceramic / K. Ahilan ... [et al.]. Neutron scattering of LiNiO[symbol] / K. Basar ... [et al.]. Preparation and properties of LiFePO[symbol] nanorods / L. Q. Mai ... [et al.]. Structural and electrochemical properties of monoclinic and othorhombic MoO[symbol] phases / O. M. Hussain ... [et al.]. Preparation of Zircon (Zr


    Yu-ying Li; Jia-song He


    Solid phase transition of the a form crystals to the β form crystals in syndiotactic polystyrene (sPS) samples has occurred in supercritical CO2. This transformation is different from those detected under other conditions. The effects of some factors (e.g. time, temperature, and pressure) on the solid phase transformation of sPS in supercritical CO2 were analyzed in detail. Experimental results show that longer time, higher temperature or higher pressure favors the transformation of the α form crystals to the β form crystals.

  12. Solid-State Explosive Reaction for Nanoporous Bulk Thermoelectric Materials.

    Zhao, Kunpeng; Duan, Haozhi; Raghavendra, Nunna; Qiu, Pengfei; Zeng, Yi; Zhang, Wenqing; Yang, Jihui; Shi, Xun; Chen, Lidong


    High-performance thermoelectric materials require ultralow lattice thermal conductivity typically through either shortening the phonon mean free path or reducing the specific heat. Beyond these two approaches, a new unique, simple, yet ultrafast solid-state explosive reaction is proposed to fabricate nanoporous bulk thermoelectric materials with well-controlled pore sizes and distributions to suppress thermal conductivity. By investigating a wide variety of functional materials, general criteria for solid-state explosive reactions are built upon both thermodynamics and kinetics, and then successfully used to tailor material's microstructures and porosity. A drastic decrease in lattice thermal conductivity down below the minimum value of the fully densified materials and enhancement in thermoelectric figure of merit are achieved in porous bulk materials. This work demonstrates that controlling materials' porosity is a very effective strategy and is easy to be combined with other approaches for optimizing thermoelectric performance. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Observation of Solid-Solid Phase Transitions in Ramp-Compressed Aluminum

    Polsin, D. N.; Boehly, T. R.; Delettrez, J. A.; Gregor, M. C.; McCoy, C. A.; Henderson, B.; Fratanduono, D. E.; Smith, R.; Kraus, R.; Eggert, J. H.; Collins, R.; Coppari, F.; Celliers, P. M.


    We present results of experiments using x-ray diffraction to study the crystalline structure of solid aluminum compressed up to 500 GPa. Aluminum is of interest because it is frequently used as a standard material in high-pressure compression experiments. At ambient pressure and temperature, Al is a face-centered cubic close-packed crystal and has been observed to transform to hexagonal close-packed (hcp) when compressed to 200GPa in a diamond anvil cell. It is predicted to transform from hcp to body-centered cubic when compressed to 315GPa. Laser-driven ramp waves will be used to compress Al to various constant-pressure states. The goal is to investigate the Al phase diagram along its isentrope, i.e., at temperatures 1000K and pressures ranging from 200 to 500 GPa. X-ray diffraction will be used to measure the crystalline structure of the compressed Al and observe the transformations that occur at various pressures. This material is based upon work supported by the Department of Energy National Nuclear Security Administration under Award Number DE-NA0001944.

  14. Understanding solids: the science of materials

    Tilley, Richard J. D.


    This edition contains new sections on the use of computing methods to solve materials problems and has been thoroughly updated to include the many developments and advances made in the past 10 years, e.g.  batteries, solar cells, lighting technology, laser...

  15. The use of lipids as phase change materials for thermal energy storage

    Phase change materials (PCMs) are substances capable of absorbing and releasing large 2 amounts of thermal energy (heat or cold) as latent heat over constant temperature as they 3 undergo a change in state of matter (phase transition), commonly, between solid and 4 liquid phases. Since the late 194...

  16. Soft solids a primer to the theoretical mechanics of materials

    Freed, Alan D


    This textbook presents the physical principles pertinent to the mathematical modeling of soft materials used in engineering practice, including both man-made materials and biological tissues. It is intended for seniors and masters-level graduate students in engineering, physics, or applied mathematics. It will also be a valuable resource for researchers working in mechanics, biomechanics, and other fields where the mechanical response of soft solids is relevant.   Soft Solids: A Primer to the Theoretical Mechanics of Materials is divided into two parts. Part I introduces the basic concepts needed to give both Eulerian and Lagrangian descriptions of the mechanical response of soft solids. Part II presents two distinct theories of elasticity and their associated theories of viscoelasticity. Seven boundary-value problems are studied over the course of the book, each pertaining to an experiment used to characterize materials. These problems are discussed at the end of each chapter, giving students the opportunit...

  17. The Effects of Solid Phase Additives on Sintering Properties of Alumina Bioceramic

    WANG Xin-yu; LI Shi-pu; HE Jian-hua; JIANG Xin; LI Jian-hua


    In order to reduce the sintering temperature and improve the preparing conditions of alumina bioceramics,the Mg-Zr-Y composite solid phase additives were added into high purity Al2O3 micro-powder by chemical coprecipitation method.The powder was shaped under 200MPa cold isostatic pressure,and then the biscuits were sintered at 1600℃ under normal pressure.The sintered alumina materials were tested and the sintering mechanism was discussed.The results show that physical properties of the material were improved comparatively.The Mg-Zr-Y composite solid additives could promote the sintering of alumina bioceramics and the mechanism is solid phase sintering.

  18. Collection-efficient, axisymmetric vacuum sublimation module for the purification of solid materials.

    May, Michael; Paul, Elizabeth; Katovic, Vladimir


    A vacuum sublimation module of axisymmetric geometry was developed and employed to purify solid-phase materials. The module provides certain practical advantages and it comprises: a metering valve, glass collector, glass lower body, main seal, threaded bushing, and glass internal cartridge (the latter to contain starting material). A complementary process was developed to de-solvate, sublime, weigh, and collect solid chemical materials exemplified by oxalic acid, ferrocene, pentachlorobenzene, chrysene, and urea. The oxalic acid sublimate was analyzed by titration, melting range, Fourier Transform Infrared (FT-IR) Spectroscopy, cyclic voltammetry, and its (aqueous phase) electrolytically generated gas. The analytical data were consistent with a high-purity, anhydrous oxalic acid sublimate. Cyclic voltammograms of 0.11 mol. % oxalic acid in water displayed a 2.1 V window on glassy carbon electrode beyond which electrolytic decomposition occurs. During module testing, fifteen relatively pure materials were sublimed with (energy efficient) passive cooling and the solid-phase recovery averaged 95 mass %. Key module design features include: compact vertical geometry, low-angle conical collector, uniformly compressed main seal, modest power consumption, transparency, glovebox compatibility, cooling options, and preferential conductive heat transfer. To help evaluate the structural (module) heat transfer, vertical temperature profiles along the dynamically evacuated lower body were measured versus electric heater power: for example, an input of 18.6 W generated a temperature 443-K at the bottom. Experimental results and engineering calculations indicate that during sublimation, solid conduction is the primary mode of heat transfer to the starting material.

  19. Collection-efficient, axisymmetric vacuum sublimation module for the purification of solid materials

    May, Michael; Paul, Elizabeth; Katovic, Vladimir


    A vacuum sublimation module of axisymmetric geometry was developed and employed to purify solid-phase materials. The module provides certain practical advantages and it comprises: a metering valve, glass collector, glass lower body, main seal, threaded bushing, and glass internal cartridge (the latter to contain starting material). A complementary process was developed to de-solvate, sublime, weigh, and collect solid chemical materials exemplified by oxalic acid, ferrocene, pentachlorobenzene, chrysene, and urea. The oxalic acid sublimate was analyzed by titration, melting range, Fourier Transform Infrared (FT-IR) Spectroscopy, cyclic voltammetry, and its (aqueous phase) electrolytically generated gas. The analytical data were consistent with a high-purity, anhydrous oxalic acid sublimate. Cyclic voltammograms of 0.11 mol. % oxalic acid in water displayed a 2.1 V window on glassy carbon electrode beyond which electrolytic decomposition occurs. During module testing, fifteen relatively pure materials were sublimed with (energy efficient) passive cooling and the solid-phase recovery averaged 95 mass %. Key module design features include: compact vertical geometry, low-angle conical collector, uniformly compressed main seal, modest power consumption, transparency, glovebox compatibility, cooling options, and preferential conductive heat transfer. To help evaluate the structural (module) heat transfer, vertical temperature profiles along the dynamically evacuated lower body were measured versus electric heater power: for example, an input of 18.6 W generated a temperature 443-K at the bottom. Experimental results and engineering calculations indicate that during sublimation, solid conduction is the primary mode of heat transfer to the starting material.

  20. A review on solid phase extraction of actinides and lanthanides with amide based extractants.

    Ansari, Seraj A; Mohapatra, Prasanta K


    Solid phase extraction is gaining attention from separation scientists due to its high chromatographic utility. Though both grafted and impregnated forms of solid phase extraction resins are popular, the later is easy to make by impregnating a given organic extractant on to an inert solid support. Solid phase extraction on an impregnated support, also known as extraction chromatography, combines the advantages of liquid-liquid extraction and the ion exchange chromatography methods. On the flip side, the impregnated extraction chromatographic resins are less stable against leaching out of the organic extractant from the pores of the support material. Grafted resins, on the other hand, have a higher stability, which allows their prolong use. The goal of this article is a brief literature review on reported actinide and lanthanide separation methods based on solid phase extractants of both the types, i.e., (i) ligand impregnation on the solid support or (ii) ligand functionalized polymers (chemically bonded resins). Though the literature survey reveals an enormous volume of studies on the extraction chromatographic separation of actinides and lanthanides using several extractants, the focus of the present article is limited to the work carried out with amide based ligands, viz. monoamides, diamides and diglycolamides. The emphasis will be on reported applied experimental results rather than on data pertaining fundamental metal complexation. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Laser-induced solid-solid phase transition in As under pressure: a theoretical prediction

    Zijlstra, Eeuwe S; Huntemann, Nils; Garcia, Martin E [Theoretische Physik, Universitaet Kassel, Heinrich-Plett-Strasse 40, 34132 Kassel (Germany)], E-mail:


    In arsenic, a pressure-induced solid-solid phase transition from the A7 into the simple cubic structure has been experimentally demonstrated (Beister et al 1990 Phys. Rev. B 41 5535). In this paper, we present calculations, which predict that this phase transition can also be induced by an ultrashort laser pulse in As under pressure. In addition, calculations for the pressure-induced phase transition are presented. Using density functional theory in the generalized gradient approximation, we found that the pressure-induced phase transition takes place at 26.3 GPa and is accompanied by a volume change {delta}V=0.5 a{sub 0}{sup 3} atom{sup -1}. The laser-induced phase transition is predicted for an applied pressure of 23.8 GPa and an absorbed laser energy of 2.8 mRy atom{sup -1}.

  2. Understanding solids the science of materials

    Tilley, Richard J D


    A modern introduction to the subject taking a unique integrated approach designed to appeal to both science and engineering students. Covering a broad spectrum of topics, this book includes numerous up-to-date examples of real materials with relevant applications and a modern treatment of key concepts. The science bias allows this book to be equally accessible to engineers, chemists and physicists. * Carefully structured into self-contained bite-sized chapters to enhance student understanding * Questions have been designed to reinforce the concepts presented * Includes coverage of radioactivit

  3. Applied solid state science advances in materials and device research

    Wolfe, Raymond


    Applied Solid State Science: Advances in Materials and Device Research, Volume 1 presents articles about junction electroluminescence; metal-insulator-semiconductor (MIS) physics; ion implantation in semiconductors; and electron transport through insulating thin films. The book describes the basic physics of carrier injection; energy transfer and recombination mechanisms; state of the art efficiencies; and future prospects for light emitting diodes. The text then discusses solid state spectroscopy, which is the pair spectra observed in gallium phosphide photoluminescence. The extensive studies

  4. Solid-phase oligosaccharide and glycopeptide synthesis using glycosynthases

    Tolborg, Jakob Fjord; Petersen, Lars; Jensen, Knud Jørgen;


    Enzymatic approaches for the preparation of oligosaccharides are interesting alternatives to traditional chemical synthesis, the main advantage being the regio- and stereoselectivity offered without the need for protecting groups. The use of solid-phase techniques offers easy workup procedures an...

  5. Solid and solution phase combinatorial synthesis of ureas

    Nieuwenhuijzen, JW; Conti, PGM; Ottenheijm, HCJ; Linders, JTM


    An efficient parallel synthesis of ureas based on amino acids is described, both in solution and on solid phase. 1,1'-Carbonylbisbenzotriazole 2 is used as the coupling reagent. The ureas 5 and 10 were obtained in high yield (80-100%) and purity (71-97%). (C) 1998 Elsevier Science Ltd. All rights re

  6. Solid Phase Synthesis of Ethyl β-Substituted Indolepropionates

    刘占祥; 阮秀秀; 黄宪


    A facile solid phase synthesis of ethyl β-substituted indolepropionates is reported. Condensation between indole, polymer-supported cyclic malonic acid ester and aldehyde yielded the trimolecular adducts, which was cleaved by pyridine/EtOH to release the final products in good yield with high purity.

  7. Recent Approaches Toward Solid Phase Synthesis of β-Lactams

    Mandal, Bablee; Ghosh, Pranab; Basu, Basudeb

    Since the discovery of penicillin in 1929, β-lactam antibiotics have been recognized as potentially chemotherapeutic drugs of incomparable effectiveness, conjugating a broad spectrum of activity with very low toxicity. The primary motif azetidin-2-one ring (β-lactam) has been considered as specific pharmacophores and scaffolds. With the advent of combinatorial chemistry and automated parallel synthesis coupled with ample interests from the pharmaceutical industries, recent trends have been driven mostly by adopting solid phase techniques and polymer-supported synthesis of β-lactams. The present survey will present an overview of the developments on the polymer-supported and solid phase techniques for the preparation of β-lactam ring or β-lactam containing antibiotics published over the last decade. Both unsubstituted and substitutions with different functional groups at various positions of β-lactams have been synthesized using solid phase technology. However, Wang resin and application of Staudinger [2+2] cycloaddition reaction have remained hitherto the major choice. It may be expected that other solid phase approaches involving different resins would be developed in the coming years.

  8. Solid-phase synthesis of 3-amino-2-pyrazolines

    Lyngsø, Lars O.; Nielsen, John


    The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to α,β-unsaturated nitriles followed by cyclization yields 3-amino-2-pyrazolines. Acylation or sulfonation of the free amino-group yields a 24 member library of 3-amino-2- pyrazolines....

  9. Solid-phase synthesis of 3-amino-2-pyrazolines

    Nielsen, John


    The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to alpha,beta-unsaturated nitriles followed by cyclization yields 3-amino-2-pyrazolines. Acylation or sulfonation of the free amino-group yields a 24 member library of 3-amino-2...

  10. Solid-phase synthesis of complex and pharmacologically interesting heterocycles

    Nielsen, Thomas Eiland


    Efficient routes for the creation of heterocycles continue to be one of the primary goals for solid-phase synthesis. Recent advances in this field rely most notably on transition-metal-catalysis and N-acyliminium chemistry to mediate a range of cyclization processes for the generation of compounds...

  11. Solid-phase synthesis of 3-amino-2-pyrazolines

    Lyngsø, Lars O.; Nielsen, John


    The development of a solid-phase synthesis of 3-amino-2-pyrazolines is described. Conjugate addition of hydrazines to α,β-unsaturated nitriles followed by cyclization yields 3-amino-2-pyrazolines. Acylation or sulfonation of the free amino-group yields a 24 member library of 3-amino-2- pyrazolines....

  12. Solid-phase synthesis of complex and pharmacologically interesting heterocycles

    Nielsen, Thomas Eiland


    Efficient routes for the creation of heterocycles continue to be one of the primary goals for solid-phase synthesis. Recent advances in this field rely most notably on transition-metal-catalysis and N-acyliminium chemistry to mediate a range of cyclization processes for the generation of compounds...

  13. Solid-phase microextraction for the analysis of biological samples

    Theodoridis, G; Koster, EHM; de Jong, GJ


    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a num

  14. Solid Phase Characterization of Tank 241-C-105 Grab Samples

    Ely, T. M. [Washington River Protection Solutions LLC, Richland, WA (United States); LaMothe, M. E. [Washington River Protection Solutions LLC, Richland, WA (United States); Lachut, J. S. [Washington River Protection Solutions LLC, Richland, WA (United States)


    The solid phase characterization (SPC) of three grab samples from single-shell Tank 241-C-105 (C-105) that were received at the laboratory the week of October 26, 2015, has been completed. The three samples were received and broken down in the 11A hot cells.

  15. Sensitive and fast mutation detection by solid phase chemical cleavage

    Hansen, Lise Lotte; Justesen, Just; Kruse, Torben A


    We have developed a solid phase chemical cleavage method (SpCCM) for screening large DNA fragments for mutations. All reactions can be carried out in microtiterwells from the first amplification of the patient (or test) DNA through the search for mutations. The reaction time is significantly...

  16. Homogeneity studies in reference materials with Zeeman solid sampling GFAAS

    Mohl, C.; Stoeppler, M.; Grobecker, K.H.


    The homogeneity of lead and cadmium in reference materials was investigated by solid sampling GFAAS. The following materials were comparatively analyzed: Standard reference materials from NBS, Washington 1567 wheat flour, 1568 rice flour and 1577a bovine liver, certified reference materials from BCR, Brussels, No 63 milk powder, No 184 bovine muscle, No 185 bovine liver, No 186 pig kidney, No 189 wholemeal flour, No 191 brown bread and a whole fish (dab) homogenate from the environmental specimen bank in the FRG. The results are remarkably different for the investigated materials.

  17. Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

    Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko


    Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

  18. Phase field modeling of flexoelectricity in solid dielectrics

    Chen, H. T.; Zhang, S. D.; Soh, A. K.; Yin, W. Y.


    A phase field model is developed to study the flexoelectricity in nanoscale solid dielectrics, which exhibit both structural and elastic inhomogeneity. The model is established for an elastic homogeneous system by taking into consideration all the important non-local interactions, such as electrostatic, elastic, polarization gradient, as well as flexoelectric terms. The model is then extended to simulate a two-phase system with strong elastic inhomogeneity. Both the microscopic domain structures and the macroscopic effective piezoelectricity are thoroughly studied using the proposed model. The results obtained show that the largest flexoelectric induced polarization exists at the interface between the matrix and the inclusion. The effective piezoelectricity is greatly influenced by the inclusion size, volume fraction, elastic stiffness, and the applied stress. The established model in the present study can provide a fundamental framework for computational study of flexoelectricity in nanoscale solid dielectrics, since various boundary conditions can be easily incorporated into the phase field model.

  19. Caloric materials near ferroic phase transitions

    Moya, X.; Kar-Narayan, S.; Mathur, N. D.


    A magnetically, electrically or mechanically responsive material can undergo significant thermal changes near a ferroic phase transition when its order parameter is modified by the conjugate applied field. The resulting magnetocaloric, electrocaloric and mechanocaloric (elastocaloric or barocaloric) effects are compared here in terms of history, experimental method, performance and prospective cooling applications.

  20. Distribution of Dechlorinating Bacteria between the Aqueous and Solid Phases

    Cápiro, N. L.; Hatt, J. K.; Wang, Y.; Loeffler, F. E.; Pennell, K. D.


    Microbial monitoring of aquifers relies on nucleic acid biomarker analysis, which is typically performed with biomass recovered from groundwater samples; however, it is unclear what fraction of the target population(s) is associated with groundwater (i.e., planktonic cells) or is attached to solid phases (i.e., biofilms). Understanding how the titer of target organism(s) in groundwater correlates with the true cell titers of the target organism in the aquifer (i.e., planktonic plus attached cells) is critical for a meaningful interpretation of the data, the prediction of bioremediation performance, and the implementation of site management strategies. To evaluate the distribution of active cells between resident solid phase and the aqueous phase, one-dimensional columns were packed under water-saturated conditions with Bio-Dechlor INOCULUM, a PCE-to ethene-dechlorinating bacterial consortium containing both multiple Dehalococcoides (Dhc) strains and Geobacter lovleyi strain SZ (GeoSZ). The columns were packed with two distinct solid matrices: a low organic content sandy Federal Fine Ottawa soil or Appling soil with higher organic matter content. Influent reduced mineral salts medium supplied at a groundwater pore-water velocity of 0.3 m/day contained both 10 mM lactate as electron donor and 0.33 mM PCE as electron acceptor. Routine collection of biomass from column side ports and effluent samples measured the titers of target cells in the aqueous phase and determined when steady state conditions had been reached. A second set of column experiments evaluated delivery and filtration effects by the solid matrix (i.e., Federal Fine Ottawa sand versus Appling soil) under the same conditions except that electron donor or acceptor were omitted (no growth conditions). Quantitative real-time PCR (qPCR) analysis using Dhc and GeoSZ 16S rRNA gene-targeted primer and probe sets determined the planktonic cell counts, and destructive sampling of the columns allowed measurement

  1. Solid rocket motor fire tests: Phases 1 and 2

    Chang, Yale; Hunter, Lawrence W.; Han, David K.; Thomas, Michael E.; Cain, Russell P.; Lennon, Andrew M.


    JHU/APL conducted a series of open-air burns of small blocks (3 to 10 kg) of solid rocket motor (SRM) propellant at the Thiokol Elkton MD facility to elucidate the thermal environment under burning propellant. The propellant was TP-H-3340A for the STAR 48 motor, with a weight ratio of 71/18/11 for the ammonium perchlorate, aluminum, and HTPB binder. Combustion inhibitor applied on the blocks allowed burning on the bottom and/or sides only. Burns were conducted on sand and concrete to simulate near-launch pad surfaces, and on graphite to simulate a low-recession surface. Unique test fixturing allowed propellant self-levitation while constraining lateral motion. Optics instrumentation consisted of a longwave infrared imaging pyrometer, a midwave spectroradiometer, and a UV/visible spectroradiometer. In-situ instrumentation consisted of rod calorimeters, Gardon gauges, elevated thermocouples, flush thermocouples, a two-color pyrometer, and Knudsen cells. Witness materials consisted of yttria, ceria, alumina, tungsten, iridium, and platinum/rhodium. Objectives of the tests were to determine propellant burn characteristics such as burn rate and self-levitation, to determine heat fluxes and temperatures, and to carry out materials analyses. A summary of qualitative results: alumina coated almost all surfaces, the concrete spalled, sand moisture content matters, the propellant self-levitated, the test fixtures worked as designed, and bottom-burning propellant does not self-extinguish. A summary of quantitative results: burn rate averaged 1.15 mm/s, thermocouples peaked at 2070 C, pyrometer readings matched MWIR data at about 2400 C, the volume-averaged plume temperatures were 2300-2400 C with peaks of 2400-2600 C, and the heat fluxes peaked at 125 W/cm2. These results are higher than other researchers' measurements of top-burning propellant in chimneys, and will be used, along with Phase 3 test results, to analyze hardware response to these environments, including General

  2. SRM (Solid Rocket Motor) propellant and polymer materials structural modeling

    Moore, Carleton J.


    The following investigation reviews and evaluates the use of stress relaxation test data for the structural analysis of Solid Rocket Motor (SRM) propellants and other polymer materials used for liners, insulators, inhibitors, and seals. The stress relaxation data is examined and a new mathematical structural model is proposed. This model has potentially wide application to structural analysis of polymer materials and other materials generally characterized as being made of viscoelastic materials. A dynamic modulus is derived from the new model for stress relaxation modulus and is compared to the old viscoelastic model and experimental data.

  3. Method of investigation of deformations of solids of incompressible materials

    Abdrakhmanova, A. I.; Garifullin, I. R.; Sultanov, L. U.


    The aim of this work is development mathematical models, algorithm for the investigation stress-strain state of elastic solids, taking into account the incompressibility materials. The constitutive equations are received using a potential energy of deformations. The system of the linear algebraic equations is received by linearization of a resolving equation. The penalty method is applied for a modelling of the incompressibility of the material. The finite element method is used for numerical solution of the problems.

  4. PVD materials for electrochromic all-solid-state devices

    Ottermann, Clemens R.; Segner, Johannes G.; Bange, Klaus


    The electrochromic properties of all solid state devices (ASSDs) are strongly defined by thin film materials used as well as the method of deposition. Various thin film materials deposited by evaporation and sputtering are described serving as electrode, reflector, electrolyte, storage medium, or electrochromic film in ASSD. The impact of process parameters upon the device functionality is shown. In addition, the long-term stability of ASSDs for the different thin film systems is reported.

  5. Solid phase synthesis of N/Fe co-doped TiO2 materials and visible light degradation of puerarin%甲基橙废水的均相催化氧化降解研究

    赵彦巧; 李建颖; 王文忠


    考察了温度,pH,H2O2、CuSO4和FeSO4添加量对催化氧化降解甲基橙的影响.结果表明:CuSO4和FeSO4对甲基橙的降解存在协同催化作用,150 mL 质量浓度为1.5 g/L甲基橙模拟废水的最佳降解条件为:温度60 ℃、pH= 3.0、过氧化氢3.75 mL、硫酸铜0.75 g、硫酸亚铁0.04 g.%The photocatalytic powdered materials, Fe-doped TiO2(Fe-TiO2) and N, Fe co-doped TiO2 (N/Fe-TiO2) ha-ve been successfully synthesized respectively, through a simple solid-state reaction process. The textural propertiesof the samples are characterized by X-ray diffraction(XRD), ultraviolet visible light spectroscopy(UV-Vis), and X-ray photoelectron spectroscopy (XPS). Moreover, the photodegradation properties of puerarin irradiated under visiblelight on the materials are studied. It clearly shows that N and Fe have been incorporated into the lattice of TiO2.Interestingly, the UV-Vis displays that the adsorption band of N/Fe-TiO2 material shifts to 600 nm. Under theconditions of 20 ℃ and pH=6.5 ,the produced photocatalytic material has pretty high photocatalytic activity on thevisible photodegradation of puerarin, and obeys the first grade reaction kinetics rules. The visible light degradationreaction rate constants of catalysts are as the following sequence: N/Fe-TiO2>TiO2>Fe-TiO2.

  6. Extraction of Pb2+ using Silica from Rice Husks Ash (RHA – Chitosan as Solid Phase

    Hanandayu Widwiastuti


    Full Text Available The existence of lead (Pb compounds in waters can be caused of waste pollution from industrial activities such as dye and battery industries. Lead has toxic characteristic and is able to causing deseases. The levels of Cr(VI can be decreased by methods such as electroplating, oxidation, reduction, and membrane separation. But this methods require high cost and produce a lot of waste. Furthermore, those methods cannot determine the small concentration of Pb2+. Therefore, solid phase extraction is used because it’s a simple method and can be used to preconcentrate Pb2+ ion. The aim of this study is to create solid phase from nature material as an alternative method to determine Pb2+ in water samples. The solid phase is silica from rice husks ash (RHA that was modified using chitosan. To achieve that aim, the optimization of silica : chitosan composition was done. The influence of Pb2+ concentration and citric acid concentration was studied to obtain optimum recovery of Pb2+. Interaction between Pb2+ ion and solid phase silica – chitosan could be estimated based on the result. The result showed the optimum composition of silica : chitosan is 65% silica : 35% chitosan with Cation Exchange Capacity (CEC 0.00455 mek/g. Mass Adsorbed Pb2+for 1 g silica : chitosan 65% is 9.715 mg/g. Optimum recovery of Pb2+ on solid phase extraction is reached at concentration of Pb2+ 10 ppm and citric acid concentration 0.05 M (88.25 % and 81.18 %. This result showed that solid phase extraction using silica – chitosan can be used as an alternative method to determine Pb2+ in water.

  7. Organic Materials Degradation in Solid State Lighting Applications

    Yazdan Mehr, M.


    In this thesis the degradation and failure mechanisms of organic materials in the optical part of LED-based products are studied. The main causes of discoloration of substrate/lens in remote phosphor of LED-based products are also comprehensively investigated. Solid State Lighting (SSL) technology i

  8. Introduction of Materials Science Through Solid State Chemistry.

    Mueller, William M.

    Presented is a report of a program of the American Society for Metals, designed to introduce materials science principles via solid state chemistry into high school chemistry courses. At the time of the inception of this program in the mid-sixties, it was felt that high school students were not being adequately exposed to career opportunities in…

  9. Organic Materials Degradation in Solid State Lighting Applications

    Yazdan Mehr, M.


    In this thesis the degradation and failure mechanisms of organic materials in the optical part of LED-based products are studied. The main causes of discoloration of substrate/lens in remote phosphor of LED-based products are also comprehensively investigated. Solid State Lighting (SSL) technology

  10. Solid-Phase Organic Synthesis and Catalysis: Some Recent Strategies Using Alumina, Silica, and Polyionic Resins

    Basudeb Basu


    Full Text Available Solid-phase organic synthesis (SPOS and catalysis have gained impetus after the seminal discovery of Merrifield’s solid-phase peptide synthesis and also because of wide applicability in combinatorial and high throughput chemistry. A large number of organic, inorganic, or organic-inorganic hybrid materials have been employed as polymeric solid supports to promote or catalyze various organic reactions. This review article provides a concise account on our approaches involving the use of (i alumina or silica, either having doped with metal salts or directly, and (ii polyionic resins to either promote various organic reactions or to immobilize reagents/metal catalysts for subsequent use in hydrogenation and cross-coupling reactions. The reaction parameters, scopes, and limitations, particularly in the context of green chemistry, have been highlighted with pertinent approaches by other groups.

  11. New Cathode Materials for Intermediate Temperature Solid Oxide Fuel Cells

    Allan J. Jacobson


    Operation of SOFCs at intermediate temperatures (500-800 C) requires new combinations of electrolyte and electrode materials that will provide both rapid ion transport across the electrolyte and electrode-electrolyte interfaces and efficient electrocatalysis of the oxygen reduction and fuel oxidation reactions. This project concentrates on materials and issues associated with cathode performance that are known to become limiting factors as the operating temperature is reduced. The specific objectives of the proposed research are to develop cathode materials that meet the electrode performance targets of 1.0 W/cm{sup 2} at 0.7 V in combination with YSZ at 700 C and with GDC, LSGM or bismuth oxide based electrolytes at 600 C. The performance targets imply an area specific resistance of {approx}0.5 {Omega}cm{sup 2} for the total cell. The research strategy is to investigate both established classes of materials and new candidates as cathodes, to determine fundamental performance parameters such as bulk diffusion, surface reactivity and interfacial transfer, and to couple these parameters to performance in single cell tests. The initial choices for study were perovskite oxides based on substituted LaFeO{sub 3} (P1 compositions), where significant data in single cell tests exist at PNNL for example, for La{sub 0.8}Sr{sub 0.2}FeO{sub 3} cathodes on both YSZ and CSO/YSZ. The materials selection was then extended to La{sub 2}NiO{sub 4} compositions (K1 compositions), and then in a longer range task we evaluated the possibility of completely unexplored group of materials that are also perovskite related, the ABM{sub 2}O{sub 5+{delta}}. A key component of the research strategy was to evaluate for each cathode material composition, the key performance parameters, including ionic and electronic conductivity, surface exchange rates, stability with respect to the specific electrolyte choice, and thermal expansion coefficients. In the initial phase, we did this in parallel with

  12. Magnetocaloric materials and first order phase transitions

    Neves Bez, Henrique

    of the properties of such materials.The experimental characterization of these materials is done through various different methods, such as X-ray diffraction, magnetometry, calorimetry, direct measurements of entropy change, capacitance dilatometry, scanning electron microscopy,energy-dispersive X-ray spectrometry......This thesis studies the first order phase transitions of the magnetocaloric materials La0.67Ca0.33MnO3 and La(Fe,Mn,Si)13Hz trying to overcome challenges that these materials face when applied in active magnetic regenerators. The study is done through experimental characterization and modelling...... and magnetocaloric regenerative tests. The magnetic, thermal and structural properties obtained from such measurements are then evaluated through different models, i.e. the Curie-Weiss law, the Bean-Rodbell model, the free electron model and the Debye model.The measured magnetocaloric properties of La0.67Ca0.33MnO3...

  13. Application of solid phase microextraction on dental composite resin analysis.

    Wang, Ven-Shing; Chang, Ta-Yuan; Lai, Chien-Chen; Chen, San-Yue; Huang, Long-Chen; Chao, Keh-Ping


    A direct immersion solid phase microextraction (DI-SPME) method was developed for the analysis of dentin monomers in saliva. Dentine monomers, such as triethylene glycol dimethacrylate (TEGDMA), urethane dimethacrylate (UDMA) and 2,2-bis-[4-(2-hydroxy-3-methacryloyloxypropoxy) phenyl]-propane (Bis-GMA), have a high molecular weight and a low vapor pressure. The polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber with a medium polarity was employed for DI-SPME, and 215 nm of detection wavelength was found to be optimum in the chromatogram of HPLC measurement. The calibration range for DI-SPME was 0.30-300 μg/mL with correlation coefficients (r) greater than 0.998 for each analyte. The DI-SPME method achieved good accuracy (recovery 96.1-101.2%) and precision (2.30-8.15% CV) for both intra- and inter-day assays of quality control samples for three target compounds. Method validation was performed on standards dissolved in blank saliva, and there was no significant difference (p>0.2) between the DI-SPME method and the liquid injection method. However, the detection limit of DI-SPME was as low as 0.03, 0.27 and 0.06 μg/mL for TEGDMA, UDMA and Bis-GMA, respectively. Real sample analyses were performed on commercial dentin products after curing for the leaching measurement. In summary, DI-SPME is a more sensitive method that requires less sample pretreatment procedures to measure the resin materials leached in saliva.

  14. Studies in Solid Phase Peptide Synthesis: A Personal Perspective

    Mitchell, A R


    By the early 1970s it had became apparent that the solid phase synthesis of ribonuclease A could not be generalized. Consequently, virtually every aspect of solid phase peptide synthesis (SPPS) was reexamined and improved during the decade of the 1970s. The sensitive detection and elimination of possible side reactions (amino acid insertion, N{sup {alpha}}-trifluoroacetylation, N{sup {alpha}{var_epsilon}}-alkylation) was examined. The quantitation of coupling efficiency in SPPS as a function of chain length was studied. A new and improved support for SPPS, the 'PAM-resin', was prepared and evaluated. These and many other studies from the Merrifield laboratory and elsewhere increased the general acceptance of SPPS leading to the 1984 Nobel Prize in Chemistry for Bruce Merrifield.

  15. Entransy dissipation minimization for liquid-solid phase change processes


    The liquid-solid phase change process of a simple one-dimensional slab is studied in this paper.By taking entransy dissipation minimization as optimization objective,the optimal external reservoir temperature profiles are derived by using optimal control theory under the condition of a fixed freezing or melting time.The entransy dissipation corresponding to the optimal heat exchange strategies of minimum entransy dissipation is 8/9 of that corresponding to constant reservoir temperature operations,which is independent of all system parameters.The obtained results for entransy dissipation minimization are also compared with those obtained for the optimal heat exchange strategies of minimum entropy generation and constant reservoir temperature operations by numerical examples.The obtained results can provide some theoretical guidelines for the choice of optimal cooling or heating strategy in practical liquid-solid phase change processes.

  16. Semi-automated microwave assisted solid-phase peptide synthesis

    Pedersen, Søren Ljungberg

    with microwaves for SPPS has gained in popularity as it for many syntheses has provided significant improvement in terms of speed, purity, and yields, maybe especially in the synthesis of long and "difficult" peptides. Thus, precise microwave heating has emerged as one new parameter for SPPS, in addition...... to coupling reagents, resins, solvents etc. We have previously reported on microwave heating to promote a range of solid-phase reactions in SPPS. Here we present a new, flexible semi-automated instrument for the application of precise microwave heating in solid-phase synthesis. It combines a slightly modified...... Biotage Initiator microwave instrument, which is available in many laboratories, with a modified semi-automated peptide synthesizer from MultiSynTech. A custom-made reaction vessel is placed permanently in the microwave oven, thus the reactor does not have to be moved between steps. Mixing is achieved...

  17. Indigenous microbial capability in solid manure residues to start-up solid-phase anaerobic digesters.

    Yap, S D; Astals, S; Jensen, P D; Batstone, D J; Tait, S


    Batch solid-phase anaerobic digestion is a technology for sustainable on-farm treatment of solid residues, but is an emerging technology that is yet to be optimised with respect to start-up and inoculation. In the present study, spent bedding from two piggeries (site A and B) were batch digested at total solids (TS) concentration of 5, 10 and 20% at mesophilic (37°C) and thermophilic (55°C) temperatures, without adding an external inoculum. The results showed that the indigenous microbial community present in spent bedding was able to recover the full methane potential of the bedding (140±5 and 227±6L CH4 kgVSfed(-1) for site A and B, respectively), but longer treatment times were required than for digestion with an added external inoculum. Nonetheless, at high solid loadings (i.e. TS level>10%), the digestion performance was affected by chemical inhibition due to ammonia and/or humic acid. Thermophilic temperatures did not influence digestion performance but did increase start-up failure risk. Further, inoculation of residues from the batch digestion to subsequent batch enhanced start-up and achieved full methane potential recovery of the bedding. Inoculation with liquid residue (leachate) was preferred over a solid residue, to preserve treatment capacity for fresh substrate. Overall, the study highlighted that indigenous microbial community in the solid manure residue was capable of recovering full methane potential and that solid-phase digestion was ultimately limited by chemical inhibition rather than lack of suitable microbial community. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. Chromatography, solid-phase extraction, and capillary electrochromatography with MIPs.

    Tóth, Blanka; Horvai, George


    Most analytical applications of molecularly imprinted polymers are based on their selective adsorption properties towards the template or its analogs. In chromatography, solid phase extraction and electrochromatography this adsorption is a dynamic process. The dynamic process combined with the nonlinear adsorption isotherm of the polymers and other factors results in complications which have limited the success of imprinted polymers. This chapter explains these problems and shows many examples of successful applications overcoming or avoiding the problems.

  19. Oscillatory burning of solid propellants including gas phase time lag.

    T'Ien, J. S.


    An analysis has been performed for oscillatory burning of solid propellants including gas phase time lag. The gaseous flame is assumed to be premixed and laminar with a one-step overall chemical reaction. The propellant is assumed to decompose according to the Arrenhius Law, with no condensed phase reaction. With this model, strong gas phase resonance has been found in certain cases at the characteristic gas-phase frequencies, but the peaking of the acoustic admittance is in the direction favoring the damping of pressure waves. At still higher frequencies, moderate wave-amplifying ability was found. The limit of low frequency response obtained previously by Denison and Baum was recovered, and the limitations of the quasi-steady theory were investigated.

  20. Simulating confined swirling gas-solid two phase jet

    金晗辉; 夏钧; 樊建人; 岑可法


    A k-ε-kp multi-fluid model was used to simulate confined swirling gas-solid two phase jet comprised of particle-laden flow from a center tube and a swirling air stream entering the test section from the coaxial annular. After considering the drag force between the two phases and gravity, a series of numerical simulations of the two-phase flow of 30μm, 45μm, 60μm diameter particles were performed on a x×r=50×50 mesh grid respectively. The results showed that the k-ε-kp multi-fluid model can be applied to predict moderate swirling multi-phase flow. When the particle diameter is large, the collision of the particles with the wall will influence the prediction accuracy. The bigger the diameter of the particles, the stronger the collision with the wall, and the more obvious the difference between measured and calculated results.

  1. Oscillatory burning of solid propellants including gas phase time lag.

    T'Ien, J. S.


    An analysis has been performed for oscillatory burning of solid propellants including gas phase time lag. The gaseous flame is assumed to be premixed and laminar with a one-step overall chemical reaction. The propellant is assumed to decompose according to the Arrenhius Law, with no condensed phase reaction. With this model, strong gas phase resonance has been found in certain cases at the characteristic gas-phase frequencies, but the peaking of the acoustic admittance is in the direction favoring the damping of pressure waves. At still higher frequencies, moderate wave-amplifying ability was found. The limit of low frequency response obtained previously by Denison and Baum was recovered, and the limitations of the quasi-steady theory were investigated.

  2. Energy Storage Properties of Phase Change Materials Prepared from PEG/CPP


    New kinds of solid-solid phase change materials have been prepared in our laboratory.In these materials, the rigid polymer chlorinated polypropylene is taken as skeletons and the flexible polymer polyethylene glycol 6000 and polyethylene glycol 10000 are taken as functional chains. Results show that chlorinated polypropylene grafted by polyethylene glycol 10000 has greater enthalpy than chlorinated polypropylene grafted by polyethylene glycol 6000.

  3. Development of Ceramic Solid-State Laser Host Material

    Prasad, Narasimha S.; Trivedi, Sudhir; Kutcher, Susan; Wang, Chen-Chia; Kim, Joo-Soo; Hommerich, Uwe; Shukla, Vijay; Sadangi, Rajendra


    Polycrystalline ceramic laser materials are gaining importance in the development of novel diode-pumped solid-state lasers. Compared to single-crystals, ceramic laser materials offer advantages in terms of ease of fabrication, shape, size, and control of dopant concentrations. Recently, we have developed Neodymium doped Yttria (Nd:Y2O3) as a solid-state ceramic laser material. A scalable production method was utilized to make spherical non agglomerated and monodisperse metastable ceramic powders of compositions that were used to fabricate polycrystalline ceramic material components. This processing technique allowed for higher doping concentrations without the segregation problems that are normally encountered in single crystalline growth. We have successfully fabricated undoped and Neodymium doped Yttria material up to 2" in diameter, Ytterbium doped Yttria, and erbium doped Yttria. We are also in the process of developing other sesquioxides such as scandium Oxide (Sc2O3) and Lutesium Oxide (Lu2O3) doped with Ytterbium, erbium and thulium dopants. In this paper, we present our initial results on the material, optical, and spectroscopic properties of the doped and undoped sesquioxide materials. Polycrystalline ceramic lasers have enormous potential applications including remote sensing, chem.-bio detection, and space exploration research. It is also potentially much less expensive to produce ceramic laser materials compared to their single crystalline counterparts because of the shorter fabrication time and the potential for mass production in large sizes.

  4. Triggerless vacuum shunting plasma by metallic and solid materials

    Yukimura, Ken; Tani, Yuuji; Masamune, Sadao


    Shunting discharge is an alternating capacitor discharge through a rod of solid-state or metallic materials. Optimization of the discharge condition has realized self-ignition of the arc discharge with low input power to the rod, leading to a much longer rod life time than in conventional shunting arc or peripheral arc. The shunting-arc-produced plasma contains mainly the ions of the solid-state material, and ion extraction from the plasma has also been demonstrated. Thus, the shunting arc works as a pulsed ion source for solid-state materials for plasma-based ion implantation (PBII) and ion processing. This article describes the characteristics of pulsed shunting arc, using the materials of carbon, niobium and silicon. The capacitor of 10 nF of which charging voltage is 10 to 25 kV using a thyratron as a closing switch. Glow discharge is firstly produced after the heat of the materials and then the plasma changes the style to the arc discharge. A negative high voltage pulse of -5 to -10 kV was applied to a target which was located at 30 cm away from the electrodes. We will discuss the ion species of the shunting plasma and ion extraction from the plasma using the time evolution of target current.

  5. Direct molecular dynamics simulation of liquid-solid phase equilibria for a three-component plasma.

    Hughto, J; Horowitz, C J; Schneider, A S; Medin, Zach; Cumming, Andrew; Berry, D K


    The neutron-rich isotope ²²Ne may be a significant impurity in carbon and oxygen white dwarfs and could impact how the stars freeze. We perform molecular dynamics simulations to determine the influence of ²²Ne in carbon-oxygen-neon systems on liquid-solid phase equilibria. Both liquid and solid phases are present simultaneously in our simulation volumes. We identify liquid, solid, and interface regions in our simulations using a bond angle metric. In general we find good agreement for the composition of liquid and solid phases between our MD simulations and the semianalytic model of Medin and Cumming. The trace presence of a third component, neon, does not appear to strongly impact the chemical separation found previously for two-component carbon and oxygen systems. This suggests that small amounts of ²²Ne may not qualitatively change how the material in white dwarf stars freezes. However, we do find systematically lower melting temperatures (higher Γ) in our MD simulations compared to the semianalytic model. This difference seems to grow with impurity parameter Q_{imp} and suggests a problem with simple corrections to the linear mixing rule for the free energy of multicomponent solid mixtures that is used in the semianalytic model.

  6. Mechanistic understanding of calcium-phosphonate solid dissolution and scale inhibitor return behavior in oilfield reservoir: formation of middle phase.

    Zhang, Ping; Shen, Dong; Ruan, Gedeng; Kan, Amy T; Tomson, Mason B


    Phosphonates are an important class of mineral scale inhibitors used for oilfield scale control. By injecting the phosphonate into an oilfield reservoir, calcium-phosphonate precipitate will form and subsequently release the phosphonate into produced water for scale control. In this study, a systematic procedure is developed to mechanistically characterize an acidic calcium-phosphonate amorphous material that is later developed into a middle phase and eventually a crystalline phase. The phosphonate used in this study is diethylenetriamine pentakis (methylene phosphonic acid) (DTPMP). An amorphous calcium-DTPMP solid is precipitated by mixing a calcium-containing solution with a DTPMP solution. The stoichiometry of this initially formed solid can be experimentally confirmed via a static dissolution test. Following another dynamic development test, two additional Ca-DTPMP solid phases, i.e., a middle phase and a crystalline phase have been observed. Electron microscopy and X-ray diffraction were employed to characterize the morphology and crystallinity of different Ca-DTPMP solids of interest. Evidently, the dynamic brine flushing of the Ca-DTPMP solid developed the initially amorphous material into a middle phase solid with an amorphous/microcrystalline structure and eventually into a crystalline material. Furthermore, a dissolution characterization study was carried out to determine the solubility product of the middle phase solid at different conditions. The obtained mechanistic understanding of the Ca-DTPMP solid related to precipitation chemistry, dissolution behavior and phase transition is critical to elucidate oilfield DTPMP return data and more importantly, can optimize the oilfield scale squeeze design to achieve an extended squeeze lifetime.

  7. Design of indirect solid-phase immunosorbent methods for detecting arenavirus antigens and antibodies

    Ivanov, A.P.; Rezapkin, G.V.; Dzagurova, T.K.; Tkachenko, E.A.


    Specifications have been elaborated for formulating indirect solid-phase enzyme-linked immunosorbent assay (ELISA) and radioimmunoassay (SPRIA) methods that employ anti-human and anti-mice G class immunoglobulin (IgG), conjugated with horseradish peroxidase and /sup 125/I for detecting the arenaviruses Junin, Machupo, Tacaribe, Amalpari, Tamiami, Lassa, and LCM (lymphocytic choriomeningitis). These methods make it possible to identify with a high degree of sensitivity arenavirus antigens and antibodies in various kinds of material.

  8. Two phase continuous digestion of solid manure on-farm: design, mass and nutrient balance

    Schäfer, Winfried; Evers, Lars; Lehto, Marja; Sorvala, Sanna; Teye, Frederick; Granstedt, Artur


    During the last decade some so called ‘dry fermentation’ prototype plants were developed for anaerobic digestion of organic material containing 15-50 % total solids. These plants show added advantages com-pared to slurry digestion plants: Less reactor volume, less process energy, less transport capacity, less odour emissions. However on-farm dry fermentation plants are not common and rarely commercially available. This paper reports about an innovative two phase prototype biogas plant designe...

  9. Determination of formaldehyde in Brazilian alcohol fuels by flow-injection solid phase spectrophotometry

    Teixeira, Leonardo Sena Gomes; Leão, Elsimar S.; Dantas,Alailson Falcão; Pinheiro, Heloísa Lúcia C.; Costa, Antonio Celso Spinola; Andrade,Jailson Bittencourt de


    p. 711–715 In thiswork, a solid phase spectrophotometric method in association with flowinjection analysis for formaldehyde determination has been developed with direct measurement of light-absorption in C18 material. The 3,5-diacetyl-1,4-dihydrolutidine produced from the reaction between formaldehyde and fluoral P was quantitatively retained on C18 support and the spectrophotometric detection was performed simultaneously at 412 nm. The retained complex was quickly eluted from C18 mater...

  10. Phase change material thermal capacitor clothing

    Buckley, Theresa M. (Inventor)


    An apparatus and method for metabolic cooling and insulation of a user in a cold environment. In its preferred embodiment the apparatus is a highly flexible composite material having a flexible matrix containing a phase change thermal storage material. The apparatus can be made to heat or cool the body or to act as a thermal buffer to protect the wearer from changing environmental conditions. The apparatus may also include an external thermal insulation layer and/or an internal thermal control layer to regulate the rate of heat exchange between the composite and the skin of the wearer. Other embodiments of the apparatus also provide 1) a path for evaporation or direct absorption of perspiration from the skin of the wearer for improved comfort and thermal control, 2) heat conductive pathways within the material for thermal equalization, 3) surface treatments for improved absorption or rejection of heat by the material, and 4) means for quickly regenerating the thermal storage capacity for reuse of the material. Applications of the composite materials are also described which take advantage of the composite's thermal characteristics. The examples described include a diver's wet suit, ski boot liners, thermal socks, gloves and a face mask for cold weather activities, and a metabolic heating or cooling blanket useful for treating hypothermia or fever patients in a medical setting and therapeutic heating or cooling orthopedic joint supports.

  11. Phase field modeling and simulation of three-phase flow on solid surfaces

    Zhang, Qian; Wang, Xiao-Ping


    Phase field models are widely used to describe the two-phase system. The evolution of the phase field variables is usually driven by the gradient flow of a total free energy functional. The generalization of the approach to an N phase (N ≥ 3) system requires some extra consistency conditions on the free energy functional in order for the model to give physically relevant results. A projection approach is proposed for the derivation of a consistent free energy functional for the three-phase Cahn-Hilliard equations. The system is then coupled with the Navier-Stokes equations to describe the three-phase flow on solid surfaces with moving contact line. An energy stable scheme is developed for the three-phase flow system. The discrete energy law of the numerical scheme is proved which ensures the stability of the scheme. We also show some numerical results for the dynamics of triple junctions and four phase contact lines.

  12. Studies on solid phase synthesis,characterization and fluorescent property of the new rare earth complexes

    Jianwei SHI


    Full Text Available Rare earth-β-diketone ligand complex luminescent material has stable chemical properties and excellent luminous property. Using europium oxide and (γ-NTA as raw materials, novel rare earth-β-dione complexes are synthesized by solid state coordination chemistry. The synthesis temperature and milling time are discussed for optimization. Experimental results show that the suitable reaction situation is at 50 ℃ and 20 h for solid-phase synthesis. The compositions and structures of the complexes are characterized by means of elemental analysis, UV-Vis and FTIR methods, and the phase stability of the complex is determined by using TG-DTA technique. It is proved that preparation of waterless binary rare earth complexes by the solid phase reaction method results in a higher product yield. The fluorescence spectra show that between Eu (Ⅲ and γ-NTA, there exists efficient energy transfer, and the rare earth complexes synthesis is an excellent red bright light-emitting material with excellent UV excited luminescence properties.

  13. Solid-Phase Preparation and Characterization of Chitosan

    GaoLe-ping; DuYu-min; ZhangDao-bin; ShiXiao-wen; ZhanHuai-yu; SongWen-hua


    Chitosan was prepared with stressing method by blending chitin and solid alkali in a single-screw extruder at given temperature and characterized by potentiometric titration, gel permeation chromatography (GPC), infrared spectrum (IR) and carborr13 magnetic resonance sperctroscopy (13C NMR). Chitosan with a deacetylation degree (DD) of 76. 1% was obtained at a mass ratio 0.2 : 1 : 1 for H20/chitin/NaOH at 160℃ for 12 mirL Compared to conventional solution method(usually 1 : 10 for chitin/NaOH), the alkali assumption greatly decreased. Molecular weight of chitosan obtained by solid-phase method(S3,M. 1.54 X 10s ) was lower than that obtained by suspension method(Y2,Mw3. 34×105). During deacetylation, molecular weight decreased with high reaction temperature and long reaction time but remained same at different initial ratios of NaOH/chitirL It might be concluded that degradation of chitosan was caused by breakout of the main chain of the oxidized chitosan catalyzed by alkali during the deactylation. IR and 13C NMR showed that structures of chitosans prepared by solid-phase method were not changed.

  14. Determining material parameters using phase-field simulations and experiments

    Zhang, Jin; Poulsen, Stefan O.; Gibbs, John W.


    A method to determine material parameters by comparing the evolution of experimentally determined 3D microstructures to simulated 3D microstructures is proposed. The temporal evolution of a dendritic solid-liquid mixture is acquired in situ using x-ray tomography. Using a time step from these dat...... variation of the best-fit parameters and the fidelity of the fitting. We find a liquid diffusion coefficient that is different from that measured using directional solidification....... as an initial condition in a phase-field simulation, the computed structure is compared to that measured experimentally at a later time. An optimization technique is used to find the material parameters that yield the best match of the simulated microstructure to the measured microstructure in a global manner...

  15. Mass, energy and material balances of SRF production process. Part 3: solid recovered fuel produced from municipal solid waste.

    Nasrullah, Muhammad; Vainikka, Pasi; Hannula, Janne; Hurme, Markku; Kärki, Janne


    This is the third and final part of the three-part article written to describe the mass, energy and material balances of the solid recovered fuel production process produced from various types of waste streams through mechanical treatment. This article focused the production of solid recovered fuel from municipal solid waste. The stream of municipal solid waste used here as an input waste material to produce solid recovered fuel is energy waste collected from households of municipality. This article presents the mass, energy and material balances of the solid recovered fuel production process. These balances are based on the proximate as well as the ultimate analysis and the composition determination of various streams of material produced in a solid recovered fuel production plant. All the process streams are sampled and treated according to CEN standard methods for solid recovered fuel. The results of the mass balance of the solid recovered fuel production process showed that 72% of the input waste material was recovered in the form of solid recovered fuel; 2.6% as ferrous metal, 0.4% as non-ferrous metal, 11% was sorted as rejects material, 12% as fine faction and 2% as heavy fraction. The energy balance of the solid recovered fuel production process showed that 86% of the total input energy content of input waste material was recovered in the form of solid recovered fuel. The remaining percentage (14%) of the input energy was split into the streams of reject material, fine fraction and heavy fraction. The material balances of this process showed that mass fraction of paper and cardboard, plastic (soft) and wood recovered in the solid recovered fuel stream was 88%, 85% and 90%, respectively, of their input mass. A high mass fraction of rubber material, plastic (PVC-plastic) and inert (stone/rock and glass particles) was found in the reject material stream. © The Author(s) 2014.

  16. Transport phenomena and drying of solids and particulate materials

    Lima, AG


    The purpose of this book, Transport Phenomena and Drying of Solids and Particulate Materials, is to provide a collection of recent contributions in the field of heat and mass transfer, transport phenomena, drying and wetting of solids and particulate materials. The main benefit of the book is that it discusses some of the most important topics related to the heat and mass transfer in solids and particulate materials. It includes a set of new developments in the field of basic and applied research work on the physical and chemical aspects of heat and mass transfer phenomena, drying and wetting processes, namely, innovations and trends in drying science and technology, drying mechanism and theory, equipment, advanced modelling, complex simulation and experimentation. At the same time, these topics will be going to the encounter of a variety of scientific and engineering disciplines. The book is divided in several chapters that intend to be a resume of the current state of knowledge for benefit of professional c...

  17. Exploring Magnetic Elastocaloric Materials for Solid-State Cooling

    Liu, Jian; Zhao, Dewei; Li, Yang


    In the past decade, there has been an increased surge in the research on elastocaloric materials for solid-state refrigerators. The strong coupling between structure and magnetism inspires the discovery of new multi-field driven elastocaloric alloys. This work is devoted to magnetic shape memory alloys suitable for mechanical cooling applications. Some novel characteristics in magnetostructural transition materials other than conventional shape memory alloys are overviewed. From the physical and engineering points of view, we have put forward general strategies to maximize elastocaloric temperature change to increase performance reversibility and to improve mechanical properties. The barocaloric effect as a sister-cooling alternative is also discussed.

  18. Review on MIEC Cathode Materials for Solid Oxide Fuel Cells

    Burnwal, Suman Kumar; Bharadwaj, S.; Kistaiah, P.


    The cathode is one of the most important components of solid oxide fuel cells (SOFCs). The reduction of oxygen at the cathode (traditional cathodes like LSM, LSGM, etc.) is the slow step in the cell reaction at intermediate temperature (600-800∘C) which is one of the key obstacles to the development of SOFCs. The mixed ionic and electronic conducting cathode (MIEC) like LSCF, BSCF, etc., has recently been proposed as a promising cathode material for SOFC due to the improvement of the kinetic of the cathode reaction. The MIEC materials provide not only the electrons for the reduction of oxygen, but also the ionic conduction required to ensure the transport of the formed oxygen ions and thereby improves the overall electrochemical performance of SOFC system. The characteristics of MIEC cathode materials and its comparison with other traditional cathode materials is studied and presented in the paper.

  19. Solid Phase Peptide Synthesis of Fusukang for AIDS

    甘一如; 戴琦; 张雪竹; 高晨昊


    A 36-residue peptide is designed to cure acquired immunodeficiency syndrome(AIDS), and is synthesized by the manual solid phase peptide synthesis technique. Different reaction conditions of the synthesis process were discussed. Stirring efficiency of mechanics and nitrogen was compared. The mechanical method displays a predominant performance. Although the coupling efficiencies of diisopropylcarbodiimide(DIC) and dicyclohexylcarbodiimide(DCC) are virtually identical, DIC offers several advantages over DCC in practice due to different physical characters. Wash conditions after deprotection and coupling were investigated to monitor washing efficiency. 0.369 2 g crude peptide was obtained.

  20. Solid-phase colorimetric method for the quantification of fucoidan.

    Lee, Jung Min; Shin, Z-U; Mavlonov, Gafurjon T; Abdurakhmonov, Ibrokhim Y; Yi, Tae-Hoo


    We described the simple, selective, and rapid method for determination of fucoidans using methylene blue staining of sulfated polysaccharides, immobilized into filter paper and consequent optic density (at A (663) nm) measurement of the eluted dye from filter paper. This solid-phase method allows selective determination of 1-20 μg fucoidan in presence of potentially interfering compounds (alginic acid, DNA, salts, proteins, and detergents). Further, we demonstrated the alternative way of using image processing software for fucoidan quantification without extraction of methylene blue dye from stained spots of fucoidan-dye complex.

  1. Direct MD simulation of liquid-solid phase equilibria for three-component plasma

    Hughto, J; Schneider, A S; Medin, Zach; Cumming, Andrew; Berry, D K


    The neutron rich isotope 22Ne may be a significant impurity in carbon and oxygen white dwarfs and could impact how the stars freeze. We perform molecular dynamics simulations to determine the influence of 22Ne in carbon-oxygen-neon systems on liquid-solid phase equilibria. Both liquid and solid phases are present simultaneously in our simulation volumes. We identify liquid, solid, and interface regions in our simulations using a bond angle metric. In general we find good agreement for the composition of liquid and solid phases between our MD simulations and the semi analytic model of Medin and Cumming. The trace presence of a third component, neon, does not appear to strongly impact the chemical separation found previously for two component carbon and oxygen systems. This suggests that small amounts of 22Ne may not qualitatively change how the material in white dwarf stars freezes. However, we do find systematically lower melting temperatures (higher Gamma) in our MD simulations compared to the semi analytic ...

  2. Material Engineering for Phase Change Memory

    Cabrera, David M.

    As semiconductor devices continue to scale downward, and portable consumer electronics become more prevalent there is a need to develop memory technology that will scale with devices and use less energy, while maintaining performance. One of the leading prototypical memories that is being investigated is phase change memory. Phase change memory (PCM) is a non-volatile memory composed of 1 transistor and 1 resistor. The resistive structure includes a memory material alloy which can change between amorphous and crystalline states repeatedly using current/voltage pulses of different lengths and magnitudes. The most widely studied PCM materials are chalcogenides - Germanium-Antimony-Tellerium (GST) with Ge2Sb2Te3 and Germanium-Tellerium (GeTe) being some of the most popular stochiometries. As these cells are scaled downward, the current/voltage needed to switch these materials becomes comparable to the voltage needed to sense the cell's state. The International Roadmap for Semiconductors aims to raise the threshold field of these devices from 66.6 V/mum to be at least 375 V/mum for the year 2024. These cells are also prone to resistance drift between states, leading to bit corruption and memory loss. Phase change material properties are known to influence PCM device performance such as crystallization temperature having an effect on data retention and litetime, while resistivity values in the amorphous and crystalline phases have an effect on the current/voltage needed to write/erase the cell. Addition of dopants is also known to modify the phase change material parameters. The materials G2S2T5, GeTe, with dopants - nitrogen, silicon, titanium, and aluminum oxide and undoped Gallium-Antimonide (GaSb) are studied for these desired characteristics. Thin films of these compositions are deposited via physical vapor deposition at IBM Watson Research Center. Crystallization temperatures are investigated using time resolved x-ray diffraction at Brookhaven National Laboratory


    E.Q. Xie; W.W. Wang; N. Jiang; D.Y. He


    Manganese silicide MnSi2-x thin films have been prepared on n-type silicon substratesthrough solid phase reaction. The heterostructures were analyzed by X-ray diffraction,Rutherford backscattering spectroscopy, Fourier transform infrared transmittance spec-troscopy and the four-point probe technique. The results show that two manganese sili-cides have been formed sequentially via the reaction of thin layer Mn with Si substrateat different irradiation annealing stages, i.e., MnSi at 450℃ and MnSi1.73 at 550℃.MnSi1.73 phase exhibits preferred growth after irradiation with infrared. In situ four-point probe measurements of sheet resistance during infrared irradiation annealingshow that nucleation of MnSi and phase transformation of MnSi to MnSi1. 73 occur at410℃ and 530℃, respectively; the MnSi phase shows metallic behavior, while MnSi1.73exhibits semiconducting behavior. Characteristic phonon bands of MnSi2-x silicides,which can be used for phase identification along with conventional XRD techniques,have been observed by FTIR spectroscopy.

  4. Calorimetry study of microwave absorption of some solid materials.

    He, Chun Lin; Ma, Shao Jian; Su, Xiu Juan; Chen, Yan Qing; Liang, Yu Shi


    In practice, the dielectric constant of a material varies the applied frequency the material composition, particle size, purity, temperature, physical state (solid or liquid), and moisture content. All of these parameters might change during processing, therefore, it is difficult to predict how well a material will absorb microwave energy in a given process. When the temperature is measured by a digital thermometer, it could not accurately reflect the true temperature of the bulk materials, especially for mixed materials. Thus, in this paper we measured the microwave absorption characteristics of different materials by calorimetry. The microwave power levels, irradiation times, and masses of the materials were varied. It was difficult to predict the microwave energy absorption characteristics of reagent-grade inorganic compounds based on their color, metallic cation, or water stoichiometry. CuO, MnO2, Fe3O4, and MnSO4 x H2O (Taishan) strongly absorbed microwave energy. Most of the remaining inorganic compounds were poor absorbers, with silica hardly absorbing any microwave energy. Carbon-based materials had significantly different microwave absorption characteristics. Activated carbon and coke were especially sensitive to microwaves, but different types of coal were poor absorbers. The jamesonite concentrate absorbed microwave energy strongly, while the zinc concentrate was a poor absorber.


    Ning Yang; Wei Wang; Wei Ge; Jinghai Li


    @@ Introduction Gas-solid two-phase flow is often encountered in chemical reactors for the process industry. For industrial users, design, scale-up, control and optimization for these reactors require a good understanding of the hydrodynamics of gas-solid two-phase flow. For researchers, exploration and prediction of the complex phenomena call for a good comprehension of the heterogeneous structure and of the dominant mechanisms of gas-solid and solid-solid interactions.

  6. High Pressure Materials Research: Novel Extended Phases of Molecular Triatomics

    Yoo, C


    Application of high pressure significantly alters the interatomic distance and thus the nature of intermolecular interaction, chemical bonding, molecular configuration, crystal structure, and stability of solid [1]. With modern advances in high-pressure technologies [2], it is feasible to achieve a large (often up to a several-fold) compression of lattice, at which condition material can be easily forced into a new physical and chemical configuration [3]. The high-pressure thus offers enhanced opportunities to discover new phases, both stable and metastable ones, and to tune exotic properties in a wide-range of atomistic length scale, substantially greater than (often being several orders of) those achieved by other thermal (varying temperatures) and chemical (varying composition or making alloys) means. Simple molecular solids like H{sub 2}, C, CO{sub 2}, N{sub 2}, O{sub 2}, H{sub 2}O, CO, NH{sub 3}, and CH{sub 4} are bounded by strong covalent intramolecular bonds, yet relatively weak intermolecular bonds of van der Waals and/or hydrogen bonds. The weak intermolecular bonds make these solids highly compressible (i.e., low bulk moduli typically less than 10 GPa), while the strong covalent bonds make them chemically inert at least initially at low pressures. Carbon-carbon single bonds, carbon-oxygen double bonds and nitrogen-nitrogen triple bonds, for example, are among the strongest. These molecular forms are, thus, often considered to remain stable in an extended region of high pressures and high temperatures. High stabilities of these covalent molecules are also the basis of which their mixtures are often presumed to be the major detonation products of energetic materials as well as the major constituents of giant planets. However, their physical/chemical stabilities are not truly understood at those extreme pressure-temperature conditions. In fact, an increasing amount of experimental evidences contradict the assumed stability of these materials at high

  7. Passive thermal management using phase change materials

    Ganatra, Yash Yogesh

    The trend of enhanced functionality and reducing thickness of mobile devices has. led to a rapid increase in power density and a potential thermal bottleneck since. thermal limits of components remain unchanged. Active cooling mechanisms are not. feasible due to size, weight and cost constraints. This work explores the feasibility. of a passive cooling system based on Phase Change Materials (PCMs) for thermal. management of mobile devices. PCMs stabilize temperatures due to the latent heat. of phase change thus increasing the operating time of the device before threshold. temperatures are exceeded. The primary contribution of this work is the identification. of key parameters which influence the design of a PCM based thermal management. system from both the experiments and the numerical models. This work first identifies strategies for integrating PCMs in an electronic device. A. detailed review of past research, including experimental techniques and computational. models, yields key material properties and metrics to evaluate the performance of. PCMs. Subsequently, a miniaturized version of a conventional thermal conductivity. measurement technique is developed to characterize thermal resistance of PCMs. Further, latent heat and transition temperatures are also characterized for a wide. range of PCMs. In-situ measurements with PCMs placed on the processor indicate that some. PCMs can extend the operating time of the device by as much as a factor of 2.48. relative to baseline tests (with no PCMs). This increase in operating time is investigated. by computational thermal models that explore various integration locations, both at the package and device level.

  8. Nucleation of the diamond phase in aluminium-solid solutions

    Hornbogen, E.; Mukhopadhyay, A. K.; Starke, E. A., Jr.


    Precipitation was studied from fcc solid solutions with silicon, germanium, copper and magnesium. Of all these elements only silicon and germanium form diamond cubic (DC) precipitates in fcc Al. Nucleation of the DC structure is enhanced if both types of atom are dissolved in the fcc lattice. This is interpreted as due to atomic size effects in the prenucleation stage. There are two modes of interference of fourth elements with nucleation of the DC phase in Al + Si, Ge. The formation of the DC phase is hardly affected if the atoms (for example, copper) are rejected from the (Si, Ge)-rich clusters. If additional types of atom are attracted by silicon and/or germanium, DC nuclei are replaced by intermetallic compounds (for example Mg2Si).

  9. Powder metallurgy: Solid and liquid phase sintering of copper

    Sheldon, Rex; Weiser, Martin W.


    Basic powder metallurgy (P/M) principles and techniques are presented in this laboratory experiment. A copper based system is used since it is relatively easy to work with and is commercially important. In addition to standard solid state sintering, small quantities of low melting metals such as tin, zinc, lead, and aluminum can be added to demonstrate liquid phase sintering and alloy formation. The Taguchi Method of experimental design was used to study the effect of particle size, pressing force, sintering temperature, and sintering time. These parameters can be easily changed to incorporate liquid phase sintering effects and some guidelines for such substitutions are presented. The experiment is typically carried out over a period of three weeks.

  10. Solid Phase Characterization of Tank 241-C-108 Residual Waste Solids Samples

    Cooke, Gary A.; Pestovich, John A.; Huber, Heinz J.


    This report presents the results for solid phase characterization (SPC) of solid samples removed from tank 241-C-108 (C-108) on August 12-13,2012, using the off-riser sampler. Samples were received at the 222-S Laboratory on August 13 and were described and photographed. The SPC analyses that were performed include scanning electron microscopy (SEM) using the ASPEX(R)l scanning electron microscope, X-ray diffraction (XRD) using the Rigaku(R) 2 MiniFlex X-ray diffractometer, and polarized light microscopy (PLM) using the Nikon(R) 3 Eclipse Pol optical microscope. The SEM is equipped with an energy dispersive X-ray spectrometer (EDS) to provide chemical information. Gary A. Cooke conducted the SEM analysis, John A. Pestovich performed the XRD analysis, and Dr. Heinz J. Huber performed the PLM examination. The results of these analyses are presented here.

  11. Optimization of solid-state synthesis process of advanced ceramics materials: influence of mixing conditions.

    Sakri Adel


    Full Text Available In this paper, the effect of mixing process on solid state reaction of solid oxide material mixture was studied. Lead piezoelectric ceramic specimens 0.5 Pb(Zn1/3,Sb2/3O3-0.5 Pb0.98La0.02(Zr0.48,Ti0.52O3 prepared by different mixing procedures, were conducted under different conditions such as order, combination and mixing time. The phase formation, composition nature, structural properties of powder mixture was analyzed by X-ray diffraction. The obtained results for different mixing processes make the solid state reaction method more selective, taking into consideration the attraction forces between the reactants and the electronegativity of oxide reactants.

  12. Solid-Phase Purification of Synthetic DNA Sequences.

    Grajkowski, Andrzej; Cieslak, Jacek; Beaucage, Serge L


    Although high-throughput methods for solid-phase synthesis of DNA sequences are currently available for synthetic biology applications and technologies for large-scale production of nucleic acid-based drugs have been exploited for various therapeutic indications, little has been done to develop high-throughput procedures for the purification of synthetic nucleic acid sequences. An efficient process for purification of phosphorothioate and native DNA sequences is described herein. This process consists of functionalizing commercial aminopropylated silica gel with aminooxyalkyl functions to enable capture of DNA sequences carrying a 5'-siloxyl ether linker with a "keto" function through an oximation reaction. Deoxyribonucleoside phosphoramidites functionalized with the 5'-siloxyl ether linker were prepared in yields of 75-83% and incorporated last into the solid-phase assembly of DNA sequences. Capture of nucleobase- and phosphate-deprotected DNA sequences released from the synthesis support is demonstrated to proceed near quantitatively. After shorter than full-length DNA sequences were washed from the capture support, the purified DNA sequences were released from this support upon treatment with tetra-n-butylammonium fluoride in dry DMSO. The purity of released DNA sequences exceeds 98%. The scalability and high-throughput features of the purification process are demonstrated without sacrificing purity of the DNA sequences.

  13. Multinuclear solid-state nuclear magnetic resonance of inorganic materials

    MacKenzie, Kenneth J D


    Techniques of solid state nuclear magnetic resonance (NMR) spectroscopy are constantly being extended to a more diverse range of materials, pressing into service an ever-expanding range of nuclides including some previously considered too intractable to provide usable results. At the same time, new developments in both hardware and software are being introduced and refined. This book covers the most important of these new developments. With sections addressed to non-specialist researchers (providing accessible answers to the most common questions about the theory and practice of NMR asked by novices) as well as a more specialised and up-to-date treatment of the most important areas of inorganic materials research to which NMR has application, this book should be useful to NMR users whatever their level of expertise and whatever inorganic materials they wish to study.

  14. Studies of phase transitions in the aripiprazole solid dosage form.

    Łaszcz, Marta; Witkowska, Anna


    Studies of the phase transitions in an active substance contained in a solid dosage form are very complicated but essential, especially if an active substance is classified as a BCS Class IV drug. The purpose of this work was the development of sensitive methods for the detection of the phase transitions in the aripiprazole tablets containing initially its form III. Aripiprazole exhibits polymorphism and pseudopolymorphism. Powder diffraction, Raman spectroscopy and differential scanning calorimetry methods were developed for the detection of the polymorphic transition between forms III and I as well as the phase transition of form III into aripiprazole monohydrate in tablets. The study involved the initial 10 mg and 30 mg tablets, as well as those stored in Al/Al blisters, a triplex blister pack and HDPE bottles (with and without desiccant) under accelerated and long term conditions. The polymorphic transition was not observed in the initial and stored tablets but it was visible on the DSC curve of the Abilify(®) 10 mg reference tablets. The formation of the monohydrate was observed in the diffractograms and Raman spectra in the tablets stored under accelerated conditions. The monohydrate phase was not detected in the tablets stored in the Al/Al blisters under long term conditions. The results showed that the Al/Al blisters can be recommended as the packaging of the aripiprazole tablets containing form III.

  15. Electric-field-assisted crystallisation in phase-change materials

    Kohary, Krisztian; Diosdado, Jorge A.V.; Ashwin, Peter; Wright, C. David [College of Engineering, Mathematics, and Physical Sciences, University of Exeter (United Kingdom)


    Phase-change materials are of intense research interest due mainly to their use in phase-change memory (PCM) devices that are emerging as a promising technology for future non-volatile, solid-state, electrical storage. Electrically driven transitions from the amorphous to the crystalline phase in such devices exhibit characteristic threshold switching. Several alternative electronic explanations for the origins of this characteristic behaviour have been put forward, for example Poole-Frenkel effects, delocalisation of tail states, field emission processes and space charge limited currents [for a full discussion, see Radielli et al., J. Appl. Phys. 103, 111101 (2008) and Simon et al., MRS Proc. 1251, H01-H011 (2010)]. However, an alternative to these conventional electronic models of threshold switching is based on electric field induced lowering of the system free energy, leading to the field induced nucleation of conducting crystal filaments. In this paper we investigate this alternative view. We present a detailed kinetics study of crystallisation in the presence of an electric field for the phase-change material Ge{sub 2}Sb{sub 2}Te{sub 5}. We derive quantitative crystallisation maps to show the effects of both temperature and electric field on crystallisation and we identify field ranges and parameter values where the electric field might play a significant role. Then we carry out physically realistic simulations of the threshold switching process in typical phase-change device structures, both with and without electric field dependent energy contributions to the system free energy. Our results show that threshold switching can be obtained by a mechanism driven purely by electric field induced nucleation, but the fields so required are large, of the order of 300 MV m{sup -1}, and significantly larger than the experimentally measured threshold fields. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  16. An Overview of 2014 SBIR Phase I and Phase II Materials Structures for Extreme Environments

    Nguyen, Hung D.; Steele, Gynelle C.; Morris, Jessica R.


    NASA's Small Business Innovation Research (SBIR) program focuses on technological innovation by investing in development of innovative concepts and technologies to help NASA mission directorates address critical research needs for Agency programs. This report highlights nine of the innovative SBIR 2014 Phase I and Phase II projects that emphasize one of NASA Glenn Research Center's six core competencies-Materials and Structures for Extreme Environments. The technologies cover a wide spectrum of applications such as high temperature environmental barrier coating systems, deployable space structures, solid oxide fuel cells, and self-lubricating hard coatings for extreme temperatures. Each featured technology describes an innovation, technical objective, and highlights NASA commercial and industrial applications. This report provides an opportunity for NASA engineers, researchers, and program managers to learn how NASA SBIR technologies could help their programs and projects, and lead to collaborations and partnerships between the small SBIR companies and NASA that would benefit both.

  17. Critical Regimes of Two-Phase Flows with a Polydisperse Solid Phase

    Barsky, Eugene


    This book brings to light peculiarities of the formation of critical regimes of two-phase flows with a polydisperse solid phase. A definition of entropy is formulated on the basis of statistical analysis of these peculiarities. The physical meaning of entropy and its correlation with other parameters determining two-phase flows are clearly defined. The interrelations and main differences between this entropy and the thermodynamic one are revealed. The main regularities of two-phase flows both in critical and in other regimes are established using the notion of entropy. This parameter serves as a basis for a deeper insight into the physics of the process and for the development of exhaustive techniques of mass exchange estimation in such flows. The book is intended for graduate and postgraduate students of engineering studying two-phase flows, and to scientists and engineers engaged in specific problems of such fields as chemical technology, mineral dressing, modern ceramics, microelectronics, pharmacology, po...

  18. Pressure effect on hysteresis in spin-crossover solid materials

    Gudyma, Iurii, E-mail: [Department of General Physics, Chernivtsi National University, Chernivtsi 58012 (Ukraine); Ivashko, Victor [Department of General Physics, Chernivtsi National University, Chernivtsi 58012 (Ukraine); Dimian, Mihai [Department of Electrical and Computer Engineering, Howard University, Washington DC 20059 (United States); Faculty of Electrical Engineering and Computer Science & Integrated Center for Research, Development and Innovation in Advanced Materials, Nanotechnologies, and Distributed Systems for fabrication and control, Stefan cel Mare University, Suceava 720229 (Romania)


    A generalized microscopic Ising-like model is proposed to describe behavior of compressible spin-crossover solids with two states: low-spin and high-spin. The model was solved in mean-field approximation and shows hysteretic behavior at low energy difference between the states. We study the thermal transition between states under external hydrostatic pressure taking into account the changes in the volume of spin-crossover molecules in different states. Depending on the applied pressure, a spin-crossover system can have three types of behavior of molecular fraction in the high-spin state: hysteretic, second-order phase transition and no-phase transition. For the hysteretic regime, it is shown that the transition temperature under pressure is increased while the width of the hysteresis reduced.

  19. Characteristics of tritium release behavior from solid breeder materials

    Kinjyo, T.; Nishikawa, M.; Yamashita, N.; Koyama, T.; Suematsu, K.; Fukada, S. [Graduate School of Engineering Science, Kyushu Univ., Fukuoka 812-8581 (Japan); Enoeda, M. [Naka Establishment, Japan Atomic Energy Agency, Ibaraki 319-1195 (Japan)


    A tritium release model has been developed by the present authors. The tritium release curves estimated by this tritium model give good agreement with experimental curves for Li {sub 4}SiO{sub 4}, Li{sub 2}TiO{sub 3}, Li{sub 2}ZrO{sub 3} or LiAlO{sub 2} under various purge gas conditions in our out-of-pile bred tritium release. The characteristics of tritium release behavior from various solid breeder materials carried out by us and in EXOTIC experiments at Petten are discussed in this study. (authors)

  20. Production behavior of irradiation defects in solid breeder materials

    Moriyama, Hirotake; Moritani, Kimikazu [Kyoto Univ. (Japan)


    The irradiation effects in solid breeder materials are important for the performance assessment of fusion reactor blanket systems. For a clearer understanding of such effects, we have studied the production behavior of irradiation defects in some lithium ceramics by an in-situ luminescence measurement technique under ion beam irradiation. The luminescence spectra were measured at different temperatures, and the temperature-transient behaviors of luminescence intensity were also measured. The production mechanisms of irradiation defects were discussed on the basis of the observations. (author)

  1. Converters and electric machines. Solid insulating materials. Electrical characteristics; Convertisseurs et machines electriques. Materiaux isolants solides. Caracteristiques electriques

    Anton, A. [Institut National Superieur de Chimie Industrielle, 76 - Rouen (France)


    The aim of this article is to allow a preselection of a solid insulating material using the most common electrical characteristics: tangent of the loss angle, relative permittivity, dielectric rigidity, superficial resistivity, transverse resistivity, resistance to high voltage creeping spark currents, index of creeping resistance. The characteristics of the main solid insulating materials are presented in tables for: thermoplastics, thermosetting materials, natural insulating materials, mineral insulating materials, rubber and synthetic elastomers, stratified insulating materials, thermoplastic films, composite synthetic papers. A comparison is made between the different materials using the three properties: tangent of the loss angle, relative permittivity and resistance to HV spark creeping currents. (J.S.)

  2. Density functional theory study of phase IV of solid hydrogen

    Pickard, Chris J.; Martinez-Canales, Miguel; Needs, Richard J.


    We have studied solid hydrogen up to pressures of 300 GPa and temperatures of 350 K using density functional theory methods and have found “mixed structures” that are more stable than those predicted earlier. Mixed structures consist of alternate layers of strongly bonded molecules and weakly bonded graphene-like sheets. Quasiharmonic vibrational calculations show that mixed structures are the most stable at room temperature over the pressure range 250-295 GPa. These structures are stabilized with respect to strongly bonded molecular phases at room temperature by the presence of lower frequency vibrational modes arising from the graphene-like sheets. Our results for the mixed structures are consistent with the experimental Raman data [M. I. Eremets and I. A. Troyan, Nat. Mater.1476-112210.1038/nmat3175 10, 927 (2011) and R. T. Howie , Phys. Rev. Lett.PRLTAO0031-900710.1103/PhysRevLett.108.125501 108, 125501 (2012)]. We find that mixed phases are reasonable structural models for phase IV of hydrogen.

  3. Oxide anode materials for solid oxide fuel cells

    Fergus, Jeffrey W. [Auburn University, Materials Research and Education Center, 275 Wilmore Laboratories, Auburn, AL 36849 (United States)


    A major advantage of solid oxide fuel cells (SOFCs) over polymer electrolyte membrane (PEM) fuel cells is their tolerance for the type and purity of fuel. This fuel flexibility is due in large part to the high operating temperature of SOFCs, but also relies on the selection and development of appropriate materials - particularly for the anode where the fuel reaction occurs. This paper reviews the oxide materials being investigated as alternatives to the most commonly used nickel-YSZ cermet anodes for SOFCs. The majority of these oxides form the perovskite structure, which provides good flexibility in doping for control of the transport properties. However, oxides that form other crystal structures, such as the cubic fluorite structure, have also shown promise for use as SOFC anodes. In this paper, oxides are compared primarily in terms of their transport properties, but other properties relative to SOFC anode performance are also discussed. (author)

  4. Crystal-Field Engineering of Solid-State Laser Materials

    Henderson, Brian; Bartram, Ralph H.


    This book examines the underlying science and design of laser materials. It emphasizes the principles of crystal-field engineering and discusses the basic physical concepts that determine laser gain and nonlinear frequency conversion in optical crystals. Henderson and Bartram develop the predictive capabilities of crystal-field engineering to show how modification of the symmetry and composition of optical centers can improve laser performance. They also discuss applications of the principles of crystal-field engineering to a variety of optical crystals in relation to the performances of laser devices. This book will be of considerable interest to physical, chemical and material scientists and to engineers involved in the science and technology of solid state lasers.


    Uday B. Pal; Srikanth Gopalan


    AC complex impedance spectroscopy studies were conducted on symmetrical cells of the type [gas, electrode/LSGM electrolyte/electrode, gas]. The electrode materials were slurry-coated on both sides of the LSGM electrolyte support. The electrodes selected for this investigation are candidate materials for SOFC electrodes. Cathode materials include La{sub 1-x}Sr{sub x}MnO{sub 3} (LSM), LSCF (La{sub 1-x}Sr{sub x}Co{sub y}Fe{sub 1-y}O{sub 3}), a two-phase particulate composite consisting of LSM + doped-lanthanum gallate (LSGM), and LSCF + LSGM. Pt metal electrodes were also used for the purpose of comparison. Anode material investigated was the Ni + GDC composite. The study revealed important details pertaining to the charge-transfer reactions that occur in such electrodes. The information obtained can be used to design electrodes for intermediate temperature SOFCs based on LSGM electrolyte.

  6. Fabrication, properties, and tritium recovery from solid breeder materials

    Johnson, C.E. (Argonne National Lab., IL (USA)); Kondo, T. (Japan Atomic Energy Research Inst., Tokyo (Japan)); Roux, N. (CEA Centre d' Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette (France)); Tanaka, S. (Tokyo Univ. (Japan)); Vollath, D. (Kernforschungszentrum Karlsruhe GmbH (Germany, F.R.))


    The breeding blanket is a key component of the fusion reactor because it directly involves tritium breeding and energy extraction, both of which are critical to development of fusion power. The lithium ceramics continue to show promise as candidate breeder materials. This promise was recognized by the International Thermonuclear Experimental Reactor (ITER) design team in its selection of ceramics as the first option for the ITER breeder material. Blanket design studies have indicated properties in the candidate materials data base that need further investigation. Current studies are focusing on tritium release behavior at high burnup, changes in thermophysical properties with burnup, compatibility between the ceramic breeder and beryllium multiplier, and phase changes with burnup. Laboratory and in-reactor tests, some as part of an international collaboration for development of ceramic breeder materials, are underway. 133 refs., 1 fig.

  7. Second sphere coordination of hybrid metal-organic materials: solid state reactivity.

    Guo, Fang; Martí-Rujas, Javier


    When compared to other hybrid metal organic materials such as metal-organic frameworks, hydrogen bonded materials self-assembled by metals and organic molecules using second sphere interactions have been poorly investigated. Consequently, their solid-sate properties are also scarce. In this perspective, earlier research mainly on host-guest chemistry and its evolution towards more extended structures by applying crystal engineering principles using second sphere coordination is described. Crystal-to-crystal guest exchange reactions, permanently porous hybrid metal organic materials, mechanochemical reactivity, thermally induced phase transformations as well as some examples of functional technological applications using second sphere adducts such as gas adsorption, separation and non-linear optical phenomena are also reported. Although some tutorial reviews on second sphere adducts have been conducted mainly in the solution state focusing on metal based anion receptors, to the best of our knowledge, an overview on relevant works that focus on the solid-state properties has not been carried out. The aim of this article is to highlight from some of the early fundamental work to the latest reports on hybrid metal-organic materials self-assembled via second sphere interactions with a focus on solid-state chemistry.

  8. Materials System for Intermediate Temperature Solid Oxide Fuel Cell

    Uday B. Pal; Srikanth Gopalan


    The objective of this work was to obtain a stable materials system for intermediate temperature solid oxide fuel cell (SOFC) capable of operating between 600-800 C with a power density greater than 0.2 W/cm{sup 2}. The solid electrolyte chosen for this system was La{sub 0.9}Sr{sub 0.1}Ga{sub 0.8}Mg{sub 0.2}O{sub 3}, (LSGM). To select the right electrode materials from a group of possible candidate materials, AC complex impedance spectroscopy studies were conducted between 600-800 C on symmetrical cells that employed the LSGM electrolyte. Based on the results of the investigation, LSGM electrolyte supported SOFCs were fabricated with La{sub 0.6}Sr{sub 0.4}Co{sub 0.8}Fe{sub 0.2}O{sub 3}-La{sub 0.9}Sr{sub 0.1}Ga{sub 0.8}Mg{sub 0.2}O{sub 3} (LSCF-LSGM) composite cathode and Nickel-Ce{sub 0.6}La{sub 0.4}O{sub 3} (Ni-LDC) composite anode having a barrier layer of Ce{sub 0.6}La{sub 0.4}O{sub 3} (LDC) between the LSGM electrolyte and the Ni-LDC anode. Electrical performance and stability of these cells were determined and the electrode polarization behavior as a function of cell current was modeled between 600-800 C. The electrical performance of the anode-supported SOFC was simulated assuming an electrode polarization behavior identical to the LSGM-electrolyte-supported SOFC. The simulated electrical performance indicated that the selected material system would provide a stable cell capable of operating between 600-800 C with a power density between 0.2 to 1 W/cm{sup 2}.

  9. Thermoelastic properties of solid phases: C++ object oriented library “SolidEOS”

    Churakov, Sergey V.


    A new object-oriented C++ library (SolidEOS) for calculating the thermoelastic properties of solids is presented. The implementation is based on the Mie-Grüneisen-Debye equation of state (EOS) augmented by lowest order correction for anharmonicity. Several commonly used static EOS like Birch-Murnaghan and Vinet models are available. Although some widely used approximation for the Debye-Grüneisen parameter and static EOS are implemented, the final behaviour of the EOS can be easily modified by overloading predefined virtual functions. The article provides a basic physical background of the modern theory of high-pressure EOS. The detailed documentation of the class hierarchy is summarized in the appendix, which accompanies the source. Several examples of practical use are given in the appendix as well. The library is appropriate for applications in geophysics, petrology, material science or any other field where thermodynamic and elastic properties of solids are relevant. The source code is available from the Computers & Geoscience software archive.

  10. Solid phase epitaxial regrowth of (001) anatase titanium dioxide

    Barlaz, David Eitan; Seebauer, Edmund G., E-mail: [Department of Chemical and Biomolecular Engineering, University of Illinois, 600 S Mathews Ave., Urbana, Illinois 61801 (United States)


    The growing interest in metal oxide based semiconductor technologies has driven the need to produce high quality epitaxial films of one metal oxide upon another. Largely unrecognized in synthetic efforts is that some metal oxides offer strongly polar surfaces and interfaces that require electrostatic stabilization to avoid a physically implausible divergence in the potential. The present work examines these issues for epitaxial growth of anatase TiO{sub 2} on strontium titanate (001). Solid phase epitaxial regrowth yields only the (001) facet, while direct crystalline growth by atomic layer deposition yields both the (112) and (001). The presence of amorphous TiO{sub 2} during regrowth may provide preferential stabilization for formation of the (001) facet.

  11. Nanoscale doping of compound semiconductors by solid phase dopant diffusion

    Ahn, Jaehyun, E-mail:; Koh, Donghyi; Roy, Anupam; Banerjee, Sanjay K., E-mail: [Department of Electrical and Computer Engineering, The University of Texas at Austin, Austin, Texas 78712 (United States); Chou, Harry [Materials Science and Engineering Program, University of Texas at Austin, Austin, Texas 78712 (United States); Kim, Taegon [Department of Electrical and Computer Engineering, The University of Texas at Austin, Austin, Texas 78712 (United States); Semiconductor R& D Center, Samsung Electronics Corporation, 1 Samsungjeonja-ro, Hwasung, Kyounggi 445-330 (Korea, Republic of); Song, Jonghan [Advanced Analysis Center, Korea Institute of Science and Technology, Cheongryang, P.O. Box 131, Seoul 130-650 (Korea, Republic of)


    Achieving damage-free, uniform, abrupt, ultra-shallow junctions while simultaneously controlling the doping concentration on the nanoscale is an ongoing challenge to the scaling down of electronic device dimensions. Here, we demonstrate a simple method of effectively doping ΙΙΙ-V compound semiconductors, specifically InGaAs, by a solid phase doping source. This method is based on the in-diffusion of oxygen and/or silicon from a deposited non-stoichiometric silicon dioxide (SiO{sub x}) film on InGaAs, which then acts as donors upon activation by annealing. The dopant profile and concentration can be controlled by the deposited film thickness and thermal annealing parameters, giving active carrier concentration of 1.4 × 10{sup 18 }cm{sup −3}. Our results also indicate that conventional silicon based processes must be carefully reviewed for compound semiconductor device fabrication to prevent unintended doping.

  12. A rapid easy—to—perform solid phase digoxin radioimmunoassay

    LiBin; ZhouMei-Ying; 等


    A solid-phase-radioimmunoassay(SPRIA) for the monitoring of blood digoxin level has been developed,in which a secondary antibody-coated polystyrene tubes are used.This noval method seems to be simple to use and only takes about an half hour.The standard curve is linear from 0.25to 4μg/L.The sensitivity of the detection is 0.1μg/L.Reproducibility studies with 3 control sera of 0.5-2.5μg/L give intraassay CV<5% and interassay CV<10%.The specimens are measured and compared with those of the conventional radioimmunoassay and the values are well correlated(r=0.96,Y=1.022X+0.04μg/L)。

  13. Solid-phase synthesis of siRNA oligonucleotides.

    Beaucage, Serge L


    Since the discovery of RNA interference (RNAi) as a means to silence the expression of specific genes, small interfering RNA (siRNA) oligonucleotides have been recognized as powerful tools for targeting therapeutically important mRNAs and eliciting their destruction. This discovery has created a high demand for synthetic oligoribonucleotides as potential therapeutics and has spurred a renaissance in the development of rapid, efficient methods for solid-phase RNA synthesis. The design and implementation of 2'-hydroxyl protecting groups that provide ribonucleoside phosphoramidites with coupling kinetics and coupling efficiencies comparable to those of deoxyribonucleoside phosphoramidites are key to the production of RNA oligonucleotides in sufficient quantity and purity for pharmaceutical applications. In this context, various siRNAs were chemically modified to identify the biophysical and biochemical parameters necessary for effective and stable RNAi-mediated gene-silencing activities.

  14. Use of molecularly imprinted solid-phase extraction for the selective clean-up of clenbuterol from calf urine

    Berggren, C; Bayoudh, S; Sherrington, D; Ensing, K


    A feasibility study was performed in order to study the possibilities in using molecularly imprinted polymers (MIPs) as sorbent material in solid-phase extraction (MISPE) for clean-up of clenbuterol from urine. A binding study of clenbuterol in several solvents was performed on a clenbuterol imprint

  15. Solid phase extraction for multiresidue analysis of anabolic steroids and related substances from calf urine using C18 and alumina columns

    Koole, A; Franke, JP; de Zeeuw, RA


    A solid phase extraction method for anabolic steroids and related substances in calf urine is reported, that is suitable as a screening method for illegal growth promoters. Two types of sorbent were used: a reversed phase C18 material and a polar alumina material. After overnight enzymatic deconjuga

  16. Thermodynamic Model Formulations for Inhomogeneous Solids with Application to Non-isothermal Phase Field Modelling

    Gladkov, Svyatoslav; Kochmann, Julian; Reese, Stefanie; Hütter, Markus; Svendsen, Bob


    The purpose of the current work is the comparison of thermodynamic model formulations for chemically and structurally inhomogeneous solids at finite deformation based on "standard" non-equilibrium thermodynamics [SNET: e. g. S. de Groot and P. Mazur, Non-equilibrium Thermodynamics, North Holland, 1962] and the general equation for non-equilibrium reversible-irreversible coupling (GENERIC) [H. C. Öttinger, Beyond Equilibrium Thermodynamics, Wiley Interscience, 2005]. In the process, non-isothermal generalizations of standard isothermal conservative [e. g. J. W. Cahn and J. E. Hilliard, Free energy of a non-uniform system. I. Interfacial energy. J. Chem. Phys. 28 (1958), 258-267] and non-conservative [e. g. S. M. Allen and J. W. Cahn, A macroscopic theory for antiphase boundary motion and its application to antiphase domain coarsening. Acta Metall. 27 (1979), 1085-1095; A. G. Khachaturyan, Theory of Structural Transformations in Solids, Wiley, New York, 1983] diffuse interface or "phase-field" models [e. g. P. C. Hohenberg and B. I. Halperin, Theory of dynamic critical phenomena, Rev. Modern Phys. 49 (1977), 435-479; N. Provatas and K. Elder, Phase Field Methods in Material Science and Engineering, Wiley-VCH, 2010.] for solids are obtained. The current treatment is consistent with, and includes, previous works [e. g. O. Penrose and P. C. Fife, Thermodynamically consistent models of phase-field type for the kinetics of phase transitions, Phys. D 43 (1990), 44-62; O. Penrose and P. C. Fife, On the relation between the standard phase-field model and a "thermodynamically consistent" phase-field model. Phys. D 69 (1993), 107-113] on non-isothermal systems as a special case. In the context of no-flux boundary conditions, the SNET- and GENERIC-based approaches are shown to be completely consistent with each other and result in equivalent temperature evolution relations.

  17. Materials Development for All-Solid-State Battery Electrolytes

    Wang, Weimin

    Solid electrolytes in all solid-state batteries, provide higher attainable energy density and improved safety. Ideal solid electrolytes require high ionic conductivity, a high elastic modulus to prevent dendrite growth, chemical compatibility with electrodes, and ease of fabrication into thin films. Although various materials types, including polymers, ceramics, and composites, are under intense investigation, unifying design principles have not been identified. In this thesis, we study the key ion transport mechanisms in relation to the structural characteristics of polymers and glassy solids, and apply derived material design strategies to develop polymer-silica hybrid materials with improved electrolyte performance characteristics. Poly(ethylene) oxide-based solid electrolytes containing ceramic nanoparticles are attractive alternatives to liquid electrolytes for high-energy density Li batteries. We compare the effect of Li1.3Al0.3Ti 1.7(PO4)3 active nanoparticles, passive TiO 2 nanoparticles and fumed silica. Up to two orders of magnitude enhancement in ionic conductivity is observed for composites with active nanoparticles, attributed to cation migration through a percolating interphase region that develops around the active nanoparticles, even at low nanoparticle loading. We investigate the structural origin of elastic properties and ionic migration mechanisms in sodium borosilicate and sodium borogermanate glass electrolyte system. A new statistical thermodynamic reaction equilibrium model is used in combination with data from nuclear magnetic resonance and Brillouin light scattering measurements to determine network structural unit fractions. The highly coordinated structural units are found to be predominantly responsible for effective mechanical load transmission, by establishing three-dimensional covalent connectivity. A strong correlation exists between bulk modulus and the activation energy for ion conduction. We describe the activated process in

  18. Phase nucleation and evolution mechanisms in heterogeneous solids

    Udupa, Anirudh

    Phase nucleation and evolution is a problem of critical importance in many applications. As the length scales are reduced, it becomes increasingly important to consider interfacial and micro-structural effects that can be safely ignored at larger length scales owing to randomness. The theory of phase nucleation has been addressed usually by the classical nucleation theory, which was originally derived for single component fluid systems, after making an assumption of equilibrium. The criterion has not been rigorously derived for solids, which are far from equilibrium due to dissipation by multiple physical drivers. In this thesis, a thermodynamically sound nucleation criterion is derived for systems with multiple interacting physical phenomena and multiple dissipating mechanisms. This is done, using the tools of continuum mechanics, by determining the change in free energy upon the introduction of a new nucleus into the system. The developed theory is demonstrated to be a generalization of the classical nucleation theory (CNT). The developed theory is then applied to the problem of electromigration driven void nucleation, a serious reliability concern for the microelectronics industry. The void grows and eventually severs the line making the chip nonfunctional. There are two classes of theories at present in the electromigration literature to address the problem of void nucleation, the vacancy supersaturation theory and the entropic dissipation theory, both of which are empirical and based on intuition developed from experimental observations. When the developed theory was applied to the problem of electromigration, it was found to be consistent with the vacancy supersaturation theory, but provided the correct energetic quantity, the chemical potential, which has contribution from both the vacancy concentration as well as the hydrostatic stress. An experiment, consisting of electromigration tests on serpentine lines, was developed to validate the developed

  19. Numerical study of light-induced phase behavior of smectic solids

    Chung, Hayoung; Park, Jaesung; Cho, Maenghyo


    By the chemical cross-linking of rigid molecules, liquid crystal polymer (LCP) has been envisaged as a novel heterogeneous material due to the fact that various optical and geometric states of the liquid crystalline (LC) phases are projected onto the polymeric constituents. The phase behavior, which refers to the macroscopic shape change of LCP under thermotropic phase change, is a compelling example of such optical-mechanical coupling. In this study, the photomechanical behavior, which broadly refers to the thermal- or light-induced actuation of smectic solids, is investigated using three-dimensional nonlinear finite element analysis (FEA). First, the various phases of LC are considered as well as their relation to polymeric conformation defined by the strain energy of the smectic polymer; a comprehensive constitutive equation that bridges the strong, optomechanical coupling is then derived. Such photomechanical coupling is incorporated in the FEA considering geometric nonlinearity, which is vital to understanding the large-scale light-induced bending behavior of the smectic solid.To demonstrate the simulation capability of the present model, numerous examples of photomechanical deformations are investigated parametrically, either by changing the operating conditions such as stimuli (postsynthesis) or the intrinsic properties (presynthesis). When compared to nematic solids, distinguished behaviors due to smectic substances are found herein and discussed through experiments. The quasisoftness that bidirectionally couples microscopic variables to mechanical behavior is also explained, while considering the effect of nonlinearity. In addition to providing a comprehensive measure that could deepen the knowledge of photomechanical coupling, the use of the proposed finite element framework offers an insight into the design of light-responsive actuating systems made of smectic solids.

  20. Comparative solution and solid-phase glycosylations toward a disaccharide library

    Agoston, K.; Kröger, Lars; Agoston, Agnes


    A comparative study on solution-phase and solid-phase oligosaccharide synthesis was performed. A 16-member library containing all regioisomers of Glc-Glc, Glc-Gal, Gal-Glc, and Gal-Gal disaccharides was synthesized both in solution and on solid phase. The various reaction conditions for different...

  1. Steady-state diffusion regime in solid-phase micro extraction kinetics

    Benhabib, K.; Laak, ter T.L.; Leeuwen, van H.P.


    The temporal evolution of diffusion-controlled analyte accumulation in solid-phase microextraction (SPME) is critically discussed in terms of the various aspects of steady-state diffusion in the two phases under conditions of fast exchange of the analyte at the solid phase film/water interface. For

  2. Solid-Phase Organic Chemistry: Synthesis of 2β-(HeterocyclylthiomethylPenam Derivatives on Solid Support

    Ernesto G. Mata


    Full Text Available The synthesis of 2β-(heterocyclylthiomethylpenam derivatives on solid support has been developed. Compounds are obtained in good to high yields (based on loading of the original resin. The key step is the solid-phase double rearrangement of the corresponding penicillin sulfoxide.

  3. The first order phase-transition of polycrystal solid surfaces with nanothickness

    Y.A. Minaev


    The fundamental equations of thermodynamics of a film have been used for describing a fundamental property of solid crystalline materials i.e. the first-order phase transition on the grain boundaries by the formation of two-dimensional liquid. The generalized equation that is obtained is used for calculating the premelting temperature of any metal, which has a value in the range of 0.55-0.86 of the melting point. The experimental diffusion coefficient of nitrogen in steel at premelting temperature is the same as in the liquid phase. The described phenomenon of phase transition on the grain boundaries decreases in case of radical modification of the existing process engineering of handling metals. It also provides a precise physical explanation to the super plasticity of fine-structure metal alloys.

  4. Test and Analysis of Solid Rocket Motor Nozzle Ablative Materials

    Clayton, J. Louie


    Asbestos free solid motor internal insulation samples were tested at the MSFC Hyperthermal Facility. Objectives of the test were to gather data for analog characterization of ablative and in-depth thermal performance of rubber materials subject to high enthalpy/pressure flow conditions. Tests were conducted over a range of convective heat fluxes for both inert and chemically reactive sub-sonic free stream gas flow. Instrumentation included use of total calorimeters, thermocouples, and a surface pyrometer for surface temperature measurement. Post-test sample forensics involved measurement of eroded depth, charred depth, total sample weight loss, and documentation of the general condition of the eroded profile. A complete Charring Material Ablator (CMA) style aero-thermal analysis was conducted for the test matrix and results compared to the measured data. In general, comparisons were possible for a number of the cases and the results show a limited predictive ability to model accurately both the ablative response and the in-depth temperature profiles. Lessons learned and modeling recommendations are made regarding future testing and modeling improvements that will increase understanding of the basic chemistry/physics associated with the complicated material ablation process of rubber materials.

  5. Ferroelectromagnetic solid solutions on the base piezoelectric ceramic materials for components of micromechatronics

    Bochenek, Dariusz; Zachariasz, Radosław; Niemiec, Przemysław; Ilczuk, Jan; Bartkowska, Joanna; Brzezińska, Dagmara


    In the presented work, a ferroelectromagnetic solid solutions based on PZT and ferrite powders have been obtained. The main aim of combination of ferroelectric and magnetic powders was to obtain material showing both electric and magnetic properties. Ferroelectric ceramic powder (in amount of 90%) was based on the doped PZT type solid solution while magnetic component was nickel-zinc ferrite Ni1-xZnxFe2O4 (in amount of 10%). The synthesis of components of ferroelectromagnetic solid solutions was performed using the solid phase sintering. Final densification of synthesized powder has been done using free sintering. The aim of the work was to obtain and examine in the first multicomponent PZT type ceramics admixed with chromium with the following chemical composition Pb0.94Sr0.06(Zr0.46Ti0.54)O3+0.25 at% Cr2O3 and next ferroelectromagnetic solid solution based on a PZT type ferroelectric powder (Pb0.94Sr0.06(Zr0.46Ti0.54)O3+0.25 at% Cr2O3) and nickel-zinc ferrite (Ni0.64Zn0.36Fe2O4), from the point of view of their mechanical and electric properties, such as: electric permittivity, ε; dielectric loss, tanδ; mechanical losses, Q-1; and Young modulus, E.

  6. Development of novel solid-phase protein formulations

    Montalvo Ortiz, Brenda Liz

    Proteins are the next-generation drugs for the treatment of several diseases. However, the number of protein drugs is still limited due to the physical or chemical instability of proteins during processing, formulation, storage, and delivery. The formulation of proteins at the solid state has advantages over liquid state, such as improved stability during long-term storage and delivery and decreases transportation costs. In this dissertation, we developed new solid-phase protein formulations in which the integrity of the protein was not compromised. The long term goal of this research was to use these protein formulations to improve protein stability in drug delivery devices, such as poly(lactic-co-glycolic) acid (PLGA). The first solid-phase protein formulation developed in this investigation was named "glassification". We proposed glassification as an alternative protein dehydration technique to the common used one, lyophilization, because this last method involves a series of steps which are detrimental to protein structure and stability. The glassification method consisted on protein dehydration by the use of organic solvents. As a result of the glassification process a small (micrometer size range) protein solid bead was obtained. The proteins used to study the glassification process were lysozyme (LYS), alpha-chymotrypsin (CHYMO) and horseradish peroxidase (HRP). These studies revealed that the glassification process itself did not alter protein structure and the activity was preserved. Ethyl acetate was the most effective organic solvent for protein glassification because it led to the highest protein residual activity, no insoluble aggregate formation and is a relatively non-toxic solvent, which allow the incorporation of these protein microparticles in PLGA microspheres. The incorporation of spherical HRP microparticles into PLGA microspheres resulted in superior properties when compared with encapsulated lyophilized HRP powder, such as improved release

  7. Challenges of infrared reflective spectroscopy of solid-phase explosives and chemicals on surfaces

    Phillips, Mark C.; Suter, Jonathan D.; Bernacki, Bruce E.; Johnson, Timothy J.


    Reliable active and passive hyperspectral imaging and detection of explosives and solid-phase chemical residue on surfaces remains a challenge and an active area of research and development. Both methods rely on reference libraries for material identification, but in many cases the reference spectra do not sufficiently resemble those instrumental signals scattered from real-world objects. We describe a physics-based model using the dispersive complex dielectric constant to explain what is often thought of as anomalous behavior of scattered or non-specular signatures encountered in active and passive sensing of explosives or chemicals on surfaces and show modeling and experimental results for RDX.

  8. Improving nutrient values of solid heavy phase for corn substitute in poultry diet

    A.P Sinurat; T Purwadaria; I.A.K Bintang; T Pasaribu


    Solid heavy phase (SHP), a by product material of palm oil factory obtained by ceramic filtration from liquid waste could be produced approximately 2 million tons/year. The by product has a potential for substituting corn in poultry feed. A series of experiment was carried out to improve nutrient value of the SHP in order to obtain a feedstuff that can substitute corn in poultry feed. The SHP was processed by either fermentation or enzymatic process. The product was then dried and analysed fo...

  9. Reducing the sulfur-dioxide binding power of sweet white wines by solid-phase extraction.

    Saidane, Dorra; Barbe, Jean-Christophe; Birot, Marc; Deleuze, Hervé


    The high sulfur-dioxide binding power of sweet white wines may be reduced by extracting the naturally present carbonyl compounds from wine that are responsible for carbonyl bisulphites formation. The carbonyl compounds mainly responsible for trapping SO2 are acetaldehyde, pyruvic acid, and 2-oxoglutaric acid. The method employed was selective solid phase extraction, using phenylsulfonylhydrazine as a scavenging agent. The scavenging function was grafted onto a support prepared from raw materials derived from lignin. This approach is more acceptable to winemakers than the polymer media previously reported, as it reduces the possible contamination of wine to molecules already present in the wine making process.

  10. Solid-liquid phase equilibria of Fe-Cr-Al alloys and spinels

    McMurray, J. W.; Hu, R.; Ushakov, S. V.; Shin, D.; Pint, B. A.; Terrani, K. A.; Navrotsky, A.


    Ferritic FeCrAl alloys are candidate accident tolerant cladding materials. There is a paucity of data concerning the melting behavior for FeCrAl and its oxides. Analysis tools have therefore had to utilize assumptions for simulations using FeCrAl cladding. The focus of this study is to examine in some detail the solid-liquid phase equilibria of FeCrAl alloys and spinels with the aim of improving the accuracy of severe accident scenario computational studies.

  11. Phase diagrams and kinetics of solid-liquid phase transitions in crystalline polymer blends

    Matkar, Rushikesh A.

    A free energy functional has been formulated based on an order parameter approach to describe the competition between liquid-liquid phase separation and solid-liquid phase separation. In the free energy description, the assumption of complete solvent rejection from the crystalline phase that is inherent in the Flory diluent theory was removed as solvent has been found to reside in the crystalline phase in the form of intercalates. Using this approach, we have calculated various phase diagrams in binary blends of crystalline and amorphous polymers that show upper or lower critical solution temperature. Also, the discrepancy in the chi values obtained from different experimental methods reported in the literature for the polymer blend of poly(vinylidenefluoride) and poly(methylmethacrylate) has been discussed in the context of the present model. Experimental phase diagram for the polymer blend of poly(caprolactone) and polystyrene has also been calculated. Of particular importance is that the crystalline phase concentration as a function of temperature has been calculated using free energy minimization methods instead of assuming it to be pure. In the limit of complete immiscibility of the solvent in the crystalline phase, the Flory diluent theory is recovered. The model is extended to binary crystalline blends and the formation of eutectic, peritectic and azeotrope phase diagrams has been explained on the basis of departure from ideal solid solution behavior. Experimental eutectic phase diagram from literature of a binary blend of crystalline polymer poly(caprolactone) and trioxane were recalculated using the aforementioned approach. Furthermore, simulations on the spatio temporal dynamics of crystallization in blends of crystalline and amorphous polymers were carried out using the Ginzburg-Landau approach. These simulations have provided insight into the distribution of the amorphous polymer in the blends during the crystallization process. The simulated results

  12. Sb-Te Phase-change Materials under Nanoscale Confinement

    Ihalawela, Chandrasiri A.

    Size, speed and efficiency are the major challenges of next generation nonvolatile memory (NVM), and phase-change memory (PCM) has captured a great attention due to its promising features. The key for PCM is rapid and reversible switching between amorphous and crystalline phases with optical or electrical excitation. The structural transition is associated with significant contrast in material properties which can be utilized in optical (CD, DVD, BD) and electronic (PCRAM) memory applications. Importantly, both the functionality and the success of PCM technology significantly depend on the core material and its properties. So investigating PC materials is crucial for the development of PCM technology to realized enhanced solutions. In regards to PC materials, Sb-Te binary plays a significant role as a basis to the well-known Ge-Sb-Te system. Unlike the conventional deposition methods (sputtering, evaporation), electrochemical deposition method is used due to its multiple advantages, such as conformality, via filling capability, etc. First, the controllable synthesis of Sb-Te thin films was studied for a wide range of compositions using this novel deposition method. Secondly, the solid electrolytic nature of stoichiometric Sb2Te3 was studied with respect to precious metals. With the understanding of 2D thin film synthesis, Sb-Te 1D nanowires (18 - 220 nm) were synthesized using templated electrodeposition, where nanoporous anodic aluminum oxide (AAO) was used as a template for the growth of nanowires. In order to gain the controllability over the deposition in high aspect ratio structures, growth mechanisms of both the thin films and nanowires were investigated. Systematic understanding gained thorough previous studies helped to formulate the ultimate goal of this dissertation. In this dissertation, the main objective is to understand the size effect of PC materials on their phase transition properties. The reduction of effective memory cell size in conjunction with

  13. Solid Phase Formylation of N-Terminus Peptides

    Anna Lucia Tornesello


    Full Text Available Formylation of amino groups is a critical reaction involved in several biological processes including post-translational modification of histones. The addition of a formyl group (CHO to the N-terminal end of a peptide chain generates biologically active molecules. N-formyl-peptides can be produced by different methods. We performed the N-formylation of two chemotactic hexapetides, Met1-Leu2-Lys3-Leu4-Ile5-Val6 and Met1-Met2-Tyr3-Ala4-Leu5-Phe6, carrying out the reaction directly on peptidyl-resin following pre-activation of formic acid with N,N-dicyclohexylcarbodiimmide (DCC in liquid phase. The overnight incubation at 4 °C resulted in a significant increase in production yields of formylated peptides compared to the reaction performed at room temperature. The method is consistently effective, rapid, and inexpensive. Moreover, the synthetic strategy can be applied for the formylation of all primary amines at N-terminus of peptide chains or amino groups of lysine side-chains in solid phase.

  14. Phase Change Material Heat Exchanger Life Test

    Lillibridge, Sean; Stephan, Ryan


    Low Lunar Orbit (LLO) poses unique thermal challenges for the orbiting space craft, particularly regarding the performance of the radiators. The IR environment of the space craft varies drastically from the light side to the dark side of the moon. The result is a situation where a radiator sized for the maximal heat load in the most adverse situation is subject to freezing on the dark side of the orbit. One solution to this problem is to implement Phase Change Material (PCM) Heat Exchangers. PCM Heat Exchangers act as a "thermal capacitor," storing thermal energy when there is too much being produced by the space craft to reject to space, and then feeding that energy back into the thermal loop when conditions are more favorable. Because they do not use an expendable resource, such as the feed water used by sublimators and evaporators, PCM Heat Exchangers are ideal for long duration LLO missions. In order to validate the performance of PCM Heat Exchangers, a life test is being conducted on four n-Pentadecane, carbon filament heat exchangers. Fluid loop performance, repeatability, and measurement of performance degradation over 2500 melt-freeze cycles will be performed.

  15. Review on thermal energy storage with phase change: materials, heat transfer analysis and applications

    Zalba, Belen; Marin, Jose M. [Dpto. Ingenieria Mecanica, Campus Politecnico, Universidad de Zaragoza, EUITIZ ' EDIFICIO B.3' Maria de Luna 3 (Actur), 50015, Zaragoza (Spain); Cabeza, Luisa F. [Dpt.d' Informatica i Enginyeria Industrial, Escola, Universitaria Politecnica, Universitat de Lleida, CREA, Jaurne 11,69,25001, Lleida (Spain); Mehling, Harald [ZAE Bayem, Division 1: Energy Conversion and Storage, Walther-Meissner-Str. 6, 85748, Garching (Germany)


    Thermal energy storage in general, and phase change materials (PCMs) in particular, have been a main topic in research for the last 20 years, but although the information is quantitatively enormous, it is also spread widely in the literature, and difficult to find. In this work, a review has been carried out of the history of thermal energy storage with solid-liquid phase change. Three aspects have been the focus of this review: materials, heat transfer and applications. The paper contains listed over 150 materials used in research as PCMs, and about 45 commercially available PCMs. The paper lists over 230 references. (Author)

  16. Microencapsulated Phase Change Composite Materials for Energy Efficient Buildings

    Thiele, Alexander

    This study aims to elucidate how phase change material (PCM)-composite materials can be leveraged to reduce the energy consumption of buildings and to provide cost savings to ratepayers. Phase change materials (PCMs) can store thermal energy in the form of latent heat when subjected to temperatures exceeding their melting point by undergoing a phase transition from solid to liquid state. Reversibly, PCMs can release this thermal energy when the system temperature falls below their solidification point. The goal in implementing composite PCM walls is to significantly reduce and time-shift the maximum thermal load on the building in order to reduce and smooth out the electricity demand for heating and cooling. This Ph.D. thesis aims to develop a set of thermal design methods and tools for exploring the use of PCM-composite building envelopes and for providing design rules for their practical implementation. First, detailed numerical simulations were used to show that the effective thermal conductivity of core-shell-matrix composites depended only on the volume fraction and thermal conductivity of the constituent materials. The effective medium approximation reported by Felske (2004) was in very good agreement with numerical predictions of the effective thermal conductivity. Second, a carefully validated transient thermal model was used to simulate microencapsulated PCM-composite walls subjected to diurnal or annual outdoor temperature and solar radiation flux. It was established that adding microencapsulated PCM to concrete walls both substantially reduced and delayed the thermal load on the building. Several design rules were established, most notably, (i) increasing the volume fraction of microencapsulated PCM within the wall increases the energy savings but at the potential expense of mechanical properties [1], (ii) the phase change temperature leading to the maximum energy and cost savings should equal the desired indoor temperature regardless of the climate

  17. Immunochemical cross-reactivity between albumin and solid-phase adsorbed histamine

    Poulsen, L K; Nolte, H; Søndergaard, I


    For production of an antibody against histamine, this was coupled to human serum albumin (HSA) and used for immunization of rabbits. To test the antiserum, an immunoradiometric assay was developed comprising solid-phase bound histamine, antisera and radiolabelled protein A. Titration and inhibition...... experiments revealed that histamine adsorbed onto a solid-phase could bind the antiserum. However, neither free histamine nor histamine coupled to unrelated carriers could inhibit the binding of antiserum to the solid-phase histamine. Cross-reactivity was demonstrated between HSA and solid-phase bound...

  18. Study on polyethylene glycol/epoxy resin composite as a form-stable phase change material

    Fang, Yutang; Kang, Huiying; Wang, Weilong; Liu, Hong; Gao, Xuenong [The Key Laboratory of Enhanced Heat Transfer and Energy Conservation, Ministry of Education, South China University of Technology, Guangzhou 510640 (China)


    Form-stable polyethylene glycol (PEG)/epoxy resin (EP) composite as a novel phase change material (PCM) was prepared using casting molding method. In this new material, PEG acts as the latent heat storage material and EP polymer serves as the supporting material, which provides structural strength and prevents the leakage of the melted PEG. The structure and morphology of the novel composite were observed using Fourier transformation infrared spectroscope (FTIR) and scanning electronic microscope (SEM). The thermo-mechanical property and transition behavior were characterized by polarizing optical microscope (POM), static thermo-mechanical analysis (TMA) and differential scanning calorimeter (DSC). The experimental results show that, as a result of the physical tangled function of the epoxy resin carrier to the PEG segment, the composite macroscopically presents the solid-solid phase change characteristic. (author)

  19. Study on polyethylene glycol/epoxy resin composite as a form-stable phase change material

    Fang Yutang, E-mail: [Key Laboratory of Enhanced Heat Transfer and Energy Conservation, Ministry of Education, South China University of Technology, Guangzhou 510640 (China); Kang Huiying; Wang Weilong; Liu Hong; Gao Xuenong [Key Laboratory of Enhanced Heat Transfer and Energy Conservation, Ministry of Education, South China University of Technology, Guangzhou 510640 (China)


    Form-stable polyethylene glycol (PEG)/epoxy resin (EP) composite as a novel phase change material (PCM) was prepared using casting molding method. In this new material, PEG acts as the latent heat storage material and EP polymer serves as the supporting material, which provides structural strength and prevents the leakage of the melted PEG. The structure and morphology of the novel composite were observed using Fourier transformation infrared spectroscope (FTIR) and scanning electronic microscope (SEM). The thermo-mechanical property and transition behavior were characterized by polarizing optical microscope (POM), static thermo-mechanical analysis (TMA) and differential scanning calorimeter (DSC). The experimental results show that, as a result of the physical tangled function of the epoxy resin carrier to the PEG segment, the composite macroscopically presents the solid-solid phase change characteristic.

  20. Laser-material interactions: A study of laser energy coupling with solids

    Shannon, M A [Lawrence Berkeley Lab., CA (United States)


    This study of laser-light interactions with solid materials ranges from low-temperature heating to explosive, plasma-forming reactions. Contained are four works concerning laser-energy coupling: laser (i) heating and (ii) melting monitored using a mirage effect technique, (iii) the mechanical stress-power generated during high-powered laser ablation, and (iv) plasma-shielding. First, a photothermal deflection (PTD) technique is presented for monitoring heat transfer during modulated laser heating of opaque solids that have not undergone phase-change. Of main interest is the physical significance of the shape, magnitude, and phase for the temporal profile of the deflection signal. Considered are the effects that thermophysical properties, boundary conditions, and geometry of the target and optical probe-beam have on the deflection response. PTD is shown to monitor spatial and temporal changes in heat flux leaving the surface due to changes in laser energy coupling. The PTD technique is then extended to detect phase-change at the surface of a solid target. Experimental data shows the onset of melt for indium and tin targets. The conditions for which melt can be detected by PTD is analyzed in terms of geometry, incident power and pulse length, and thermophysical properties of the target and surroundings. Next, monitoring high-powered laser ablation of materials with stress-power is introduced. The motivation for considering stress-power is given, followed by a theoretical discussion of stress-power and how it is determined experimentally. Experiments are presented for the ablation of aluminum targets as a function of energy and intensity. The stress-power response is analyzed for its physical significance. Lastly, the influence of plasma-shielding during high-powered pulsed laser-material interactions is considered. Crater size, emission, and stress-power are measured to determine the role that the gas medium and laser pulse length have on plasma shielding.

  1. Imprinted magnetic graphene oxide for the mini-solid phase extraction of Eu (III) from coal mine area

    Patra, Santanu; Roy, Ekta; Madhuri, Rashmi; Sharma, Prashant K.


    The present work represents the preparation of imprinted magnetic reduced graphene oxide and applied it for the selective removal of Eu (III) from local coal mines area. A simple solid phase extraction method was used for this purpose. The material shows a very high adsorption as well as removal efficiency towards Eu (III), which suggest that the material have potential to be used in future for their real time applications in removal of Eu (III) from complex matrices.

  2. Novel Materials and Devices for Solid-State Neutron Detection

    Manginell, Ronald P. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Pfeifer, Kent B. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)


    There is a need in many fields, such as nuclear medicine, non-proliferation, energy exploration, national security, homeland security, nuclear energy, etc, for miniature, thermal neutron detectors. Until recently, thermal neutron detection has required physically large devices to provide sufficient neutron interaction and transduction signal. Miniaturization would allow broader use in the fields just mentioned and open up other applications potentially. Recent research shows promise in creating smaller neutron detectors through the combination of high-neutron-cross-section converter materials and solid-state devices. Yet, till recently it is difficult to measure low neutron fluxes by solidstate means given the need for optimized converter materials (purity, chemical composition and thickness) and a lack of designs capable of efficient transduction of the neutron conversion products (x-rays, electrons, gamma rays). Gadolinium-based semiconductor heterojunctions have detected electrons produced by Gd-neutron reactions but only at high neutron fluxes. One of the main limitations to this type of approach is the use of thin converter layers and the inability to utilize all the conversion products. In this LDRD we have optimized the converter material thickness and chemical composition to improve capture of conversion electrons and have detected thermal neutrons with high fidelity at low flux. We are also examining different semiconductor materials and converter materials to attempt to capture a greater percentage of the conversion electrons, both low and higher energy varieties. We have studied detector size and bias scaling, and cross-sensitivity to xrays and shown that we can detect low fluxes of thermal neutrons in less than 30 minutes with high selectivity by our approach. We are currently studying improvements in performance with direct placement of the Gd converter on the detector. The advancement of sensitive, miniature neutron detectors will have benefits in

  3. On the formation of molecules and solid-state compounds from the AGB to the PN phases

    Garcia-Hernandez, D A


    During the asymptoyic giant branch (AGB) phase, different elements are dredge-up to the stellar surface depending on progenitor mass and metallicity. When the mass loss increases at the end of the AGB, a circumstellar dust shell is formed, where different (C-rich or O-rich) molecules and solid-state compounds are formed. These are further processed in the transition phase between AGB stars and planetary nebulae (PNe) to create more complex organic molecules and inorganic solid-state compounds (e.g., polycyclic aromatic hydrocarbons, fullerenes, and graphene precursors in C-rich environments and oxides and crystalline silicates in O-rich ones). We present an observational review of the different molecules and solid-state materials that are formed from the AGB to the PN phases. We focus on the formation routes of complex fullerene (and fullerene-based) molecules as well as on the level of dust processing depending on metallicity.

  4. On the formation of molecules and solid-state compounds from the AGB to the PN phases

    García-Hernández, D. A.; Manchado, A.


    During the asymptoyic giant branch (AGB) phase, different elements are dredge- up to the stellar surface depending on progenitor mass and metallicity. When the mass loss increases at the end of the AGB, a circumstellar dust shell is formed, where different (C-rich or O-rich) molecules and solid-state compounds are formed. These are further processed in the transition phase between AGB stars and planetary nebulae (PNe) to create more complex organic molecules and inorganic solid-state compounds (e.g., polycyclic aromatic hydrocarbons, fullerenes, and graphene precursors in C-rich environments and oxides and crystalline silicates in O-rich ones). We present an observational review of the different molecules and solid-state materials that are formed from the AGB to the PN phases. We focus on the formation routes of complex fullerene (and fullerene-based) molecules as well as on the level of dust processing depending on metallicity.

  5. A two-phase solid/fluid model for dense granular flows including dilatancy effects

    Mangeney, Anne; Bouchut, Francois; Fernandez-Nieto, Enrique; Koné, El-Hadj; Narbona-Reina, Gladys


    Describing grain/fluid interaction in debris flows models is still an open and challenging issue with key impact on hazard assessment [{Iverson et al.}, 2010]. We present here a two-phase two-thin-layer model for fluidized debris flows that takes into account dilatancy effects. It describes the velocity of both the solid and the fluid phases, the compression/dilatation of the granular media and its interaction with the pore fluid pressure [{Bouchut et al.}, 2016]. The model is derived from a 3D two-phase model proposed by {Jackson} [2000] based on the 4 equations of mass and momentum conservation within the two phases. This system has 5 unknowns: the solid and fluid velocities, the solid and fluid pressures and the solid volume fraction. As a result, an additional equation inside the mixture is necessary to close the system. Surprisingly, this issue is inadequately accounted for in the models that have been developed on the basis of Jackson's work [{Bouchut et al.}, 2015]. In particular, {Pitman and Le} [2005] replaced this closure simply by imposing an extra boundary condition at the surface of the flow. When making a shallow expansion, this condition can be considered as a closure condition. However, the corresponding model cannot account for a dissipative energy balance. We propose here an approach to correctly deal with the thermodynamics of Jackson's model by closing the mixture equations by a weak compressibility relation following {Roux and Radjai} [1998]. This relation implies that the occurrence of dilation or contraction of the granular material in the model depends on whether the solid volume fraction is respectively higher or lower than a critical value. When dilation occurs, the fluid is sucked into the granular material, the pore pressure decreases and the friction force on the granular phase increases. On the contrary, in the case of contraction, the fluid is expelled from the mixture, the pore pressure increases and the friction force diminishes. To

  6. Solid-fluid mixture microstructure design of composite materials with application to tissue engineering scaffold design

    Lin, Cheng-Yu

    The ability to design the material microstructure brings the use of composite materials into the next generation. In this paper, we report pioneering research to implement the computational material microstructure design into the internal architecture design for a tissue engineering scaffold. A tissue engineering design postulate is that scaffolds should match specified healthy tissue stiffness, while concurrently providing sufficient porosity for cell migration and tissue regeneration. Employing the inverse homogenization method and the adaptive topology optimization method, a complex 3D microstructure can be designed to perform with the anisotropic elastic stiffness and porosities analogous to a native bone specimen. Besides the elastic stiffness from its solid part, fluid in the porous region also plays an important role in tissue engineering. The flow of fluid through the pores brings nutrients to cells in the tissue matrix and also removes their waste. Fluid permeability of cylinderical trabecular bone grafts was found to predict clinical success. Deriving from Darcy's Law, we developed software to calculate the homogenized fluid permeability of 3D cancellous voxel models, which were directly reconstructed from micro-CT images. Furthermore, an Evolutionary Structural Optimization (ESO) algorithm was utilized to maximize fluid permeability in the microstructure. The fluid optimization scheme was then collaborated with solid phase optimization through Multidisciplinary Design Optimization (MDO) to create an integrated solid-fluid mixture microstructure design. In addition, to ensure the fabrication feasibility, we also implemented a post-optimization process to enhance design results by improving the dynamic stiffness to eliminate weak connections and checkerboard pattern. The design scaffolds were then built by an indirect solid freeform fabrication (SFF) technique using various bio-compatible materials and ready for further investment. This computational

  7. Vacuum-assisted headspace solid phase microextraction of polycyclic aromatic hydrocarbons in solid samples.

    Yiantzi, Evangelia; Kalogerakis, Nicolas; Psillakis, Elefteria


    For the first time, Vacuum Assisted Headspace Solid Phase Microextraction (Vac-HSSPME) is used for the recovery of polycyclic aromatic hydrocarbons (PAHs) from solid matrices. The procedure was investigated both theoretically and experimentally. According to the theory, reducing the total pressure increases the vapor flux of chemicals at the soil surface, and hence improves HSSPME extraction kinetics. Vac-HSSPME sampling could be further enhanced by adding water as a modifier and creating a slurry mixture. For these soil-water mixtures, reduced pressure conditions may increase the volatilization rates of compounds with a low K(H) present in the aqueous phase of the slurry mixture and result in a faster HSSPME extraction process. Nevertheless, analyte desorption from soil to water may become a rate-limiting step when significant depletion of the aqueous analyte concentration takes place during Vac-HSSPME. Sand samples spiked with PAHs were used as simple solid matrices and the effect of different experimental parameters was investigated (extraction temperature, modifiers and extraction time). Vac-HSSPME sampling of dry spiked sand samples provided the first experimental evidence of the positive combined effect of reduced pressure and temperature on HSSPME. Although adding 2 mL of water as a modifier improved Vac-HSSPME, humidity decreased the amount of naphthalene extracted at equilibrium as well as impaired extraction of all analytes at elevated sampling temperatures. Within short HSSPME sampling times and under mild sampling temperatures, Vac-HSSPME yielded linear calibration curves in the range of 1-400 ng g(-1) and, with the exception of fluorene, regression coefficients were found higher than 0.99. The limits of detection for spiked sand samples ranged from 0.003 to 0.233 ng g(-1) and repeatability from 4.3 to 10 %. Finally, the amount of PAHs extracted from spiked soil samples was smaller compared to spiked sand samples, confirming that soil could bind target

  8. Novel Nanostructured Solid Materials for Modulating Oral Drug Delivery from Solid-State Lipid-Based Drug Delivery Systems.

    Dening, Tahnee J; Rao, Shasha; Thomas, Nicky; Prestidge, Clive A


    Lipid-based drug delivery systems (LBDDS) have gained significant attention in recent times, owing to their ability to overcome the challenges limiting the oral delivery of poorly water-soluble drugs. Despite the successful commercialization of several LBDDS products over the years, a large discrepancy exists between the number of poorly water-soluble drugs displaying suboptimal in vivo performances and the application of LBDDS to mitigate their various delivery challenges. Conventional LBDDS, including lipid solutions and suspensions, emulsions, and self-emulsifying formulations, suffer from various drawbacks limiting their widespread use and commercialization. Accordingly, solid-state LBDDS, fabricated by adsorbing LBDDS onto a chemically inert solid carrier material, have attracted substantial interest as a viable means of stabilizing LBDDS whilst eliminating some of the various limitations. This review describes the impact of solid carrier choice on LBDDS performance and highlights the importance of appropriate solid carrier material selection when designing hybrid solid-state LBDDS. Specifically, emphasis is placed on discussing the ability of the specific solid carrier to modulate drug release, control lipase action and lipid digestion, and enhance biopharmaceutical performance above the original liquid-state LBDDS. To encourage the interested reader to consider their solid carrier choice on a higher level, various novel materials with the potential for future use as solid carriers for LBDDS are described. This review is highly significant in guiding future research directions in the solid-state LBDDS field and fostering the translation of these delivery systems to the pharmaceutical marketplace.

  9. Solid-State Physics An Introduction to Principles of Materials Science

    Ibach, Harald


    This new edition of the popular introduction to solid-state physics provides a comprehensive overview on basic theoretical and experimental concepts of material science. Additional sections emphasize current topics in solid-state physics. Notably, sections on important devices, aspects of non-periodic structures of matter, phase transitions, defects, superconductors and nanostructures have been added, the chapters presenting semi- and superconductivity had been completly updated. Students will benefit significantly from solving the exercises given at the end of each chapter. This book is intended for university students in physics, engineering and electrical engineering. This edition has been carefully revised, updated, and enlarged. Among the key recent developments incorporated throughout GMR (giant magneto resistance), thin-film magnetic properties, magnetic hysteresis and domain walls, quantum transport, metamaterials, and preparation techniques for nanostructures. From a review of the original edition �...

  10. Laboratory Evaluation of Nitrile Fuel Tank Materials (Phase 2)


    Laboratory Evaluation of Nitrile Fuel Tank Materials (Phase II) by James M. Sloan, David Flanagan, Daniel DeSchepper, Paul Touchet, and...21005-5066 ARL-TR-6627 September 2013 Laboratory Evaluation of Nitrile Fuel Tank Materials (Phase II) James M. Sloan, David Flanagan, and...COVERED (From - To) October 2011–March 2013 4. TITLE AND SUBTITLE Laboratory Evaluation of Nitrile Fuel Tank Materials (Phase II) 5a. CONTRACT NUMBER

  11. Modeling the solid-liquid phase transition in saturated triglycerides

    Pink, David A.; Hanna, Charles B.; Sandt, Christophe; MacDonald, Adam J.; MacEachern, Ronald; Corkery, Robert; Rousseau, Dérick


    We investigated theoretically two competing published scenarios for the melting transition of the triglyceride trilaurin (TL): those of (1) Corkery et al. [Langmuir 23, 7241 (2007)], in which the average state of each TL molecule in the liquid phase is a discotic "Y" conformer whose three chains are dynamically twisted, with an average angle of ˜120° between them, and those of (2) Cebula et al. [J. Am. Oil Chem. Soc. 69, 130 (1992)], in which the liquid-state conformation of the TL molecule in the liquid phase is a nematic h∗-conformer whose three chains are in a modified "chair" conformation. We developed two competing models for the two scenarios, in which TL molecules are in a nematic compact-chair (or "h") conformation, with extended, possibly all-trans, chains at low-temperatures, and in either a Y conformation or an h∗ conformation in the liquid state at temperatures higher than the phase-transition temperature, T∗=319 K. We defined an h-Y model as a realization of the proposal of Corkery et al. [Langmuir 23, 7241 (2007)], and explored its predictions by mapping it onto an Ising model in a temperature-dependent field, performing a mean-field approximation, and calculating the transition enthalpy ΔH. We found that the most plausible realization of the h-Y model, as applied to the solid-liquid phase transition in TL, and likely to all saturated triglycerides, gave a value of ΔH in reasonable agreement with the experiment. We then defined an alternative h-h∗ model as a realization of the proposal of Cebula et al. [J. Am. Oil Chem. Soc. 69, 130 (1992)], in which the liquid phase exhibits an average symmetry breaking similar to an h conformation, but with twisted chains, to see whether it could describe the TL phase transition. The h-h∗ model gave a value of ΔH that was too small by a factor of ˜3-4. We also predicted the temperature dependence of the 1132 cm-1 Raman band for both models, and performed measurements of the ratios of three TL Raman

  12. Selective Separation of Fe-Concentrates in EAF Slags Using Mechanical Dissimilarity of Solid Phases

    Jung, Sung Suk; Jung, Keeyoung; Sohn, Il


    We sought to develop an optimized particle size-dependent separation method to lower the Fe content of pulverized glass-ceramic electric arc furnace (EAF) slag for its improved reclamation as construction materials by considering the structures and the mechanical behavior of the discrete solid phases. After an isothermal crystallization process to enhance the spinel growth, the Vickers hardness and fracture toughness were measured on the spinel and amorphous phases separately from the solidified slag using indentation methods. The characteristic differences in the hardness of the phases were magnified when this glass-ceramic composite was isothermally crystallized. The hardness of the spinel was observed to be lower in slags with higher FetO/Al2O3 mass ratios due to the triclinic unit cell expansion of the spinel, whereas the hardness of the amorphous phase decreased with increasing isothermal period because of the structural transformation into a silicate-dominant network. Fracture toughness could be calculated based on the hardness and crack length, where the Young's modulus was determined using nanoindentation. The amorphous phase with a lower Fe content and lower fracture toughness resulted in finer powder distribution after pulverization, allowing better separation of the primary crystalline spinel containing higher Fe content from the Fe-deficient amorphous phase according to the particle size.

  13. Preparation of Pt/C Catalyst with Solid Phase Reaction Method


    The Pt/C catalyst was prepared with solid phase reaction method (Pt/C(S)) for the first time. Its performances were compared with that prepared by the traditional liquid phase reaction method. The results demonstrate that the electrocatalytic activity of Pt/C catalyst with solid phase reaction method for methanol oxidation is higher than that with liquid phase reaction method. XRD and TEM measurements indicate that the Pt/C(S) possesses low crystalline extent and small particle size.

  14. Analysis of Phase Separation in High Performance PbTe–PbS Thermoelectric Materials

    Girard, Steven N. [Northwestern University; Schmidt-Rohr, Klaus [Ames Laboratory; Chasapis, Thomas C. [Northwestern University; Hatzikraniotis, Euripides [Aristotle University of Thessaloniki; Njegic, B. [Ames Laboratory; Levin, E. M. [Ames Laboratory; Rawal, A. [Ames Laboratory; Paraskevopoulos, Konstantios M. [Aristotle University of Thessaloniki; Kanatzidis, Mercouri G. [Northwestern University


    Phase immiscibility in PbTe–based thermoelectric materials is an effective means of top-down synthesis of nanostructured composites exhibiting low lattice thermal conductivities. PbTe1-x Sx thermoelectric materials can be synthesized as metastable solid solution alloys through rapid quenching. Subsequent post-annealing induces phase separation at the nanometer scale, producing nanostructures that increase phonon scattering and reduce lattice thermal conductivity. However, there has yet to be any study investigating in detail the local chemical structure of both the solid solution and nanostructured variants of this material system. Herein, quenched and annealed (i.e., solid solution and phase-separated) samples of PbTe–PbS are analyzed by in situ high-resolution synchrotron powder X-ray diffraction, solid-state 125Te nuclear magnetic resonance (NMR), and infrared (IR) spectroscopy analysis. For high concentrations of PbS in PbTe, e.g., x >16%, NMR and IR analyses reveal that rapidly quenched samples exhibit incipient phase separation that is not detected by state-of-the-art synchrotron X-ray diffraction, providing an example of a PbTe thermoelectric “alloy” that is in fact phase inhomogeneous. Thermally-induced PbS phase separation in PbTe–PbS occurs close to 200 °C for all compositions studied, and the solubility of the PbS phase in PbTe at elevated temperatures >500 °C is reported. The findings of this study suggest that there may be a large number of thermoelectric alloy systems that are phase inhomogeneous or nanostructured despite adherence to Vegard's Law of alloys, highlighting the importance of careful chemical characterization to differentiate between thermoelectric alloys and composites.

  15. Molecularly imprinted solid phase extraction of fluconazole from pharmaceutical formulations.

    Manzoor, S; Buffon, R; Rossi, A V


    This work encompasses a direct and coherent strategy to synthesise a molecularly imprinted polymer (MIP) capable of extracting fluconazole from its sample. The MIP was successfully prepared from methacrylic acid (functional monomer), ethyleneglycoldimethacrylate (crosslinker) and acetonitrile (porogenic solvent) in the presence of fluconazole as the template molecule through a non-covalent approach. The non-imprinted polymer (NIP) was prepared following the same synthetic scheme, but in the absence of the template. The data obtained from scanning electronic microscopy, infrared spectroscopy, thermogravimetric and nitrogen Brunauer-Emmett-Teller plot helped to elucidate the structural as well as the morphological characteristics of the MIP and NIP. The application of MIP as a sorbent was demonstrated by packing it in solid phase extraction cartridges to extract fluconazole from commercial capsule samples through an offline analytical procedure. The quantification of fluconazole was accomplished through UPLC-MS, which resulted in LOD≤1.63×10(-10) mM. Furthermore, a high percentage recovery of 91±10% (n=9) was obtained. The ability of the MIP for selective recognition of fluconazole was evaluated by comparison with the structural analogues, miconazole, tioconazole and secnidazole, resulting in percentage recoveries of 51, 35 and 32%, respectively.

  16. Automated Solid-Phase Radiofluorination Using Polymer-Supported Phosphazenes

    Bente Mathiessen


    Full Text Available The polymer supported phosphazene bases PS-P2tBu and the novel PS-P2PEG allowed for efficient extraction of [18F]F− from proton irradiated [18O]H2O and subsequent radiofluorination of a broad range of substrates directly on the resin. The highest radiochemical yields were obtained with aliphatic sulfonates (69% and bromides (42%; the total radiosynthesis time was 35–45 min. The multivariate analysis showed that the radiochemical yields and purities were controlled by the resin load, reaction temperature, and column packing effects. The resins could be reused several times with the same or different substrates. The fully automated on-column radiofluorination methodology was applied to the radiosynthesis of the important PET radiotracers [18F]FLT and [18F]FDG. The latter was produced with 40% yield on a 120 GBq scale and passed GMP-regulated quality control required for commercial production of [18F]FDG. The combination of compact form factor, simplicity of [18F]F− recovery and processing, and column reusability can make solid phase radiofluorination an attractive radiochemistry platform for the emerging dose-on-demand instruments for bedside production of PET radiotracers.

  17. Binding of properdin to solid-phase immune complexes

    Junker, A; Baatrup, G; Svehag, S E


    The capacity of serum to support deposition of C3, properdin and factor B was studied by enzyme-linked immunosorbent assay using solid-phase immune complexes (IC) for activation of complement. Deposition of C3 and properdin occurred in fairly dilute normal human serum (NHS), but factor B uptake...... was hardly detectable. Alternative pathway-mediated deposition of C3 with slow kinetics was demonstrated in C2-deficient serum and in NHS depleted of C1q, factor D and properdin (C1qDP-depleted serum) after reconstitution with factor D and properdin. Efficient uptake of properdin required a functional...... classical pathway, in the presence of which C3 and properdin were rapidly deposited onto the IC. Judging from findings in C3-deficient serum, factor I-deficient serum, and C1qDPB-depleted serum, the uptake of properdin was strictly C3-dependent, and did not require the presence of factors B and D. Thus, C3b...

  18. Microwave heating in solid-phase peptide synthesis.

    Pedersen, Søren L; Tofteng, A Pernille; Malik, Leila; Jensen, Knud J


    The highly refined organic chemistry in solid-phase synthesis has made it the method of choice not only to assemble peptides but also small proteins - mainly on a laboratory scale but increasingly also on an industrial scale. While conductive heating occasionally has been applied to peptide synthesis, precise microwave irradiation to heat the reaction mixture during coupling and N(α)-deprotection has become increasingly popular. It has often provided dramatic reductions in synthesis times, accompanied by an increase in the crude peptide purity. Microwave heating has been proven especially relevant for sequences which might form β-sheet type structures and for sterically difficult couplings. The beneficial effect of microwave heating appears so far to be due to the precise nature of this type of heating, rather than a peptide-specific microwave effect. However, microwave heating as such is not a panacea for all difficulties in peptide syntheses and the conditions may need to be adjusted for the incorporation of Cys, His and Asp in peptides, and for the synthesis of, for example, phosphopeptides, glycopeptides, and N-methylated peptides. Here we provide a comprehensive overview of the advances in microwave heating for peptide synthesis, with a focus on systematic studies and general protocols, as well as important applications. The assembly of β-peptides, peptoids and pseudopeptides are also evaluated in this critical review (254 references).

  19. Solid-phase microextraction and the human fecal VOC metabolome.

    Emma Dixon

    Full Text Available The diagnostic potential and health implications of volatile organic compounds (VOCs present in human feces has begun to receive considerable attention. Headspace solid-phase microextraction (SPME has greatly facilitated the isolation and analysis of VOCs from human feces. Pioneering human fecal VOC metabolomic investigations have utilized a single SPME fiber type for analyte extraction and analysis. However, we hypothesized that the multifarious nature of metabolites present in human feces dictates the use of several diverse SPME fiber coatings for more comprehensive metabolomic coverage. We report here an evaluation of eight different commercially available SPME fibers, in combination with both GC-MS and GC-FID, and identify the 50/30 µm CAR-DVB-PDMS, 85 µm CAR-PDMS, 65 µm DVB-PDMS, 7 µm PDMS, and 60 µm PEG SPME fibers as a minimal set of fibers appropriate for human fecal VOC metabolomics, collectively isolating approximately 90% of the total metabolites obtained when using all eight fibers. We also evaluate the effect of extraction duration on metabolite isolation and illustrate that ex vivo enteric microbial fermentation has no effect on metabolite composition during prolonged extractions if the SPME is performed as described herein.

  20. Phase I studies of porfiromycin (NSC--56410) in solid tumors.

    Grage, T B; Weiss, A J; Wilson, W; Reynolds, V


    Porfiromycin was given to a group of patients with a variety of solid tumors. Of 114 patients admitted to the study, 103 yielded evaluable data. The following dosage schedules were used to determine the toxicity of porfiromycin when given in multiple doses by intravenous injection: 0.2 mg/kg x 5 days, 0.3 mg/kg x 5 days, 0.35 mg/kg x 5 days, 0.4 mg/kg x 5 days, 0.24 mg/kg x 10 days and 0.6 mg/kg weekly. Toxic effects noted were mainly leukopenia, thrombocytopenia, and, when injected paravenously, local tissue necrosis. Biological effects were noted at all dosage levels and were more severe at the higher dosages. The data suggest that profiromycin administered intravenously at a dose of 0.35 mg/kg daily for 5 days results in moderate hermatological toxicity and clinical evaluation in a Phase II study at this dosage level is indicated.

  1. Automated solid-phase peptide synthesis to obtain therapeutic peptides

    Veronika Mäde


    Full Text Available The great versatility and the inherent high affinities of peptides for their respective targets have led to tremendous progress for therapeutic applications in the last years. In order to increase the drugability of these frequently unstable and rapidly cleared molecules, chemical modifications are of great interest. Automated solid-phase peptide synthesis (SPPS offers a suitable technology to produce chemically engineered peptides. This review concentrates on the application of SPPS by Fmoc/t-Bu protecting-group strategy, which is most commonly used. Critical issues and suggestions for the synthesis are covered. The development of automated methods from conventional to essentially improved microwave-assisted instruments is discussed. In order to improve pharmacokinetic properties of peptides, lipidation and PEGylation are described as covalent conjugation methods, which can be applied by a combination of automated and manual synthesis approaches. The synthesis and application of SPPS is described for neuropeptide Y receptor analogs as an example for bioactive hormones. The applied strategies represent innovative and potent methods for the development of novel peptide drug candidates that can be manufactured with optimized automated synthesis technologies.

  2. Headspace solid-phase microextraction for wine volatile analysis.

    Azzi-Achkouty, Samar; Estephan, Nathalie; Ouaini, Naïm; Rutledge, Douglas N


    The most commonly used technique to prepare samples for the analysis of wine volatile is the headspace solid-phase microextraction (HS-SPME). This method has gained popularity in last few years, as it is a unique solventless preparation technique. In this paper, a summary of recently published studies using HS-SPME for the analysis of wine aromas, with special emphasis on the method developed, has been compiled. Several papers are discussed in detail, mainly with respect to the SPME conditions used. A brief summary of the reviews related to HS-SPME analysis is given and discussed. Several parameters affecting the HS-SPME, such as the salt concentration and the agitation conditions, are used in the same way as used in several papers. The HS-SPME extraction proved to be sufficiently sensitive to satisfy legislative requirements related to low detection and quantification limits as well as method accuracy and precision requirements. However, in order to achieve the best performance and precision, the protocol needs to be optimized for each case. The effect of different parameters must be well characterized to ensure correct extraction and desorption to ensure the transfer of extracted compounds into the analytical system. The operating parameters, such as time, temperature, and agitation, must then be kept constant for all the samples.

  3. Laser (cooling) refrigeration in erbium based solid state materials

    Lynch, Jonathan W.

    The objective of this study was to investigate the potential of erbium based solid state materials for laser refrigeration in bulk material. A great deal of work in the field has been focused on the use of ytterbium based ZBLAN glass. Some experiments have also reported cooling in thulium based solid state materials but with considerably less success. We proposed that erbium had many attractive features compared to ytterbium and therefore should be tried for cooling. The low lying energy level structure of erbium provides energy levels that could bring obtainable temperatures two orders of magnitude lower. Erbium transitions of interest for cooling fall in the near IR region (0.87 microns and 1.5 microns). Lasers for one of these transitions, in the 1.5 micron region, are well developed for communication and are in the eye-safe and water and atmosphere transparent region. Theoretical calculations are also presented so as to identify energy levels of the eleven 4f electrons in Er3+ in Cs2NaYCl 6:Er3+ and the transitions between them. The strengths of the optical transitions between them have been calculated. Knowledge of such energy levels and the strength of the laser induced transitions between them is crucial for understanding the refrigeration mechanisms and different energy transfer pathways following the laser irradiation. The crystal host for erbium was a hexa-chloro-elpasolite crystal, Cs 2NaYCl6:Er3+ with an 80% (stoichiometric) concentration of erbium. The best cooling results were obtained using the 0.87 micron transition. We have demonstrated bulk cooling in this crystal with a temperature difference of ~6.2 K below the surrounding temperature. The temperatures of the crystal and its immediate surrounding environment were measured using differential thermometry. Refrigeration experiments using the 1.5 micron transition were performed and the results are presented. The demonstrated temperature difference was orders of magnitude smaller. Only a temperature

  4. Energy efficiency of buildings with phase-change materials

    Lukić Predrag


    Full Text Available The construction of energy efficient buildings using innovative building materials such as phase change materials, in addition to improving indoor comfort, energy savings and costs, can be achieved by increasing their market value. Because of its ability to absorb and release energy at predictable temperatures, phase change materials are effective in controlling and maintaining the thermal environment in the building. The use of phase changing materials, materials stored latent energy storage is an effective form of heat. [Projekat Ministarstva nauke Republike Srbije, br. TR36016: Experimental and theoretical investigation of frames and plates with semi-rigid connections from the view of the second order theory and stability analysis

  5. Study on the Motion state of Powdery materials in Dense-phase Pneumatic Conveying Pipe

    Lia Zhihua


    Full Text Available Using the method of computational fluid dynamics, a model is created about powdery materials flowing in the dense-phase pneumatic conveying pipe. the motion state powdery materials flowing in the horizontal and vertical pipe is simulated. It is found that in the horizontal pipe the powdery materials represent the flow of dune-like state, and continuously move forward in this form, the volume fraction of powdery materials at the pipe's bottom is large, the velocity is low; In the vertical pipe, the columnar solid-plug can form and scatter continuously, and the motion state is closer to fluidization.

  6. Nanoscale Phase Immiscibility in High-ZT Bulk Lead Telluride Thermoelectric Materials

    Girard, Steven Neal

    Renewable energy initiatives have increased interest in thermoelectric materials as an option for inexpensive and environmentally friendly waste heat-to-power generation. Unfortunately, low efficiencies have limited their wide-scale utilization. This work describes the synthesis and characterization of bulk nanostructured thermoelectric materials wherein natural phase immiscibility is manipulated to selectively generate nanoscale inclusions of a second phase that improve their efficiency through reductions in lattice thermal conductivity. The PbTe-PbS system exhibits natural phase separation by nucleation and growth or spinodal decomposition phase transformations depending on composition and temperature treatment. Through rapid quenching, nearly ideal solid solution alloys of PbTe-PbS are observed by powder X-ray diffraction. However, characterization by solid-state NMR and IR reflectivity show that solid solutions are obtained for rapidly quenched samples within the nucleation and growth region of the phase diagram, but samples within the spinodal decomposition region exhibit very slight phase immiscibility. We report the temperatures of phase separation using high temperature powder X-ray diffraction. Microscopy reveals that phase separation in PbTe-PbS naturally produces nanoinclusions. A decrease in lattice thermal conductivity is observed as a result of the solid solution-to-nanostructured phase transformation in this materials system, increasing thermoelectric figure of merit. Sn addition to PbTe-PbS produces a pseudobinary system of PbTe-PbSnS 2. This materials system produces microscale lamellae that effectively reduce lattice thermal conductivity. Unfortunately, the PbSnS2 inclusions also scatter electrons, reducing electrical conductivity and producing only a minimal increase in thermoelectric figure of merit. We additionally investigate PbSnS2 as prepared through Bridgman crystal growth. PbTe-PbS doped with Na appears to increase the kinetic rate of

  7. Determining the solid phases hosting arsenic in Mekong Delta sediments

    Wucher, M.; Stuckey, J. W.; McCurdy, S.; Fendorf, S.


    The major river systems originating from the Himalaya deposit arsenic bearing sediment into the deltas of South and Southeast Asia. High rates of sediment and organic carbon deposition combined with frequent flooding leads to anaerobic processes that release arsenic into the pore-water. Arsenic concentrations in the groundwater of these sedimentary basins are often above the World Health Organization drinking water standard of 10 μg As L-1. As a result, 150 million people are at risk of chronic arsenic poisoning through water and rice consumption. The composition of the iron bearing phases hosting the arsenic in these deltaic sediments is poorly understood. Here we implemented a suite of selective chemical extractions to help constrain the types of arsenic bearing solid phases, which were complimented with synchrotron-based X-ray absorption spectroscopy and X-ray diffraction analyses to define the arsenic and iron mineralogy of the system. Sediment cores were collected in triplicate from a seasonally-inundated wetland in Cambodia at depths of 10, 50, 100, and 150 centimeters. We hypothesize that (i) arsenic will be predominantly associated with iron oxides, and (ii) the ratio of crystalline to amorphous iron oxides will increase with sediment depth (and age). We performed four selective extractions in parallel to quantify the various pools of arsenic. First, 1 M MgCl2 was used to extract electrostatically-bound arsenic (labile forms) from the sediment. Second, 1 M NaH2PO4 targeted strongly adsorbed arsenic. Third, 1 M HCl was used to liberated arsenic coprecipitated with amorphous Fe/Mn oxides, carbonates, and acid-volatile sulfides. Finally, a dithionite extraction was used to account for arsenic associated with reducible Fe/Mn oxides. Through this work, we identified the composition of the phases hosting arsenic at various depths through the soil profile, improving our understanding of how arsenic persists in the aquifer. In addition, defining the arsenic and

  8. An acid-stable tert-butyldiarylsilyl (TBDAS) linker for solid-phase organic synthesis.

    Diblasi, Christine M; Macks, Daniel E; Tan, Derek S


    [reaction: see text] A new, robust tert-butyldiarylsilyl (TBDAS) linker has been developed for solid-phase organic synthesis. This linker is stable to both protic and Lewis acidic reaction conditions, overcoming a significant limitation of previously reported silyl linkers. Solid-phase acetal deprotection, olefination, asymmetric allylation, and silyl protecting group deblocking reactions have been demonstrated with TBDAS-linked substrates.


    A. R. Koohpaei ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani


    Full Text Available Solid phase extraction is one of the major applications of molecularly imprinted polymers fields for clean-up of environmental and biological samples namely molecularly imprinted solid-phase extraction. In this study, solid phase extraction using the imprinted polymer has been optimized with the experimental design approach for a triazine herbicide, named atrazine with regard to the critical factors which influence the molecular imprinted solid phase extraction efficiency such as sample pH, concentration, flow-rate, volume, elution solvent, washing solvent and sorbent mass. Optimization methods that involve changing one factor at a time can be laborious. A novel approach for the optimization of imprinted solid-phase extraction using chemometrics is described. The factors were evaluated statistically and also validated with spiked water samples and showed a good reproducibility over six consecutive days as well as six within-day experiments. Also, in order to the evaluate efficiency of the optimized molecularly imprinted solid-phase extraction protocols, enrichment capacity, reusability and cross-reactivity of cartridges have been also evaluated. Finally, selective molecularly imprinted solid-phase extraction of atrazine was successfully demonstrated with a recovery above 90% for spiked drinking water samples. It was concluded that the chemometrics is frequently employed for analytical method optimization and based on the obtained results, it is believed that the central composite design could prove beneficial for aiding the molecularly imprinted polymer and molecularly imprinted solid-phase extraction development.

  10. Facile synthesis of aliphatic isothiocyanates and thioureas on solid phase using peptide coupling reagents

    Boas, Ulrik; Andersen, Heidi Gertz; Christensen, Jørn B.;


    Peptide coupling reagents can be used as versatile reagents for the formation of aliphatic isothiocyanates and thioureas on solid phase from the corresponding solid-phase anchored aliphatic primary amines. The formation of the thioureas is fast and highly chemoselective, and proceeds via formation...

  11. The Iron-Iron Carbide Phase Diagram: A Practical Guide to Some Descriptive Solid State Chemistry.

    Long, Gary J.; Leighly, H. P., Jr.


    Discusses the solid state chemistry of iron and steel in terms of the iron-iron carbide phase diagram. Suggests that this is an excellent way of introducing the phase diagram (equilibrium diagram) to undergraduate students while at the same time introducing the descriptive solid state chemistry of iron and steel. (Author/JN)

  12. Complement fixation by solid phase immune complexes. Reduced capacity in SLE sera

    Baatrup, G; Jonsson, H; Sjöholm, A


    We describe an ELISA for assessment of complement function based on the capacity of serum to support fixation of complement components to solid phase immune complexes (IC). Microplates were coated with aggregated bovine serum albumin (BSA) followed by rabbit anti-BSA IgG. The solid phase IC were ...

  13. Solid-state retrodirective phased array concepts for microwave power transmission from Solar Power Satellite

    Schroeder, K. G.; Petroff, I. K.


    Two prototype solid-state phased array systems concepts for potential use in the Solar Power Satellite are described. In both concepts, the beam is centered on the rectenna by means of phase conjugation of a pilot signal emanating from the ground. Also discussed is on-going solid-state amplifier development.

  14. Solid State NMR Studies of Energy Conversion and Storage Materials

    Jankuru Hennadige, Sohan Roshel De Silva

    NMR (Nuclear magnetic resonance) spectroscopy is utilized to study energy conversion and storage materials. Different types of NMR techniques including Magic Angle Spinning, Cross-polarization and relaxation measurement experiments were employed. Four different projects are discussed in this dissertation. First, three types of CFx battery materials were investigated. Electrochemical studies have demonstrated different electrochemical performances by one type, delivering superior performance over the other two. 13C and 19F MAS NMR techniques are employed to identify the atomic/molecular structural factors that might account for differences in electrochemical performance among different types. Next as the second project, layered polymer dielectrics were investigated by NMR. Previous studies have shown that thin film capacitors are improved by using alternate layers of two polymers with complementary properties: one with a high breakdown strength and one with high dielectric constant as opposed to monolithic layers. 13C to 1H cross-polarization techniques were used to investigate any inter-layer properties that may cause the increase in the dielectric strength. The third project was to study two types of thermoelectric materials. These samples were made of heavily doped phosphorous and boron in silicon by two different methods: ball-milled and annealed. These samples were investigated by NMR to determine the degree of disorder and obtain insight into the doping efficiency. The last ongoing project is on a lithium-ion battery system. The nature of passivating layers or the solid electrolyte interphase (SEI) formed on the electrodes surface is important because of the direct correlation between the SEI and the battery life time/durability. Multinuclear (7Li, 19F, 31P) techniques are employed to identify the composition of the SEI formation of both positive and negative electrodes.

  15. Solid residues from Italian municipal solid waste incinerators: A source for "critical" raw materials.

    Funari, Valerio; Braga, Roberto; Bokhari, Syed Nadeem Hussain; Dinelli, Enrico; Meisel, Thomas


    The incineration of municipal solid wastes is an important part of the waste management system along with recycling and waste disposal, and the solid residues produced after the thermal process have received attention for environmental concerns and the recovery of valuable metals. This study focuses on the Critical Raw Materials (CRM) content in solid residues from two Italian municipal waste incinerator (MSWI) plants. We sampled untreated bottom ash and fly ash residues, i.e. the two main outputs of common grate-furnace incinerators, and determined their total elemental composition with sensitive analytical techniques such as XRF and ICP-MS. After the removal of a few coarse metallic objects from bottom ashes, the corresponding ICP solutions were obtained using strong digestion methods, to ensure the dissolution of the most refractory components that could host significant amounts of precious metals and CRM. The integration of accurate chemical data with a substance flow analysis, which takes into account the mass balance and uncertainties assessment, indicates that bottom and fly ashes can be considered as a low concentration stream of precious and high-tech metals. The magnesium, copper, antimony and zinc contents are close to the corresponding values of a low-grade ore. The distribution of the elements flow between bottom and fly ash, and within different grain size fractions of bottom ash, is appraised. Most elements are enriched in the bottom ash flow, especially in the fine grained fractions. However, the calculated transfer coefficients indicate that Sb and Zn strongly partition into the fly ashes. The comparison with available studies indicates that the CRM concentrations in the untreated solid residues are comparable with those residues that undergo post-treatment beneficiations, e.g. separation between ferrous and non-ferrous fractions. The suggested separate collection of "fresh" bottom ash, which could be processed for further mineral upgrading, can

  16. Solid-state thermochromism and phase transitions of charge transfer 1,3-diamino-4,6-dinitrobenzene dyes.

    Lee, Jong Hoon; Naumov, Pance; Chung, Ihn Hee; Lee, Sang Cheol


    The lower 1,3-bis(hydroxyalkylamino) homologues of the strong intramolecular X-type charge transfer (CT) system 1,3-diamino-4,6-dinitrobenzene (DADNB) exhibit reversible color change in the solid state from yellow at room temperature (RT) to orange and red at high temperature (HT). To investigate the structural prerequisites for occurrence of this phenomenon, we prepared 10 new derivatives of DADNB where the hydroxyalkyl arms at the amino groups were replaced with substituents having different electronic and steric profiles. Two of the new materials exhibit sharp and reversible thermochromic change in the solid state: when heated, the bis(aminoethyl) derivative (DADNB-1) undergoes color change from orange-red to brown, while one of the three polymorphs of the bisphenyl product (DADNB-2) changes its color from red to yellow. The physicochemical analysis and the crystal structures of seven of these compounds, one of which is trimorphic, confirmed that both phenomena are due to solid-solid phase transitions. The brown high-temperature phase of DADNB-1 presents the first example where the absorption is shifted beyond the red region. Form C of DADNB-2 is the first material of this group that exhibits "negative" thermochromism, where the high-temperature phase absorbs at lower wavelength than the low-temperature one. The results demonstrate the potentials of these simple and easily accessible organic molecular materials for thermal switching of the optical properties by utility of intermolecular interactions to modulate the intramolecular CT.

  17. Local Gas Phase Flow Characteristics of a Gas—Liquid—Solid Three—Phase Reversed Flow Jet Loop Reactor

    WENJianping; ChenYunlin; 等


    The local gas-phase flow characteristics such as local gas holdup (εg), local bubble velocity (Vb) and local bubble mean diameter(db) at a specified point in a gas-liquid-solid three-phase reversed flow jet loop reactor was experimentally investigated by a five-point conductivity probe. The effects of gas jet flow rate, liquid jet flow rate, solid loading, nozzle diameter and axial position on the local εg,Vb and db profiles were discussed. The presence of solids at low solid concentrations not only increased the local εg and Vb, but also decreased the local db. The optimum solid olading for the maximum local εg and Vb together with the minimum local db was 0.16×10-3m3, corresponding to a solid volume fraction,εS=2.5%.

  18. Material growth and characterization for solid state devices

    Collis, Ward J.; Abul-Fadl, A.; Iyer, S.


    During this period InGaAs and InGaAsP were grown on (100)InP by liquid phase electroepitaxy (LPEE). Results of the epitaxial growth of InGaAs on sputtered quartz masked substrates are presented. The resulting surface morphology can be related to the current density distribution near the edges of a masked pattern. The quaternary InGaAs was grown with compositions corresponding to 1.3 micron and 1.5 micron emission wavelengths. Growth rates were found to be linearly dependent upon current density, and a strong dependence upon composition was noted. These compositions lie in the miscibility gap region of the alloy phase diagram at the 645 C growth temperature. Growths were performed at 685 C to avoid the miscibility gap. Epilayers were characterized by photoluminescence, X-ray diffraction, secondary ion mass spectrometry, and Hall effect measurements. Aluminum oxide was deposited on silicon and InGaAs substrates for the characterization of this material as an insulator in a field effect transistor structure. It was determined that the results did not warrant further work with the deposition from an aluminum isopropoxide source. A metallographic vapor phase epitaxy system installation is nearing completion for use in hybrid III-V semiconductor epilayer growths.

  19. Inhibition of a solid phase reaction among excipients that accelerates drug release from a solid dispersion with aging.

    Mizuno, Masayasu; Hirakura, Yutaka; Yamane, Ikuro; Miyanishi, Hideo; Yokota, Shoji; Hattori, Munetaka; Kajiyama, Atsushi


    Hydrophobic drug substances can be formulated as a solid dispersion or solution using macromolecular matrices with high glass transition temperatures to attain satisfactory dissolution. However, very few marketed products have previously relied on solid dispersion technology due to physical and chemical instability problems, and processing difficulties. In the present study, a modified release product of a therapeutic drug for hypertension, Barnidipine hydrochloride, was developed. The drug product consisted of solid dispersion based on a matrix of carboxymethylethylcellulose (CMEC), which was produced using the spray-coating method. An enteric coat layer was sprayed on the surface of the solid dispersion to control drug release. Interestingly, the release rate accelerated as the drug product aged, while there were no indications of deceleration of the release rate which was due to crystallization of the drug substance. To prevent changes in the dissolution kinetics during storage periods, a variety of processing conditions were tried. It was found that not only use of non-aqueous solvents but also a reduction in coating temperatures consistently resulted in stable solid dispersions. The molecular bases of dissolution of the drug substance from those matrices were investigated. The molecular weight of CMEC was found to be a dominant factor that determined dissolution kinetics, which followed zero-order release, suggesting an involvement of an osmotic pumping mechanism. While dissolution was faster using a higher molecular weight CMEC, the molecular weight of CMEC in the drug product slowly increased with aging (solid phase reaction) depending on the processing conditions, causing the time-induced elevation of dissolution. While no crystalline components were found in the solid dispersion, the amorphous structure maintained a degree of non-equilibrium by nature. Plasticization by water in the coating solution relaxed the amorphous system and facilitated phase

  20. Application of solid waste containing lead for gamma ray shielding material



    Abstract. The basic strategies to decrease solid waste disposal problems have focused on the reduction of waste production and recovery of usable materials using waste and making raw materials. Generally, various materials have been used for radiation shielding in different areas and situations. In this study, a novel shielding material produced by a metallurgical solid waste containing lead has been analyzed in order to make a shielding material against gamma radiation. The photon total mass...

  1. Alternative anode materials for solid oxide fuel cells

    Goodenough, John B.; Huang, Yun-Hui [Texas Materials Institute, ETC 9.102, 1 University Station, C2200, The University of Texas at Austin, Austin, TX 78712 (United States)


    The electrolyte of a solid oxide fuel cell (SOFC) is an O{sup 2-}-ion conductor. The anode must oxidize the fuel with O{sup 2-} ions received from the electrolyte and it must deliver electrons of the fuel chemisorption reaction to a current collector. Cells operating on H{sub 2} and CO generally use a porous Ni/electrolyte cermet that supports a thin, dense electrolyte. Ni acts as both the electronic conductor and the catalyst for splitting the H{sub 2} bond; the oxidation of H{sub 2} to H{sub 2}O occurs at the Ni/electrolyte/H{sub 2} triple-phase boundary (TPB). The CO is oxidized at the oxide component of the cermet, which may be the electrolyte, yttria-stabilized zirconia, or a mixed oxide-ion/electron conductor (MIEC). The MIEC is commonly a Gd-doped ceria. The design and fabrication of these anodes are evaluated. Use of natural gas as the fuel requires another strategy, and MIECs are being explored for this application. The several constraints on these MIECs are outlined, and preliminary results of this on-going investigation are reviewed. (author)

  2. Stress-Induced Phase Transformation in Incompressible Materials and Stability of Multi-Phase Deformation


    The stress-induced phase transformation in incompressible materials and the interfacial stability of multi-phase deformation were studied. The existence of multi-phase deformation was determined through exploring whether the material would lose the strong ellipticity at some deformation gradient.Then, according to the stability criterion which is based on a quasi-static approach, the stability of the multi-phase deformation in incompressible materials was investigated by studying the growth/decay behaviour of the interface in the undeformed configuration when it is perturbed. At last, the way to define multi-phase deformation in incompressible materials was concluded and testified by a corresponding numerical example.

  3. Modeling of Impact Properties of Auxetic Materials: Phase 1


    underlying metal substrate from impact damage will be determined, and compared to the effect of solid polymer coatings (containing no honeycomb shaped air...higher indentation resistance, higher fracture toughness and greater resistance to impact damage . These unique features of the auxetic materials make... Elastoplasticity of auxetic materials, Computational Material Science, in press. [24] Horrigan, E.J., Smith, C.W., Scarpa, F.L., Gaspar, N., Javadi, A.A

  4. New Lithium Solid Electrolytes, Thio-Lisicon Materials Design Concept and Application to Solid State Battery

    Kanno, Ryoji; Murayama, Masahiro; Sakamoto, Kazuyuki


    Materials design concept of the new crystalline 'thio-LlSICON' (LIthium Superlonic CONductor) family was discussed. The thio-LISICON was found in the ternary systems, Li2S-MS2-M'xSy (M=Si, Ge, M'=P, Sb, Al, Zn, etc), and showed the highest conductivity of 2.2 × 10-3 Scm-1 at 25°C of any sintered ceramic, together with negligible electronic conductivity, high electrochemical stability, no reaction with lithium metal, and no phase transition up to 300°C. The advantage and disadvantage of the crystalline materials were discussed based on the ionic conduction, chemical stability and electrochemical potential window.

  5. Two and three dimensional electron backscattered diffraction analysis of solid oxide cells materials

    Saowadee, Nath

    in solid oxide fuel cell and electrolysis cell. Conductivity of STN is one of the important properties that researchers desire to improve. Grin boundary conductivity contributes to the overall conductivity of the STN. Grain boundary density controlled by mainly grain growth in material processing. Grain...... boundary migration in grain growth involves grain boundary mobility and net pressure on it. Thus grain boundary energy and pressure of STN were calculated in this work. Secondary phase is undesired in STN and YSZ synthesis. The secondary phase in ceramics with the same compounds can have different lattice...... the lattice constant. Both 2D and 3D EBSD were used in acquiring microstructure and crystallographic information of STN and YSZ. Prior to EBSD data collection, effect of FIB milling on STN and YSZ was investigated to optimize EBSD data quality and acquisition time for 3D-EBSD experiments by FIB serial...

  6. Pressure Effects on Solid State Phase Transformation of Aluminium Bronze in Cooling Process

    WANG Hai-Yan; CHEN Yan; LIU Yu-Wen; LI Fei; LIU Jian-Hua; PENG Gui-Rong; WANG Wen-Kui


    Effects of high pressure (6 GPa) on the solid state phase transformation kinetic parameters of aluminum bronze during the cooling process are investigated, based on the measurement and calculation of its solid state phase transformation temperature, duration and activation energy and the observation of its microstructures. The results show that high pressure treatment can reduce the solid phase transformation temperature and activation energy in the cooling process and can shorten the phase transformation duration, which is favorable when forming fine-grained aluminum bronze.

  7. The importance of screening solid-state phases of a racemic modification of a chiral drug: thermodynamic and structural characterization of solid-state phases of etiracetam.

    Herman, Christelle; Vermylen, Valérie; Norberg, Bernadette; Wouters, Johan; Leyssens, Tom


    In this contribution different solid-state forms of the racemic compound (RS)-2-(2-oxo-pyrrolidin-1yl)-butyramide are studied from a structural and thermal point of view. Three different solid-state phases were identified, including two polymorphs and one hydrate phase. Comparison is made with the structure of the (S)-enantiomer, for which only one solid-state phase is known. The basic structural motif found in both polymorphs of the racemic compound is similar, but the basic motif observed for the hydrate differs. These synthons could in principle be used in future polymorph prediction studies to screen for possible alternative forms of the enantiopure compound. Based on the structure of the hydrate, further efforts should therefore be made in order to identify a hydrate structure of the enantiopure compound. Studying the different phases of a racemic compound can therefore help to guide polymorphic screening of an enantiopure compound.

  8. Solid and liquid phase equilibria and solid-hydrate formation in binary mixtures of water with amines

    车冠全; 彭文烈; 黄良恩; 古喜兰; 车飙


    Solid and liquid phase diagrams have been constructed for {water+triethylamine,or+N,N-dimethylformamide(DMF) or+N,N-dimethlacetamide (DMA)} Solid-hydrates form with the empirical formulae N(C2H5)3 3H2O,DMF 3H2O,DMF 2H2O,DMA 3H2O and (DMA)2 3H2O.All are congruently melting except the first which melts incongruently.The solid-hydrate formation is attributed to hydrogen bond.The results are compared with the references

  9. Quaternary ammonium-functionalized silica sorbents for the solid-phase extraction of aromatic amines under normal phase conditions.

    Vidal, Lorena; Robin, Orlane; Parshintsev, Jevgeni; Mikkola, Jyri-Pekka; Riekkola, Marja-Liisa


    Quaternary ammonium-functionalized silica materials were synthesized and applied for solid-phase extraction (SPE) of aromatic amines, which are classified as priority pollutants by US Environmental Protection Agency. Hexamethylenetetramine used for silica surface modification for the first time was employed as SPE sorbent under normal phase conditions. Hexaminium-functionalized silica demonstrated excellent extraction efficiencies for o-toluidine, 4-ethylaniline and quinoline (recoveries 101-107%), while for N,N-dimethylaniline and N-isopropylaniline recoveries were from low to moderate (14-46%). In addition, the suitability of 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica as SPE sorbent was tested under normal phase conditions. The recoveries achieved for the five aromatic amines ranged from 89 to 99%. The stability of the sorbent was evaluated during and after 150 extractions. Coefficients of variation between 4.5 and 10.2% proved a high stability of the synthesized sorbent. Elution was carried out using acetonitrile in the case of hexaminium-functionalized silica and water for 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica sorbent. After the extraction the analytes were separated and detected by liquid chromatography ultraviolet detection (LC-UV). The retention mechanism of the materials was primarily based on polar hydrogen bonding and π-π interactions. Comparison made with activated silica proved the quaternary ammonium-functionalized materials to offer different selectivity and better extraction efficiencies for aromatic amines. Finally, 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica sorbent was successfully tested for the extraction of wastewater and soil samples.

  10. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Herrero Latorre, C., E-mail: [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)


    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  11. Solid phase epitaxial regrowth of (100)GaAs

    Almonte, Marlene Isabel [California Univ., Berkeley, CA (United States). Dept. of Materials Science and Mineral Engineering


    This thesis showed that low temperature (250°C) SPE of stoichiometrically balanced ion implanted GaAs layers can yield good epitaxial recovery for doses near the amorphization threshold. For 250°C anneals, most of the regrowth occurred in the first 10 min. HRTEM revealed much lower stacking fault density in the co-implanted sample than in the As-only and Ga-only samples with comparable doses. After low temp annealing, the nonstoichiometric samples had a large number of residual defects. For higher dose implants, very high temperatures (700°C) were needed to remove residual defects for all samples. The stoichiometrically balanced layer did not regrow better than the Ga-only and As-only samples. The co-implanted sample exhibited a thinner amorphous layer and a room temperature (RT) annealing effect. The amorphous layer regrew about 5 nm, suggesting that stoichiometrically balanced amorphous layers can regrow even at RT. Mechanisms for solid phase crystallization in (100)GasAs is discussed: nucleation and growth of randomly oriented crystallites and SPE. These two mechanisms compete in compound semiconductors at much lower temperatures than in Si. For the low dose As-only and Ga-only samples with low-temp anneals, both mechanisms are active. For this amorphization threshold dose, crystallites remain in the amorphous layer for all as-implants. 250°C annealing showed recrystallization from the surface and bulk for these samples; for the co-implant, the mechanism is not evident.

  12. Ultrarapid mutation detection by multiplex, solid-phase chemical cleavage

    Rowley, G.; Saad, S.; Giannelli, F.; Green, P.M. [Guy`s & St. Thomas`s Hospitals, London (United Kingdom)


    The chemical cleavage of mismatches in heteroduplexes formed by probe and test DNA detects and locates any sequence change in long DNA segments ({approximately}1.8 kb), and its efficiency has been well tested in the analysis of both average (e.g., coagulation factor IX) and large, complex genes (e.g., coagulation factor VIII and dystrophin). In the latter application RT/PCR products allow the examination of all essential sequences of the gene in a minimum number of reactions. We use two specific chemical reactants (hydroxylamine and osmium tetroxide) and piperidine cleavage of the above procedure to develop a very fast mutation screening method. This is based on: (1) 5{prime} or internal fluorescent labeling to allow concurrent screening of three to four DNA fragments and (2) solid-phase chemistry to use a microliter format and reduce the time required for the procedure, from amplification of sequence to gel loading inclusive, to one person-working-day. We test the two variations of the method, one entailing 5{prime} labeling of probe DNA and the other uniform labeling of both probe and target DNA, by detecting 114 known hemophilia B (coagulation factor IX) mutations and by analyzing 129 new patients. Uniform labeling of both probe and target DNA prior to formation of the heteroduplexes leads to almost twofold redundancy in the ability to detect mutations. Alternatively, the latter procedure may offer very efficient though less than 100% screening for sequence changes with only hydroxylamine. The full method with two chemical reactions (hydroxylamine and osmium tetroxide) should allow one person to screen with virtually 100% accuracy more than 300 kb of sequence in three ABI 373 gels in 1 day. 26 refs., 7 figs., 1 tab.

  13. Porous, High Capacity Coatings for Solid Phase Microextraction by Sputtering.

    Diwan, Anubhav; Singh, Bhupinder; Roychowdhury, Tuhin; Yan, DanDan; Tedone, Laura; Nesterenko, Pavel N; Paull, Brett; Sevy, Eric T; Shellie, Robert A; Kaykhaii, Massoud; Linford, Matthew R


    We describe a new process for preparing porous solid phase microextraction (SPME) coatings by the sputtering of silicon onto silica fibers. The microstructure of these coatings is a function of the substrate geometry and mean free path of the silicon atoms, and the coating thickness is controlled by the sputtering time. Sputtered silicon structures on silica fibers were treated with piranha solution (a mixture of concd H2SO4 and 30% H2O2) to increase the concentration of silanol groups on their surfaces, and the nanostructures were silanized with octadecyldimethylmethoxysilane in the gas phase. The attachment of this hydrophobic ligand was confirmed by X-ray photoelectron spectroscopy and contact angle goniometry on model, planar silicon substrates. Sputtered silicon coatings adhered strongly to their surfaces, as they were able to pass the Scotch tape adhesion test. The extraction time and temperature for headspace extraction of mixtures of alkanes and alcohols on the sputtered fibers were optimized (5 min and 40 °C), and the extraction performances of SPME fibers with 1.0 or 2.0 μm of sputtered silicon were compared to those from a commercial 7 μm poly(dimethylsiloxane) (PDMS) fiber. For mixtures of alcohols, aldehydes, amines, and esters, the 2.0 μm sputtered silicon fiber yielded signals that were 3-9, 3-5, 2.5-4.5, and 1.5-2 times higher, respectively, than those of the commercial fiber. For the heavier alkanes (undecane-hexadecane), the 2.0 μm sputtered fiber yielded signals that were approximately 1.0-1.5 times higher than the commercial fiber. The sputtered fibers extracted low molecular weight analytes that were not detectable with the commercial fiber. The selectivity of the sputtered fibers appears to favor analytes that have both a hydrophobic component and hydrogen-bonding capabilities. No detectable carryover between runs was noted for the sputtered fibers. The repeatability (RSD%) for a fiber (n = 3) was less than 10% for all analytes tested


    Yuliya Modna


    Full Text Available The acute destructive pneumonias (ADP occupy up to 80% of the total number of pneumonias. They require constant improvement of treatment strategy. Nowadays the use of surfactants is a part of most treatment protocols. The aim was to study the features of the solid phase bronchoalveolar lavage in children with the ADPs in the dynamics of complex treatment with exogenous surfactant.Material and methods: We examined 39 patients of contaminated surgery. We identified 2 groups of patients. The patients of first group (n=27 had pulmonary pleural form of ADP, the second group (n=12 had pulmonary form of ADP. All patients got classical treatment and the earlier draining of pleural cavity. We used as an antiseptic reamberin 1.5% by 10 ml/kg and endobronchially injected exogenous surfactant Bl in dose12 mg/kg body weight a day, 6 mg/kg every 12 hours. All the children were made a bronchoscopy to obtain BAL to study the crystallization properties. The solid phase of BAL was studied by method of cuneal dehydration.Results: All facies before treatment were divided into two groups according to classification of facies of biological fluids. Only the facies of the second and the third types were detected there. It was revealed that the sizes of the zones of the facies were different in the comparison groups before treatment and after. And the level of crystalline structures and amorphous aggregates were different in the groups with different degrees of inflammation.Conclusion: So, we can assume that the change in surfactant system is characterized by changes in the morphological structure of solids phases of BAL. And the morphological structure of BAL depends on the chemical composition of BAL.

  15. Solid-phase laser-induced forward transfer of variable shapes using a liquid-crystal spatial light modulator

    Pohl, R.; Jansink, M.; Römer, G. R. B. E.; Huis in `t Veld, A. J.


    Laser-induced forward transfer is a promising method for 3D printing of various materials, including metals. The ejection mechanism is complex and depends strongly on the experimental parameters, such as laser fluence and donor layer thickness. However, the process can be categorized by the physical condition of the ejected material, i.e., the donor layer is transferred in liquid phase or the material is transferred as a `pellet' in solid phase. Currently, solid-phase transfer faces several problems. Large shearing forces, occurring at the pellet perimeter during transfer, limit the similarity between the desired pellet shape and the deposited pellet shape. Furthermore, the deposited pellet may be surrounded by debris particles formed by undesired transferred donor material. This work introduces a novel approach for laser-induced forward transfer of variable shaped solid-phase pellets. A liquid-crystal spatial light modulator (SLM) is used to apply grayscale intensity modulation to an incident laser beam to shape the intensity profile. Optimized beams consist of a high fluence perimeter around an interior characterized by a lower fluence level. These beams are used successfully to transfer solid-phase pellets out of a 100-nm Au donor layer using a single laser pulse. The flexibility of the SLM allows a variable desired pellet shape. The shapes of the resulting deposited pellets show a high degree of similarity to the desired shapes. Debris-free deposited pellets are achieved by pre-machining the donor layer, prior to the transfer, using a double-pulse process.

  16. A New Kind of Shape-stabilized Phase Change Materials

    XIAO Liguang; DING Rui; SUN Hao; WANG Fujun


    Based on the lowest melting point and Schroeder's theoretical calculation formula, nanomodified organic composite phase change materials (PCMs) were prepared. The phase transition temperature and the latent heat of the materials were 24 ℃ and 172 J/g, respectively. A new shape-stabilized phase change materials were prepared, using high density polyethylene as supporting material. The PCM kept the shape when temperature was higher than melting point. Thus, it can directly contact with heat transfer media. The structure,morphology and thermal behavior of PCM were analyzed by FTIR, SEM and DSC.

  17. Effective utilization of incinerated municipal solid waste incineration ash: zeolitic material synthesis and silica extraction.

    Bac, Bui Hoang; Song, Yungoo; Moon, Yonghee; Kim, Myung Hun; Kang, Il Mo


    In this study the effective utilization of two types of municipal solid waste incinerator (MSWI) ashes, namely air-cooled ash (ACS) and water-cooled ash (WCS) samples obtained from a municipal solid waste incineration plant, was examined by applying zeolitic material synthesis and silica extraction. The influence of the experimental conditions including the ratio of sample : NaOH solution, the reaction temperature and time, and the concentration of NaOH solution were investigated. The results for the 25 experimental trials can be summarized as: (1) the formation of tobermorite and/or pectolite-1A as a major component in most conditions; (2) the synthesis of hydroxycancrinite as a major phase at 200 degrees C; (3) a dramatic increase in the extracted SiO(2) yield at 1 : 30 value of sample : NaOH ratio and 200 degrees C, even at short reaction times; and (4) relatively high SiO(2) yields for WCS ashes rather than ACS ashes. An increase in the reaction time improved the quantity of synthesized zeolitic materials. The reaction temperature determined the type of zeolite. An increase in the NaOH concentration can be an essential factor to improve zeolitic material synthesis, but it significantly reduced the yield of SiO(2) extraction. In conclusion, suitable conditions for obtaining both SiO(2) extraction and synthesized zeolites from the ashes of the incinerated solid waste materials should be: 200 degrees C reaction temperature; a 1 : 30 (g : mL) value for the sample : NaOH ratio; 2 mol L(-1) NaOH concentration; and a reaction time of more than 24 h.

  18. Phase Equilibrium Investigations of Planetary Materials

    Grove, T. L.


    This grant provided funds to carry out experimental studies designed to illuminate the conditions of melting and chemical differentiation that has occurred in planetary interiors. Studies focused on the conditions of mare basalt generation in the moon's interior and on processes that led to core formation in the Shergottite Parent Body (Mars). Studies also examined physical processes that could lead to the segregation of metal-rich sulfide melts in an olivine-rich solid matrix. The major results of each paper are discussed below and copies of the papers are attached as Appendix I.

  19. Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

    Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina


    Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction.

  20. Investigating the potential of metal-organic framework material as an adsorbent for matrix solid-phase dispersion extraction of pesticides during analysis of dehydrated Hyptis pectinata medicinal plant by GC/MS.

    Aquino, Adriano; Ferreira, Jordana Alves; Navickiene, Sandro; Wanderley, Kaline A; de Sá, Gilberto F; Júnior, Severino A


    Metal-organic frameworks aluminum terephthalate MIL-53 and Cu-benzene-1,3,5-tricarboxylate (BTC) were tested for extraction of pyrimethanil, ametryn, dichlofluanid, tetraconazole, flumetralin, kresoximmethyl, and tebuconazole from the medicinal plant Hyptis pectinata, with analysis using GC/MS in the selected ion monitoring mode. Experiments carried out at different fortification levels (0.1, 0.5, and 1.0 microg/g) resulted in recoveries in the range 61 to 107% with RSD values between 3 and 12% for the metal-organic framework materials. Detection and quantification limits ranged from 0.02 to 0.07 and 0.05 to 0.1 microg/g, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.04-20.0 microg/g), with correlation coefficients ranging from 0.9987 to 0.9998. Comparison of MIL-53 and Cu-BTC with C18-bonded silica showed good performance of the MIL-53 metal-organic framework as a sorbent for the pesticides tested.

  1. Thermomechanics of solid materials with application to the Gurson-Tvergaard material model

    Santaoja, K. [VTT Manufacturing Technology, Espoo (Finland). Materials and Structural Integrity


    The elastic-plastic material model for porous material proposed by Gurson and Tvergaard is evaluated. First a general description is given of constitutive equations for solid materials by thermomechanics with internal variables. The role and definition of internal variables are briefly discussed and the following definition is given: The independent variables present (possibly hidden) in the basic laws for thermomechanics are called controllable variables. The other independent variables are called internal variables. An internal variable is shown always to be a state variable. This work shows that if the specific dissipation function is a homogeneous function of degree one in the fluxes, a description for a time-independent process is obtained. When damage to materials is evaluated, usually a scalar-valued or tensorial variable called damage is introduced in the set of internal variables. A problem arises when determining the relationship between physically observable weakening of the material and the value for damage. Here a more feasible approach is used. Instead of damage, the void volume fraction is inserted into the set of internal variables. This allows use of an analytical equation for description of the mechanical weakening of the material. An extension to the material model proposed by Gurson and modified by Tvergaard is derived. The derivation is based on results obtained by thermomechanics and damage mechanics. The main difference between the original Gurson-Tvergaard material model and the extended one lies in the definition of the internal variable `equivalent tensile flow stress in the matrix material` denoted by {sigma}{sup M}. Using classical plasticity theory, Tvergaard elegantly derived an evolution equation for {sigma}{sup M}. This is not necessary in the present model, since damage mechanics gives an analytical equation between the stress tensor {sigma} and {sigma}M. Investigation of the Clausius-Duhem inequality shows that in compression

  2. Determination of high-molecular weight polycyclic aromatic hydrocarbons in high performance liquid chromatography fractions of coal tar standard reference material 1597a via solid-phase nanoextraction and laser-excited time-resolved Shpol'skii spectroscopy

    Wilson, Walter B.; Alfarhani, Bassam; Moore, Anthony F. T.; Bisson, Cristina; Wise, Stephen A.; Campiglia, Andres D.


    This article presents an alternative approach for the analysis of high molecular weight – polycyclic aromatic hydrocarbons (HMW-PAHs) with molecular mass 302 Da in complex environmental samples. This is not a trivial task due to the large number of molecular mass 302 Da isomers with very similar chromatographic elution times and similar, possibly even virtually identical, mass fragmentation patterns. The method presented here is based on 4.2 K laser-excited time-resolved Shpol'skii spectroscopy, a high resolution spectroscopic technique with the appropriate selectivity for the unambiguous determination of PAHs with the same molecular mass. The potential of this approach is demonstrated here with the analysis of a coal tar standard reference material (SRM) 1597a. Liquid chromatography fractions were submitted to the spectroscopic analysis of five targeted isomers, namely dibenzo[a,l]pyrene, dibenzo[a,e]pyrene, dibenzo[a,i]pyrene, naphtho[2,3-a]pyrene and dibenzo[a,h]pyrene. Prior to analyte determination, the liquid chromatographic fractions were pre-concentrated with gold nanoparticles. Complete analysis was possible with microliters of chromatographic fractions and organic solvents. The limits of detection varied from 0.05 (dibenzo[a,l]pyrene) to 0.24 μg L−1 (dibenzo[a,e]pyrene). The excellent analytical figures of merit associated to its non-destructive nature, which provides ample opportunity for further analysis with other instrumental methods, makes this approach an attractive alternative for the determination of PAH isomers in complex environmental samples. PMID:26653471

  3. Determination of high-molecular weight polycyclic aromatic hydrocarbons in high performance liquid chromatography fractions of coal tar standard reference material 1597a via solid-phase nanoextraction and laser-excited time-resolved Shpol'skii spectroscopy.

    Wilson, Walter B; Alfarhani, Bassam; Moore, Anthony F T; Bisson, Cristina; Wise, Stephen A; Campiglia, Andres D


    This article presents an alternative approach for the analysis of high molecular weight - polycyclic aromatic hydrocarbons (HMW-PAHs) with molecular mass 302 Da in complex environmental samples. This is not a trivial task due to the large number of molecular mass 302 Da isomers with very similar chromatographic elution times and similar, possibly even virtually identical, mass fragmentation patterns. The method presented here is based on 4.2K laser-excited time-resolved Shpol'skii spectroscopy, a high resolution spectroscopic technique with the appropriate selectivity for the unambiguous determination of PAHs with the same molecular mass. The potential of this approach is demonstrated here with the analysis of a coal tar standard reference material (SRM) 1597a. Liquid chromatography fractions were submitted to the spectroscopic analysis of five targeted isomers, namely dibenzo[a,l]pyrene, dibenzo[a,e]pyrene, dibenzo[a,i]pyrene, naphtho[2,3-a]pyrene and dibenzo[a,h]pyrene. Prior to analyte determination, the liquid chromatographic fractions were pre-concentrated with gold nanoparticles. Complete analysis was possible with microliters of chromatographic fractions and organic solvents. The limits of detection varied from 0.05 (dibenzo[a,l]pyrene) to 0.24 µg L(-1) (dibenzo[a,e]pyrene). The excellent analytical figures of merit associated to its non-destructive nature, which provides ample opportunity for further analysis with other instrumental methods, makes this approach an attractive alternative for the determination of PAH isomers in complex environmental samples.

  4. New Family of Materials with Negative Coefficients of Thermal Expansion: The Effect of MgO, CoO, MnO, NiO, or CuO on the Phase Stability and Thermal Expansion of Solid Solution Phases Derived from BaZn2Si2O7.

    Thieme, Christian; Waurischk, Tina; Heitmann, Stephan; Rüssel, Christian


    Recently, a silicate with the composition SrxBa1-xZn2Si2O7 was reported, which exhibits a negative coefficient of thermal expansion. The compound BaZn2Si2O7 shows a highly positive coefficient of thermal expansion up to a temperature of 280 °C and then transfers to a high temperature phase, which exhibits a coefficient of thermal expansion near zero or negative over a limited temperature range up to around 500 °C. This high temperature modification can be stabilized to room temperature if Ba(2+) is replaced by Sr(2+). In the solid solution SrxBa1-xZn2Si2O7, also Zn(2+) can be replaced in a wide concentration range by other cations with the respective valency. In the present study, Zn was partially or completely replaced by Mg, Co, Mn, Ni, or Cu. If the high temperature phase is stable at room temperature, the thermal expansion is negative, and if the partial substitution exceeds a certain concentration threshold, the low temperature phase with the crystal structure of BaZn2Si2O7 and highly positive thermal expansion is formed. The lowest mean coefficients of thermal expansion were measured for the composition Ba0.5Sr0.5Zn1.4Co0.6Si2O7 with a value of -2.9 × 10(-6) K(-1). In general, a lower Zn-concentration leads to a higher anisotropy and a lower mean coefficient of thermal expansion.

  5. Proposed method for controlling turbid particles in solid-phase bioluminescent toxicity measurement.

    Yeo, Seul-Ki; Park, Jun-Boum; Ahn, Joo-Sung; Han, Young-Soo


    In the recent half century, numerous methods have been developed to assess ecological toxicity. However, the presence of solid-particle turbidity sometimes causes such tests to end with questionable results. Many researchers focused on controlling this arbitrary turbidity effect when using the Microtox® solid-phase toxicity system, but there is not yet a standard method. In this study, we examined four solid-phase sample test methods recommended in the Microtox® manual, or proposed from the literature, and compared the existing methods with our proposed method (centrifuged basic solid-phase test, c-BSPT). Four existing methods use the following strategies to control turbid particles: complete separation of liquid and solid using 0.45-μm filtration before contacting solid samples and bacteria, natural settlement, moderate separation of large particles using coarser pore size filtration, and exclusion of light loss in the toxicity calculation caused by turbidity after full disturbance of samples. Our proposed method uses moderate centrifugation to separate out the heavier soil particles from the lighter bacteria after direct contact between them. Among the solid-phase methods tested, in which the bacteria and solid particles were in direct contact (i.e., the three existing methods and the newly proposed one, c-BSPT), no single method could be recommended as optimal for samples over a range of turbidity. Instead, a simple screening strategy for selecting a sample-dependent solid-phase test method was suggested, depending on the turbidity of the solid suspension. The results of this study highlight the importance of considering solid particles, and the necessity for optimal selection of test method to reduce errors in the measurement of solid-phase toxicity.

  6. Microwave spectroscopic observation of distinct electron solid phases in wide quantum wells.

    Hatke, A T; Liu, Yang; Magill, B A; Moon, B H; Engel, L W; Shayegan, M; Pfeiffer, L N; West, K W; Baldwin, K W


    In high magnetic fields, two-dimensional electron systems can form a number of phases in which interelectron repulsion plays the central role, since the kinetic energy is frozen out by Landau quantization. These phases include the well-known liquids of the fractional quantum Hall effect, as well as solid phases with broken spatial symmetry and crystalline order. Solids can occur at the low Landau-filling termination of the fractional quantum Hall effect series but also within integer quantum Hall effects. Here we present microwave spectroscopy studies of wide quantum wells that clearly reveal two distinct solid phases, hidden within what in d.c. transport would be the zero diagonal conductivity of an integer quantum-Hall-effect state. Explanation of these solids is not possible with the simple picture of a Wigner solid of ordinary (quasi) electrons or holes.

  7. Phase stress measurements in composite materials

    Akiniwa, Yoshiaki; Tanaka, Keisuke [Nagoya Univ. (Japan). School of Engineering


    Using an aluminum alloy composite containing 20 wt.% of SiC powder and an aluminum alloy itself, a phase stress under monoaxial tensile load was tested using x-ray and neutron methods, to compare both of them. For specimens, a 20 vol.% SiC powder reinforced aluminum alloy and an aluminum alloy itself were used. As a result, the following results could be obtained. Young`s modulus and Poisson ratio of the aluminum alloy itself using x-ray method were E=74.5 GPa and {nu}=0.312, respectively, and those using neutron method were E=75.3 GPa and {nu}=0.384, respectively. A relationship between loading stress and lattice strain of the aluminum alloy itself using neutron method was possible to approximate linearly by containing macroscopic plastic deformation region. The lattice strain of each phase in the composite increased proportionally with loading stress in its elastic region, but when remarkably increasing plastic deformation, the lattice strain decreased proportionally in aluminum phase and increased in SiC phase. (G.K.)

  8. Phase interface effects in the total enthalpy-based lattice Boltzmann model for solid-liquid phase change

    Huang, Rongzong; Wu, Huiying


    In this paper, phase interface effects, including the differences in thermophysical properties between solid and liquid phases and the numerical diffusion across phase interface, are investigated for the recently developed total enthalpy-based lattice Boltzmann model for solid-liquid phase change, which has high computational efficiency by avoiding iteration procedure and linear equation system solving. For the differences in thermophysical properties (thermal conductivity and specific heat) between solid and liquid phases, a novel reference specific heat is introduced to improve the total enthalpy-based lattice Boltzmann model, which makes the thermal conductivity and specific heat decoupled. Therefore, the differences in thermal conductivity and specific heat can be handled by the dimensionless relaxation time and equilibrium distribution function, respectively. As for the numerical diffusion across phase interface, it is revealed for the first time and found to be induced by solid-liquid phase change. To reduce such numerical diffusion, multiple-relaxation-time collision scheme is exploited, and a special value (one fourth) for the so-called "magic" parameter, a combination of two relaxation parameters, is found. Numerical tests show that the differences in thermophysical properties can be correctly handled and the numerical diffusion across phase interface can be dramatically reduced. Finally, theoretical analyses are carried out to offer insights into the roles of the reference specific heat and "magic" parameter in the treatments of phase interface effects.

  9. Solid phase extraction and determination of carbamate pesticides in water samples by reverse-phase HPLC

    Moreno-Tovar, J.; Santos-Delgado, M.J. [Departamento de Quimica Analitica, Facultad de ciencias Quimicas, Universidad Complutense de Madrid (Spain)


    Solid phase extraction. SPE. using C{sub 1}8 bonded silica cartridges for trace amounts determination of carbaryl, propoxur, thiram, propham and methiocarb in water samples was studied and the breakthrough volume of the cartridges was established. The high enrichment factor and large injection volume admissible in the isocratic reverse-phase HPLC system allows pesticides determination with UV detection at 22o nm even at a concentration lower than 0.05 mug/L. Purified tap natural and underground water samples were spiked with carbamate pesticides in the concentration range 0.16-16.0 mug/L. Large volumes of samples (up to 2L) were passed through available C{sub 1}8, cartridges and eluted with acetonitrile. The preconcentrated samples were analyzed by HPLC using a Spherisorb ODS column with a 42.58 acetonitrile-water mobile phase. From replicate samples, recovery for the pesticides ranged from 79.0 to 103.7% except for thiran which is not retained. Tehe relative standard deviation (n=4 at 0.16 to 1.61 mug/L concetration level) range from 1.1 to 6.8%. (Author) 14 refs.

  10. Solid Phase Extraction Disk Procedure to Determine 239Pu in Soils

    ZHANG Ji-qiao;ZHAO Ya-ping;DING You-qian;ZHANG Sheng-dong;YANG Jin-ling


    Full Text Available 239Pu in many soil samples should be analyzed to survey radioactive pollution level in nuclear facilities and its affinity environment efficiently. In order to input the opt conditions for column experiment, the experiments of the static adsorption coefficient of 239Pu to solid phase extraction disk with different contact time, concentration of HNO3 and different temperature were carried out. The chemical procedure for the rapid separation and determination of 239Pu in soils had been formulated, which using solid phase extraction disk (EmporeTM Anion Exchange-SR as extraction material and liquid scintillation spectrometry counting as measurement. In the procedure, soil sample usage was 10 g, and were leached by 8 mol/L HNO3, the chemical recovery of the procedure was about 78.9%, and the minimum detectable concentration was 3.7 Bq/kg. It took less than 3 hours once and the presence of 137Cs, 90Sr-90Y and natural uranium, 241Am, 99Tc did not interfere with the procedure, owning high DF of them. The procedure can be used extensively in determination of 239Pu in soils.

  11. Determination of amphetamines in human urine by headspace solid-phase microextraction and gas chromatography.

    Raikos, Nikolaos; Christopoulou, Klio; Theodoridis, Georgios; Tsoukali, Heleni; Psaroulis, Dimitrios


    Solid-phase microextraction (SPME) is under investigation for its usefulness in the determination of a widening variety of volatile and semivolatile analytes in biological fluids and materials. Semivolatiles are increasingly under study as analytical targets, and difficulties with small partition coefficients and long equilibration times have been identified. Amphetamines were selected as semivolatiles exhibiting these limitations and methods to optimize their determination were investigated. A 100- micro m polydimethylsiloxane (PDMS)-coated SPME fiber was used for the extraction of the amphetamines from human urine. Amphetamine determination was made using gas chromatography (GC) with flame-ionization detection (FID). Temperature, time and salt saturation were optimized to obtain consistent extraction. A simple procedure for the analysis of amphetamine (AMP) and methamphetamine (MA) in urine was developed and another for 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxy-N-methamphetamine (MDMA) and 3,4-methylenedioxy-N-ethylamphetamine (MDEA) using headspace solid-phase microextraction (HS-SPME) and GC-FID. Higher recoveries were obtained for amphetamine (19.5-47%) and methamphetamine (20-38.1%) than MDA (5.1-6.6%), MDMA (7-9.6%) and MDEA (5.4-9.6%).

  12. Carbon nanocones/disks as new coating for solid-phase microextraction.

    Jiménez-Soto, Juan Manuel; Cárdenas, Soledad; Valcárcel, Miguel


    In this article, the potential of carbon nanocones/disks as coating for solid-phase microextraction has been evaluated for the first time. The nanostructures were immobilized on a stainless steel needle by means of an organic binder. The fiber coating obtained was ca. 50 microm of thickness and 35 mm in length. The evaluation of the sorbent capacity was carried out through the determination of toluene, ethylbenzene, xylene isomers and styrene in water samples following the headspace sampling modality (15 min, 30 degrees C). The fiber was then transferred to a 10 mL vial which was sealed and heated at 110 degrees C for 15 min in the headspace module of the instrument to achieve the thermal desorption of the analytes. Then 2.5 mL of the headspace generated were injected in the gas chromatograph-mass spectrometer for analytes separation and quantitation. The detection and quantitation limits obtained for 10 mL of sample were 0.15 and 0.5 ng mL(-1) (0.6 and 2 ng mL(-1) for toluene). The optimized procedure was applied to the determination of the selected volatile compounds in waters collected from different locations. The recovery values obtained (average recovery ca. 92%) demonstrated the usefulness of the carbon nanocones/disks as sorbent material in solid-phase microextraction.

  13. Novel polymeric resin for solid phase extraction and determination of lead in waters

    Karaaslan, Nagihan M.; Cengiz, Emine; Yaman, Mehmet [Science Faculty, Department of Chemistry, Firat University, Elazig (Turkey); Senkal, B. Filiz [Science and Arts Faculty, Department of Chemistry, Istanbul Technical University, Istanbul (Turkey)


    Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry and the high costs of other sensitive methods in compared to flame atomic absorption spectrometry (FAAS). Among preconcentration techniques, solid-phase extraction is the most popular because of a number of advantages. In this work, thiol-containing sulfonamide resin was synthesized, characterized, and applied as a new sorption material for solid phase extraction and determination of lead in natural water samples. The optimization of experimental conditions was performed using the parameters including pH, contact time, and volumes of initial and elution solutions. After preconcentration procedure, FAAS was used for determinations. The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent as well as high sorption capacity. Consequently, 280-fold improvement in the sensitivity of analytical scheme was achieved by combining the slotted tube atom trap-atomic absorption spectrometry (STAT-FAAS) and the developed preconcentration method. The limit of detection was found to be 0.15 ng mL{sup -1}. The Pb{sup 2+} concentrations in the studied water samples were found to be in the range of 0.9-6.7 ng mL{sup -1}. (Copyright copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  14. Titanium dioxide solid phase for inorganic species adsorption and determination: the case of arsenic.

    Vera, R; Fontàs, C; Anticó, E


    We have evaluated a new titanium dioxide (Adsorbsia As600) for the adsorption of both inorganic As (V) and As (III) species. In order to characterize the sorbent, batch experiments were undertaken to determine the capacities of As (III) and As (V) at pH 7.3, which were found to be 0.21 and 0.14 mmol g(-1), respectively. Elution of adsorbed species was only possible using basic solutions, and arsenic desorbed under batch conditions was 50 % when 60 mg of loaded titanium dioxide was treated with 0.5 M NaOH solution. Moreover, its use as a sorbent for solid-phase extraction and preconcentration of arsenic species from well waters has been investigated, without any previous pretreatment of the sample. Solid-phase extraction was implemented by packing several minicolumns with Adsorbsia As600. The method has been validated showing good accuracy and precision. Acceptable recoveries were obtained when spiked waters at 100-200 μg L(-1) were measured. The presence of major anions commonly found in waters did not affect arsenic adsoption, and only silicate at 100 mg L(-1) level severely competed with arsenic species to bind to the material. Finally, the measured concentrations in water samples containing arsenic from the Pyrinees (Catalonia, Spain) showed good agreement with the ICP-MS results.

  15. Dead lithium phase investigation of Sn-Zn alloy as anode materials for lithium ion battery

    HUANG ZhaoWen; HU SheJun; HOU XianHua; RU Qiang; YU HongWen; ZHAO LingZhi; LI WeiShan


    In this work, based on First-principle plane wave pseudo-potential method, we have carried out an in-depth study on the possible dead lithium phase of Sn-Zn alloy as anode materials for lithium ion batteries. Through investigation, we found that the phases LixSn4Zn4(x = 2, 4, 6, 8) contributed to reversible capacity, while the phases LixSn4Zns-(x-4)(x = 4.74, 7.72) led to capacity loss due to high formation energy, namely, they were the dead lithium phases during the charge/discharge process. And we come up with a new idea that stable lithium alloy phase with high lithiation formation energy (dead lithium phase) can also result in high loss of active lithium ion, besides the traditional expression that the formation of solid electrolyte interface film leads to high capacity loss.

  16. Melting of nanoparticles-enhanced phase change material (NEPCM) in vertical semicircle enclosure: numerical study

    Jourabian, Mahmoud [University of Trieste, Piazzale (Italy); Farhadi, Mousa [Babol Noshirvani University of Technology, Shariati Avenue (Iran, Islamic Republic of)


    Convection melting of ice as a Phase change material (PCM) dispersed with Cu nanoparticles, which is encapsulated in a semicircle enclosure is studied numerically. The enthalpy-based Lattice Boltzmann method (LBM) combined with a Double distribution function (DDF) model is used to solve the convection-diffusion equation. The increase in solid concentration of nanoparticles results in the enhancement of thermal conductivity of PCM and the decrease in the latent heat of fusion. By enhancing solid concentration of nanoparticles, the viscosity of nanofluid increases and convective heat transfer dwindles. For all Rayleigh numbers investigated in this study, the insertion of nanoparticles in PCM has no effect on the average Nusselt number.

  17. Nonminimum Phase Behavior of Laser Material Processing

    Römer, G.R.B.E.; Weerkamp, N.P.; Meijer, J.; Postma, S.


    Optical sensors are increasingly applied in laser material processing to monitor and control the lasermaterial interaction zone. Dynamic models, relating the sensor signals (e.g. as temperature or molten area) to the process inputs (e.g. laser power or beam velocity), provide the basis for the desig

  18. Characterization of interactions between soil solid phase and soil solution in the initial ecosystem development phase

    Zimmermann, Claudia; Schaaf, Wolfgang


    In the initial phase of soil formation interactions between solid and liquid phases and processes like mineral weathering, formation of reactive surfaces and accumulation of organic matter play a decisive role in developing soil properties. As part of the Transregional Collaborative Research Centre (SFB/TRR 38) 'Patterns and processes of initial ecosystem development' in an artificial catchment, these interactions are studied at the catchment 'Chicken Creek' (Gerwin et al. 2009). To link the interactions between soil solid phase and soil solution at the micro-scale with observed processes at the catchment scale, microcosm experiments under controlled laboratory conditions were carried out. Main objectives were to determine the transformation processes of C and N from litter decomposition within the gaseous, liquid and solid phase, the interaction with mineral surfaces and its role for the establishment of biogeochemical cycles. The microcosm experiments were established in a climate chamber at constant 10 ° C. In total 48 soil columns (diameter: 14.4 cm; height: 30 cm) were filled with two different quaternary substrates (sand and loamy sand) representing the textural variation within the catchment at a bulk density of 1.4-1.5 g*cm-3. The columns were automatically irrigated four times a day with 6.6 ml each (corresponding to 600 mm*yr-1). The gaseous phase in the headspace of the microcosms was analysed continuously for CO2 and N2O contents. C and N transformation processes were studied using 13C and 15N labelled litter of two different plant species occurring at the catchment (Lotus corniculatus, Calamagrostis epigejos) that was incorporated into the microcosm surface. All treatments including a control ran with four replicates over a period of 40 weeks. Two additional microcosms act as pure litter controls where substrate was replaced by glass pearls. Litter and substrate were analysed before and after the experiment. Percolate was continuously collected and

  19. The growth and tensile deformation behavior of the silver solid solution phase with zinc

    Wu, Jiaqi, E-mail: [Department of Electrical Engineering and Computer Science, University of California, Irvine, CA 92697-2660 (United States); Materials and Manufacturing Technology, University of California, Irvine, CA 92697-2660 (United States); Lee, Chin C. [Department of Electrical Engineering and Computer Science, University of California, Irvine, CA 92697-2660 (United States); Materials and Manufacturing Technology, University of California, Irvine, CA 92697-2660 (United States)


    The growth of homogeneous silver solid solution phase with zinc are conducted at two different compositions. X-ray diffraction (XRD) and Scanning electron microscope/Energy dispersive X-ray spectroscopy (SEM/EDX) are carried out for phase identification and chemical composition verification. The mechanical properties of silver solid solution phase with zinc are evaluated by tensile test. The engineering and true stress vs. strain curves are presented and analyzed, with those of pure silver in comparison. According to the experimental results, silver solid solution phase with zinc at both compositions show tempered yield strength, high tensile strength and large uniform strain compared to those of pure silver. Fractography further confirmed the superior ductility of silver solid solution phase with zinc at both compositions. Our preliminary but encouraging results may pave the way for the silver based alloys to be applied in industries such as electronic packaging and structure engineering.

  20. Mixed micelle cloud point-magnetic dispersive μ-solid phase extraction of doxazosin and alfuzosin.

    Gao, Nannan; Wu, Hao; Chang, Yafen; Guo, Xiaozhen; Zhang, Lizhen; Du, Liming; Fu, Yunlong


    Mixed micelle cloud point extraction (MM-CPE) combined with magnetic dispersive μ-solid phase extraction (MD-μ-SPE) has been developed as a new approach for the extraction of doxazosin (DOX) and alfuzosin (ALF) prior to fluorescence analysis. The mixed micelle anionic surfactant sodium dodecyl sulfate and non-ionic polyoxyethylene(7.5)nonylphenylether was used as the extraction solvent in MM-CPE, and diatomite bonding Fe₃O₄ magnetic nanoparticles were used as the adsorbent in MD-μ-SPE. The method was based on MM-CPE of DOX and ALF in the surfactant-rich phase. Magnetic materials were used to retrieve the surfactant-rich phase, which easily separated from the aqueous phase under magnetic field. At optimum conditions, a linear relationship between DOX and ALF was obtained in the range of 5-300 ng mL(-1), and the limits of detection were 0.21 and 0.16 ng mL(-1), respectively. The proposed method was successfully applied for the determination of the drugs in pharmaceutical preparations, urine samples, and plasma samples.

  1. Vapour phase approach for iron oxide nanoparticle synthesis from solid precursors

    Singh, Mandeep; Ulbrich, Pavel; Prokopec, Vadym [Institute of Chemical Technology Prague, Technicka 5, 166 28 Prague 6 (Czech Republic); Svoboda, Pavel [Faculty of Mathematics and Physics, Charles University, Ke Karlovu 5, 120 00 Prague 2 (Czech Republic); Šantavá, Eva [Institute of Physics ASCR, Na Slovance 2, 182 21 Prague 8 (Czech Republic); Štěpánek, František, E-mail: [Institute of Chemical Technology Prague, Technicka 5, 166 28 Prague 6 (Czech Republic)


    A new non-solution mediated approach to the synthesis of iron oxide nanoparticles directly from solid FeCl{sub 2} salt precursors has been developed. The method is rapid, simple and scalable. The structural properties and the phase of the resulting iron oxide particles has been determined by a range of methods including XRD, FT-IR and Mössbauer spectroscopy, and the phase is shown to be maghemite (γ-Fe{sub 2}O{sub 3}). The magnetic properties of the iron oxide particles have been measured using SQUID, confirming superparamagnetic behaviour of the powder and a saturation magnetization of 53.0 emu g{sup −1} at 300 K. Aqueous dispersions at increasing concentrations were prepared and their heating rate under a 400 kHz alternating magnetic field measured. The specific absorption rate (SAR) of the iron oxide was found to be 84.8 W g{sup −1}, which makes the material suitable for the formulation of ferrofluids or ferrogels with RF heating properties. - Graphical Abstract: Superparamagnetic iron oxide nanoparticles obtained by a novel vapour phase approach. Highlights: ► Novel vapour phase (non-solvent) approach for iron oxide nanoparticle synthesis. ► Attractive alternative approach to the present co-precipitation method. ► Better magnetic properties with high coercivity of nanoparticles. ► A high specific absorption rate (SAR) for hyperthermia applications.

  2. Mixed micelle cloud point-magnetic dispersive μ-solid phase extraction of doxazosin and alfuzosin

    Gao, Nannan; Wu, Hao; Chang, Yafen; Guo, Xiaozhen; Zhang, Lizhen; Du, Liming; Fu, Yunlong


    Mixed micelle cloud point extraction (MM-CPE) combined with magnetic dispersive μ-solid phase extraction (MD-μ-SPE) has been developed as a new approach for the extraction of doxazosin (DOX) and alfuzosin (ALF) prior to fluorescence analysis. The mixed micelle anionic surfactant sodium dodecyl sulfate and non-ionic polyoxyethylene(7.5)nonylphenylether was used as the extraction solvent in MM-CPE, and diatomite bonding Fe3O4 magnetic nanoparticles were used as the adsorbent in MD-μ-SPE. The method was based on MM-CPE of DOX and ALF in the surfactant-rich phase. Magnetic materials were used to retrieve the surfactant-rich phase, which easily separated from the aqueous phase under magnetic field. At optimum conditions, a linear relationship between DOX and ALF was obtained in the range of 5-300 ng mL-1, and the limits of detection were 0.21 and 0.16 ng mL-1, respectively. The proposed method was successfully applied for the determination of the drugs in pharmaceutical preparations, urine samples, and plasma samples.

  3. Mechanochemical spinodal decomposition: a phenomenological theory of phase transformations in multi-component, crystalline solids

    Rudraraju, Shiva; van der Ven, Anton; Garikipati, Krishna


    We present a phenomenological treatment of diffusion-driven martensitic phase transformations in multi-component crystalline solids that arise from non-convex free energies in mechanical and chemical variables. The treatment describes diffusional phase transformations that are accompanied by symmetry-breaking structural changes of the crystal unit cell and reveals the importance of a mechanochemical spinodal, defined as the region in strain-composition space, where the free-energy density function is non-convex. The approach is relevant to phase transformations wherein the structural order parameters can be expressed as linear combinations of strains relative to a high-symmetry reference crystal. The governing equations describing mechanochemical spinodal decomposition are variationally derived from a free-energy density function that accounts for interfacial energy via gradients of the rapidly varying strain and composition fields. A robust computational framework for treating the coupled, higher-order diffusion and nonlinear strain gradient elasticity problems is presented. Because the local strains in an inhomogeneous, transforming microstructure can be finite, the elasticity problem must account for geometric nonlinearity. An evaluation of available experimental phase diagrams and first-principles free energies suggests that mechanochemical spinodal decomposition should occur in metal hydrides such as ZrH2-2c. The rich physics that ensues is explored in several numerical examples in two and three dimensions, and the relevance of the mechanism is discussed in the context of important electrode materials for Li-ion batteries and high-temperature ceramics.


    D. V. Kuis


    Full Text Available The mechanism of structure formation in super-solid carbon phase in nanocomposite on the basis of iron and nano-disperse carbon, which can be used at development of technology and composition of creation of new materials using inexpensive nano-carbon materials is offered.

  5. 76 FR 46290 - EPA Seeking Input Materials Measurement; Municipal Solid Waste (MSW), Recycling, and Source...


    ... and steel scrap, other metals, paper fiber) sustainability; C&D materials; and zero waste. Topic 3... AGENCY EPA Seeking Input Materials Measurement; Municipal Solid Waste (MSW), Recycling, and Source... Report called ``Municipal Solid Waste in the United States'' as part of a broader discussion about...

  6. Unusual seeding mechanism for enhanced performance in solid-phase magnetic extraction of Rare Earth Elements

    Polido Legaria, Elizabeth; Rocha, Joao; Tai, Cheuk-Wai; Kessler, Vadim G.; Seisenbaeva, Gulaim A.


    Due to the increasing demand of Rare Earth Elements (REE or RE), new and more efficient techniques for their extraction are necessary, suitable for both mining and recycling processes. Current techniques such as solvent extraction or solid adsorbents entail drawbacks such as using big volumes of harmful solvents or limited capacity. Hybrid nanoadsorbents based on SiO2 and highly stable γ-Fe2O3-SiO2 nanoparticles, proved recently to be very attractive for adsorption of REE, yet not being the absolute key to solve the problem. In the present work, we introduce a highly appealing new approach in which the nanoparticles, rather than behaving as adsorbent materials, perform as inducers of crystallization for the REE in the form of hydroxides, allowing their facile and practically total removal from solution. This induced crystallization is achieved by tuning the pH, offering an uptake efficiency more than 20 times higher than previously reported (up to 900 mg RE3+/g vs. 40 mg RE3+/g). The obtained phases were characterized by SEM-EDS, TEM, STEM and EFTEM and 13C and 29Si solid state NMR. Magnetic studies showed that the materials possessed enough magnetic properties to be easily removed by a magnet, opening ways for an efficient and industrially applicable separation technique.

  7. Preparation and Mechanical Properties of Solid-phase Grafting Nanocomposites of PVC/Graft Copolymers/MMT

    ZHOU Dunbai; CAI Changgen; JIA Demin


    In order to improve the mechanical properties of PVC, by solid-phase grafting reaction, grafting on and nano-modifying the PVC process synchronously, acrylic monomers not only graft on PVC, but also are intercalated into the layers of MMT in the heating process. Blending PVC and the MMT-PVC grafting copolymers, we can get nanocomposites of PVC/ grafters/ MMT, and the mechanical performance of the material is improved.

  8. Application of phase-change materials in memory taxonomy.

    Wang, Lei; Tu, Liang; Wen, Jing


    Phase-change materials are suitable for data storage because they exhibit reversible transitions between crystalline and amorphous states that have distinguishable electrical and optical properties. Consequently, these materials find applications in diverse memory devices ranging from conventional optical discs to emerging nanophotonic devices. Current research efforts are mostly devoted to phase-change random access memory, whereas the applications of phase-change materials in other types of memory devices are rarely reported. Here we review the physical principles of phase-change materials and devices aiming to help researchers understand the concept of phase-change memory. We classify phase-change memory devices into phase-change optical disc, phase-change scanning probe memory, phase-change random access memory, and phase-change nanophotonic device, according to their locations in memory hierarchy. For each device type we discuss the physical principles in conjunction with merits and weakness for data storage applications. We also outline state-of-the-art technologies and future prospects.

  9. Solid phase precipitates in (Zr,Th)-OH-(oxalate, malonate) ternary aqueous system

    Kobayashi, T.; Sasaki, T.; Takagi, I.; Moriyama, H. [Kyoto Univ. (Japan). Dept. of Nuclear Engineering


    The solubility-limiting solid phases in the ternary aqueous systems of Zr(IV)/OH/oxalate, Zr(IV)/OH/malonate, Th(IV)/OH/oxalate and Th(IV)/OH/malonate were characterized by elemental analysis, X-ray diffraction, thermogravimetric analysis and differential thermal analysis. The ternary solid phase of M(IV)/OH/carboxylate was observed to form, even under acidic conditions, depending on the pH and the concentration of carboxylate ligand. In the presence of a large excess of carboxylic acid, however; the binary M(IV)-carboxylate solid phase formed. (orig.)

  10. Design and Synthesis of a Dual Linker for Solid Phase Synthesis of Oleanolic Acid Derivatives

    Shaorong Wang


    Full Text Available A hydrophilic amino-terminated poly(ethylene glycol-type dual linker for solid phase synthesis of oleanolic acid derivatives using trityl chloride resin was designed and synthesized for the first time. Model reactions in both liquid and solid phase were performed to show the feasibility of its selective cleavage at two different sites. The biological assay results indicated that the long and flexible alkyl ether functionality in the linker is less likely to be critical for the binding event. Following the successful solid-phase synthesis of model compounds, the potential of this dual linker in reaction monitoring and target identification is deemed worthy of further study.

  11. Application of results of geological exploration of deposits of solid mineral raw materials in mining

    Ilić Miloje M.


    Full Text Available Important application in mining have the results of geological exploration of the deposits of solid mineral raw materials, before all geological data obtained (including their interpretations regarding basic properties of the deposts and their changeability, and regarding quantity and quality (i.e. resources and reserves of the belonging mineral raw material which have an essential significance for mineral projects. The geological data, together with the other relevant data (in the first place technical and economic ones are applied as basic parameters in documentation of mineral projects. Since the successfulness of the projects is dependent upon the confidence of the data, a special attention is dedicated to the acts that contribute to attaining of an adequate level of confidence of the data, as follows: a a gradual realization of the projects through two phases (geological and mining ones having seven development stages (reconnaissance, prospecting, preliminary exploration and detailed exploration stages of the geological phase and mine design, mine construction and mine production stages of the mining phase; b finding out optimal solutions in drawing up a plan of exploratory workings and its carrying out in accordance with basic properties of a deposit and their changeability; c a realistic estimation of mineral resources/reserves as a predominantly geological task (not 'calculation' of the resources/reserves as a mathematical task; d an objective evaluation of the successfulness of a project at the end of every geological stage ‒ presented in corresponding geological analyses and technical-economic studies.

  12. Solid-fluid and solid-solid equilibrium in hard sphere united atom models of n-alkanes: rotator phase stability.

    Cao, M; Monson, P A


    We present a study of the phase behavior for models of n-alkanes with chain lengths up to C(21) based on hard sphere united atom models of methyl and methylene groups, with fixed bond lengths and C-C-C bond angles. We extend earlier work on such models of shorter alkanes by allowing for gauche conformations in the chains. We focus particularly on the orientational order about the chain axes in the solid phase near the melting point, and our model shows how the loss of this orientational order leads to the formation of rotator phases. We have made extensive calculations of the thermodynamic properties of the models as well as order parameters for tracking the degree of orientational order around the chain axis. Depending on the chain length and whether the carbon number is even or odd, the model exhibits both a rotator phase and a more orientationally ordered solid phase in addition to the fluid phase. Our results indicate that the transition between the two solid phases is first-order with a small density change. The results are qualitatively similar to those seen experimentally and show that rotator phases can appear in models of alkanes without explicit treatment of attractive forces or explicit treatment of the hydrogen atoms in the chains.

  13. Single phase 3D phononic band gap material.

    Warmuth, Franziska; Wormser, Maximilian; Körner, Carolin


    Phononic band gap materials are capable of prohibiting the propagation of mechanical waves in certain frequency ranges. Band gaps are produced by combining different phases with different properties within one material. In this paper, we present a novel cellular material consisting of only one phase with a phononic band gap. Different phases are modelled by lattice structure design based on eigenmode analysis. Test samples are built from a titanium alloy using selective electron beam melting. For the first time, the predicted phononic band gaps via FEM simulation are experimentally verified. In addition, it is shown how the position and extension of the band gaps can be tuned by utilizing knowledge-based design.

  14. Thin Film Composite Materials, Phase 2


    were Kevlar coated with silicone, EPDM , or neoprene rubber, with the following results: 1. Tensile testing of coated Kevlar fabric is very difficult...materials. 2. A method was developed for measuring water vapor permeability. Neoprene and EPDM are promising as coatings with good water resistance; however...control the folding of the fabric, since the diameters of the spiral channel will be fixed. Because of the stability imparted by the channel, it is

  15. Site-Targeted Interfacial Solid-Phase Chemistry: Surface Functionalization of Organic Monolayers via Chemical Transformations Locally Induced at the Boundary between Two Solids.

    Maoz, Rivka; Burshtain, Doron; Cohen, Hagai; Nelson, Peter; Berson, Jonathan; Yoffe, Alexander; Sagiv, Jacob


    Effective control of chemistry at interfaces is of fundamental importance for the advancement of methods of surface functionalization and patterning that are at the basis of many scientific and technological applications. A conceptually new type of interfacial chemical transformations has been discovered, confined to the contact surface between two solid materials, which may be induced by exposure to X-rays, electrons or UV light, or by the application of electrical bias. One of the reacting solids is a removable thin film coating that acts as a reagent/catalyst in the chemical modification of the solid surface on which it is applied. Given the diversity of thin film coatings that may be used as solid reagents/catalysts and the lateral confinement options provided by the use of irradiation masks, conductive AFM probes or stamps, and electron beams in such solid-phase reactions, this approach is suitable for precise targeting of different desired chemical modifications to predefined surface sites spanning the macro- to nanoscale.

  16. Liquid phase sintering, II: Computer study of skeletal settling and solid phase extrication in a microgravity environment

    Nikolić Z.S.


    Full Text Available A two-dimensional numerical method based on the Brownian motion model and on the Densification model for simulation of liquid phase sintering in microgravity environment will be developed. Both models will be based on domain topology (two-dimensional particle representation and control volume methodology and on three submodels for domain translation, solid skeleton formation and domain extrication. This method will be tested in order to conduct a study of diffusion phenomena and microgravitational effects on microstructural evolution influenced by skeletal settling combined with solid-phase extrication during liquid phase sintering of porous W-Ni system.

  17. Potential electrode materials for symmetrical Solid Oxide Fuel Cells

    Ruiz Morales, J. C.


    Full Text Available Chromites, titanates and Pt-YSZ-CeO2 cermets have been investigated as potential electrode materials for an alternative concept of Solid Oxide Fuel Cell (SOFC, the symmetrical SOFCs (SFC. In this configuration, the same electrode material is used simultaneously as anode and cathode. Interconnector materials, such as chromites, could be considered as potential SFC electrodes, at least under pure hydrogen-fed at relatively high temperatures, as they do not exhibit significant catalytic activity towards hydrocarbon oxidation. This may be overcome by partially substituting Cr in the perovskite B-sites by other transition metal cations such as Mn. La0.75Sr0.25Cr0.5Mn0.5O3-δ (LSCM is a good candidate for such SFCs, rendering fuel cell performances in excess of 500 and 300mW/cm2 using pure H2 and CH4 as fuel, at 950 oC. Similarly, typical n-type electronic conductors traditionally regarded as anode materials, such as strontium titanates, may also operate under oxidising conditions as cathodes by substituting some Ti content for Fe to introduce p-type conductivity. Preliminary electrochemical experiments on La4Sr8Ti12-xFexO38-δ-based SFCs show that they perform reasonably well under humidified H2, at high temperatures. A third group of materials is the support material of any typical cermet anode, i.e. YSZ, CeO2 plus a current collector. It has been found that this combination could be optimised to operate as SFC electrodes, rendering performances of 400mW/cm2 under humidified pure H2 at 950oC.

    Cromitas, titanatos y cermets de Pt-YSZ-CeO2 han sido investigados como potenciales materiales de electrodo para un concepto alternativo de Pilas de Combustible de Óxidos Sólidos (SOFC, las pilas SOFC simétricas (SFC. En

  18. Thermodynamic stability of perovskite and lanthanum nickelate-type cathode materials for solid oxide fuel cells

    Cetin, Deniz

    The need for cleaner and more efficient alternative energy sources is becoming urgent as concerns mount about climate change wrought by greenhouse gas emissions. Solid oxide fuel cells (SOFCs) are one of the most efficient options if the goal is to reduce emissions while still operating on fossil energy resources. One of the foremost problems in SOFCs that causes efficiency loss is the polarization resistance associated with the oxygen reduction reaction(ORR) at the cathodes. Hence, improving the cathode design will greatly enhance the overall performance of SOFCs. Lanthanum nickelate, La2NiO4+delta (LNO), is a mixed ionic and electronic conductor that has competitive surface oxygen exchange and transport properties and excellent electrical conductivity compared to perovskite-type oxides. This makes it an excellent candidate for solid oxide fuel cell (SOFC) applications. It has been previously shown that composites of LNO with Sm0.2Ce0.8O2-delta (SDC20) as cathode materials lead to higher performance than standalone LNO. However, in contact with lanthanide-doped ceria, LNO decomposes resulting in free NiO and ceria with higher lanthanide dopant concentration. In this study, the aforementioned instability of LNO has been addressed by compositional tailoring of LNO: lanthanide doped ceria (LnxCe 1-xO2,LnDC)composite. By increasing the lanthanide dopant concentration in the ceria phase close to its solubility limit, the LNO phase has been stabilized in the LNO:LnDC composites. Electrical conductivity of the composites as a function of LNO volume fraction and temperature has been measured, and analyzed using a resistive network model which allows the identification of a percolation threshold for the LNO phase. The thermomechanical compatibility of these composites has been investigated with SOFC systems through measurement of the coefficients of thermal expansion. LNO:LDC40 composites containing LNO lower than 50 vol%and higher than 40 vol% were identified as being

  19. 75 FR 64585 - Bulk Solid Hazardous Materials: Harmonization With the International Maritime Solid Bulk Cargoes...


    ... nonsubstantive changes, however, to correct grammar, internal paragraph references, and a temperature conversion... means the English version of the ``International Maritime Solid Bulk Cargoes Code'' published by...

  20. Use of a PKZh-902 instrument for monitoring solid phases in an organic coolant

    Gavrillin, A.I.; Gagarin, S.I.; Sokolov, V.E.; Zabelin, A.I.


    Preliminary tests have been performed with a PKZh-902 in checking feed and circulating coolant, and also in evaluating the performance of the cleaning devices. The test program involved determining the stability of the esnsor materials in ditolymethane, examining the effects of radioactive products and those of the optical characteristics of impurities in the first-loop coolant on the readings and errors of measurement, and checking the scope for using the instrument for continuous monitoring of particle concentrations. Results confirm that the PKZh-902 enables one to monitor the composition and concentration of the solid dispersed phase reliably and with adequate accuracy in the feed coolant. The use for monitoring the loop coolant requires additonal research.

  1. Recent Developments in Solid-Phase Extraction for Near and Attenuated Total Reflection Infrared Spectroscopic Analysis

    Christian W. Huck


    Full Text Available A review with more than 100 references on the principles and recent developments in the solid-phase extraction (SPE prior and for in situ near and attenuated total reflection (ATR infrared spectroscopic analysis is presented. New materials, chromatographic modalities, experimental setups and configurations are described. Their advantages for fast sample preparation for distinct classes of compounds containing different functional groups in order to enhance selectivity and sensitivity are discussed and compared. This is the first review highlighting both the fundamentals of SPE, near and ATR spectroscopy with a view to real sample applicability and routine analysis. Most of real sample analyses examples are found in environmental research, followed by food- and bioanalysis. In this contribution a comprehensive overview of the most potent SPE-NIR and SPE-ATR approaches is summarized and provided.

  2. Solid Phase Luminescence of Several Rare Earth Ions on Ion-Exchange Films

    Tanner, Stephen P.; Street, Kenneth W., Jr.


    The development and characterization of a novel ion-exchange film for solid-phase fluorometry and phosphorimetry is reported. This new cation-exchange material is suitable for spectroscopic applications in the ultraviolet and visible regions. It is advantageous because it, as a single entity, is easily recovered from solution and mounted in the spectrofluorometers. After preconcentration on the film, the luminescence intensity of lanthanide ions is several orders of magnitude greater than that of the corresponding solution, depending on the volume of solution and the amount of film. This procedure allows emission spectral measurements and determination of lanthanide ions at solution concentrations of < 5 (micro)g/L. The film may be stored for subsequent reuse or as a permanent record of the analysis. The major drawback to the use of the film is slow uptake of analyte due to diffusion limitations.

  3. Solid phase extraction of iron and lead in environmental matrices on amberlite xad-1180/pv

    Mustafa Soylak


    Full Text Available A solid phase extraction procedure using Amberlite XAD-1180/Pyrocatechol violet (PV chelating resin for the determination of iron and lead ions in various environmental samples was established. The procedure is based on the sorption of lead(II and iron(III ions onto the resin at pH 9, followed by elution with 1 mol/L HNO3 and determination by flame atomic absorption spectrometry. The influence of alkaline, earth alkaline and some transition metals, as interferents, are discussed. The recoveries for the spiked analytes were greater than 95%. The detection limits for lead and iron by FAAS were 0.37 µg/L and 0.20 µg/L, respectively. Validation of the method described here was performed by using three certified reference materials (SRM 1515 Apple Leaves, SRM 2711 Montana Soil and NRCC-SLRS-4 Riverine Water. The procedure was successfully applied to natural waters and human hair.

  4. Silica supported Fe(3)O(4) magnetic nanoparticles for magnetic solid-phase extraction and magnetic in-tube solid-phase microextraction: application to organophosphorous compounds.

    Moliner-Martinez, Y; Vitta, Yosmery; Prima-Garcia, Helena; González-Fuenzalida, R A; Ribera, Antonio; Campíns-Falcó, P; Coronado, Eugenio


    This work demonstrates the application of silica supported Fe3O4 nanoparticles as sorbent phase for magnetic solid-phase extraction (MSPE) and magnetic on-line in-tube solid-phase microextraction (Magnetic-IT-SPME) combined with capillary liquid chromatography-diode array detection (CapLC-DAD) to determine organophosphorous compounds (OPs) at trace level. In MSPE, magnetism is used as separation tool while in Magnetic-IT-SPME, the application of an external magnetic field gave rise to a significant improvement of the adsorption of OPs on the sorbent phase. Extraction efficiency, analysis time, reproducibility and sensitivity have been compared. This work showed that Magnetic-IT-SPME can be extended to OPs with successful results in terms of simplicity, speed, extraction efficiency and limit of detection. Finally, wastewater samples were analysed to determine OPs at nanograms per litre.

  5. Utilizing ion-pairing hydrophilic interaction chromatography solid phase extraction for efficient glycopeptide enrichment in glycoproteomics

    Mysling, Simon; Palmisano, Giuseppe; Højrup, Peter;


    Glycopeptide enrichment is a prerequisite to enable structural characterization of protein glycosylation in glycoproteomics. Here we present an improved method for glycopeptide enrichment based on zwitter-ionic hydrophilic interaction chromatography solid phase extraction (ZIC-HILIC SPE...

  6. Study on New Sensitive Method of Determination of Phosphorus by Solid Phase Spectrophotometry


    The use of solid phase spectrophotometry for the determination of trace phosphorus in the system of phosphomolybdate-fructose is described. The adsorption of the system on anion-exchange resin is reported.

  7. Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

    Mashile, Geaneth Pertunia; Nomngongo, Philiswa N


    Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

  8. Design and Solid-Phase Synthesis of Multiple Muramyl Dipeptide (MMD)


    As a non-specific modulator of macrophage, multiplied muramyl dipeptide (MMD) is solid-phase synthesized by application of standard Fmoc chemistry strategy. Tam's multiple antigen system (MAS) is used as our four branched-linker on Lysine.

  9. Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

    Zielinska, K.


    Solid phase microextraction (SPME) is applied in the speciation analysis of the hydrophobic compound triclosan in an aqueous medium containing sorbing SiO2 nanoparticles (NPs). It is found that these NPs, as well as their complexes with triclosan, partition between the bulk medium and the solid

  10. Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

    Zielinska, K.


    Solid phase microextraction (SPME) is applied in the speciation analysis of the hydrophobic compound triclosan in an aqueous medium containing sorbing SiO2 nanoparticles (NPs). It is found that these NPs, as well as their complexes with triclosan, partition between the bulk medium and the solid phas

  11. Solid-phase micro-extraction in bioanalysis, exemplified by lidocaine determination

    de Jong, GJ; Koster, EHM


    Solid-phase micro-extraction (SPME) is a never sample preparation technique that can be used for gaseous, liquid or solid samples in conjunction with GC, HPLC or CE (e.g. [1]). The use of SPME for the analysis of drugs in biofluids is also becoming popular (e.g. [2]). The principle is that a fused s

  12. Al-MoSi2 Composite Materials: Analysis of Microstructure, Sliding Wear, Solid Particle Erosion, and Aqueous Corrosion

    Gousia, V.; Tsioukis, A.; Lekatou, A.; Karantzalis, A. E.


    In this effort, AMCs reinforced with new intermetallic phases, were produced through casting and compared as far as their microstructure, sliding wear, solid particle erosion, and aqueous corrosion response. Casting was selected as a production method based on the concept: (a) ease-to-handle and low cost production route and (b) optimum homogeneity of the reinforcing phase distribution. The MoSi2 phase was produced through vacuum arc melting and the resulting drops were milled for 30 h to produce fine powder, the characteristics of which were ascertained through SEM-EDS and XRD analysis. MoSi2 was used as precursor source for the final reinforcing phase. The powder material was incorporated in molten Al1050 alloy to additions of 2, 5 and 10 vol.% respectively. Extensive reactivity between the molten Al and the MoSi2 particles was observed, leading to the formation of new reinforcing phases mainly of the Al-Mo system. In all cases, a uniform particle distribution was observed, mainly characterized by isolated intermetallic phases and few intermetallic phase clusters. Sliding wear showed a beneficial action of the reinforcing phase on the wear of the composites. Surface oxidation, plastic deformation, crack formation, and debris abrasive action were the main degradation features. The results of solid particle erosion showed that the mechanism is different as the impact angle and the vol.% change. Regarding the corrosion, the analysis revealed localized corrosion effects. The composite behavior was not altered significantly compared to that of the monolithic matrix.

  13. Isostructural solid-solid phase transition in monolayers of soft core-shell particles at fluid interfaces: structure and mechanics.

    Rey, Marcel; Fernández-Rodríguez, Miguel Ángel; Steinacher, Mathias; Scheidegger, Laura; Geisel, Karen; Richtering, Walter; Squires, Todd M; Isa, Lucio


    We have studied the complete two-dimensional phase diagram of a core-shell microgel-laden fluid interface by synchronizing its compression with the deposition of the interfacial monolayer. Applying a new protocol, different positions on the substrate correspond to different values of the monolayer surface pressure and specific area. Analyzing the microstructure of the deposited monolayers, we discovered an isostructural solid-solid phase transition between two crystalline phases with the same hexagonal symmetry, but with two different lattice constants. The two phases corresponded to shell-shell and core-core inter-particle contacts, respectively; with increasing surface pressure the former mechanically failed enabling the particle cores to come into contact. In the phase-transition region, clusters of particles in core-core contacts nucleate, melting the surrounding shell-shell crystal, until the whole monolayer moves into the second phase. We furthermore measured the interfacial rheology of the monolayers as a function of the surface pressure using an interfacial microdisk rheometer. The interfaces always showed a strong elastic response, with a dip in the shear elastic modulus in correspondence with the melting of the shell-shell phase, followed by a steep increase upon the formation of a percolating network of the core-core contacts. These results demonstrate that the core-shell nature of the particles leads to a rich mechanical and structural behavior that can be externally tuned by compressing the interface, indicating new routes for applications, e.g. in surface patterning or emulsion stabilization.

  14. Enhancing heat capacity of colloidal suspension using nanoscale encapsulated phase-change materials for heat transfer.

    Hong, Yan; Ding, Shujiang; Wu, Wei; Hu, Jianjun; Voevodin, Andrey A; Gschwender, Lois; Snyder, Ed; Chow, Louis; Su, Ming


    This paper describes a new method to enhance the heat-transfer property of a single-phase liquid by adding encapsulated phase-change nanoparticles (nano-PCMs), which absorb thermal energy during solid-liquid phase changes. Silica-encapsulated indium nanoparticles and polymer-encapsulated paraffin (wax) nanoparticles have been made using colloid method, and suspended into poly-alpha-olefin (PAO) and water for potential high- and low-temperature applications, respectively. The shells prevent leakage and agglomeration of molten phase-change materials, and enhance the dielectric properties of indium nanoparticles. The heat-transfer coefficients of PAO containing indium nanoparticles (30% by mass) and water containing paraffin nanoparticles (10% by mass) are 1.6 and 1.75 times higher than those of corresponding single-phase fluids. The structural integrity of encapsulation allows repeated use of such nanoparticles for many cycles in high heat generating devices.

  15. Molecularly imprinted solid-phase extraction for the screening of antihyperglycemic biguanides.

    Feng, Sherry Y; Lai, Edward P C; Dabek-Zlotorzynska, Ewa; Sadeghi, Susan


    A new molecularly imprinted polymer (MIP) was specifically synthesized as a smart material for the recognition of metformin hydrochloride in solid-phase extraction. Particles of this MIP were packed into a stainless-steel tubing (50 mm x 0.8 mm i.d.) equipped with an exit frit. This micro-column was employed in the development of a molecularly imprinted solid-phase extraction (MISPE) method for metformin determination. The MISPE instrumentation consisted of a micrometer pump, an injector valve equipped with a 20-microl sample loop, a UV detector, and an integrator. With CH3CN as the mobile phase flowing at 0.5 ml/min, 95 +/- 2% binding could be achieved for 1200 ng of metformin from one injection of a phosphate-buffered sample solution (pH 2.5). Methanol + 3% trifluoroacetic acid was good for quantitative pulsed elution (PE) of the bound metformin. The MISPE-PE method, with UV detection at 240 nm, afforded a detection limit of 16 ng (or 0.8 microg/ml) for metformin. However, the micro-column interacted indiscriminately with phenformin with a 49 +/- 2% binding. A systematic investigation of binding selectivity was conducted with respect to sample composition (including the solvent, matrix, pH, buffer and surfactant effects). An intermediate step of differential pulsed elution used acetonitrile with 5% picric acid to remove phenformin and other structural analogues. A final pulsed elution of metformin for direct UV detection was achieved using 3% trifluoroacetic acid in methanol.

  16. Application of material flow analysis to municipal solid waste in Maputo City, Mozambique.

    Dos Muchangos, Leticia Sarmento; Tokai, Akihiro; Hanashima, Atsuko


    Understanding waste flows within an urban area is important for identifying the main problems and improvement opportunities for efficient waste management. Assessment tools such as material flow analysis (MFA), an extensively applied method in waste management studies, provide a structured and objective evaluating process to characterize the waste management system best, to identify its shortcomings and to propose suitable strategies. This paper presents the application of MFA to municipal solid waste management (MSWM) in Maputo City, the capital of Mozambique. The results included the identification and quantification of the main input and output flows of the MSWM system in 2007 and 2014, from the generation, material recovery and collection, to final disposal and the unaccounted flow of municipal solid waste (MSW). We estimated that the waste generation increased from 397×10(3) tonnes in 2007 to 437×10(3) tonnes in 2014, whereas the total material recovery was insignificant in both years - 3×10(3) and 7×10(3) tonnes, respectively. As for collection and final disposal, the official collection of waste to the local dumpsite in the inner city increased about threefold, from 76×10(3) to 253×10(6) tonnes. For waste unaccounted for, the estimates indicated a reduction during the study period from 300×10(3) to 158×10(3) tonnes, due to the increase of collection services. The emphasized aspects include the need for practical waste reduction strategies, the opportunity to explore the potential for material recovery, careful consideration regarding the growing trend of illegal dumping and the urgency in phasing-out from the harmful practice of open dumping.

  17. Solid Phase Equilibria in the Pi-Ga-As and Pt-Ga-Sb Systems


    OFFICE OF NAVAL RESEARCH Research Contract N00014-87-K-0014 R&T Code 413E026---01 AD-A 198 654 TECHNICAL REPORT No. 9 SOLID PHASE EQUILIBRIA IN THE...Classtcation) UNCLASSLFIED: Tech.Rept.#9 SOLID PHASE EQUILIBRIA IN T11: Pt-Ga-As AND Pt-Ga-Sb SYST’IS 12 PERSONAL AuTiOR(S) C.T. Tsai and R.S. Williats 13a TYPE

  18. Expedient protocol for solid-phase synthesis of secondary and tertiary amines

    Olsen, Christian A; Witt, Matthias; Jaroszewski, Jerzy W


    [reaction: see text] An expedient solid-phase synthetic approach to secondary and tertiary amines was developed. The protocol employs conversion of resin-bound amino alcohols to the corresponding iodides, followed by iodide displacement with primary or secondary amines or with unprotected amino...... alcohols. This two-step procedure, affording products in good to excellent yields, is suitable for solid-phase synthesis of polyamines....

  19. Multivariate Quantification of the Solid State Phase Composition of Co-Amorphous Naproxen-Indomethacin

    Beyer, Andreas; Grohganz, Holger; Löbmann, Korbinian


    regression approach that enables the simultaneous determination of up to four solid state fractions: crystalline naproxen, γ-indomethacin, α-indomethacin as well as co-amorphous naproxen-indomethacin. For this purpose, a calibration set that covers the whole range of possible combinations of the four...... four solid state phases, involving one co-amorphous phase, can be quantified with this XRPD data-based approach....

  20. The MAX Phases: Unique New Carbide and Nitride Materials

    Barsoum, Michel W.; El-Raghy, Tamer


    One of the major challenges in engineering is the need for versatile materials to serve rapidly developing technologies. For durability and high performance in extreme environments, metals seem ideal: They are electrical and thermal conductors, damage-tolerant and able to withstand high temperatures. Ceramics offer a different set of qualities, being elastically rigid, lightweight, resistant to fatigue and oxidation and even better at enduring high temperatures. An ideal high-performance structural material for, say, jet engines would have all these qualities—and a new class of materials being explored by the authors meets the test. They are fabricating layered materials combining transition metals, carbon or nitrogen and silicon or a related material. The materials form a new class of solids, the nanolaminates, which exhibits new physics along with unusual machinability.

  1. Confined crystals of the smallest phase-change material.

    Giusca, Cristina E; Stolojan, Vlad; Sloan, Jeremy; Börrnert, Felix; Shiozawa, Hidetsugu; Sader, Kasim; Rümmeli, Mark H; Büchner, Bernd; Silva, S Ravi P


    The demand for high-density memory in tandem with limitations imposed by the minimum feature size of current storage devices has created a need for new materials that can store information in smaller volumes than currently possible. Successfully employed in commercial optical data storage products, phase-change materials, that can reversibly and rapidly change from an amorphous phase to a crystalline phase when subject to heating or cooling have been identified for the development of the next generation electronic memories. There are limitations to the miniaturization of these devices due to current synthesis and theoretical considerations that place a lower limit of 2 nm on the minimum bit size, below which the material does not transform in the structural phase. We show here that by using carbon nanotubes of less than 2 nm diameter as templates phase-change nanowires confined to their smallest conceivable scale are obtained. Contrary to previous experimental evidence and theoretical expectations, the nanowires are found to crystallize at this scale and display amorphous-to-crystalline phase changes, fulfilling an important prerequisite of a memory element. We show evidence for the smallest phase-change material, extending thus the size limit to explore phase-change memory devices at extreme scales.

  2. Solid-Phase Synthesis of PEGylated Lipopeptides Using Click Chemistry

    Jølck, Rasmus Irming; Berg, Rolf Henrik; Andresen, Thomas Lars


    A versatile methodology for efficient synthesis of PEGylated lipopeptides via CuAAC “Click” conjugation between alkyne-bearing solid-supported lipopeptides and azido-functionalized PEGs is described. This new and very robust method offers a unique platform for synthesizing PEGylated lipopeptides...

  3. Design and Analysis of Phase Change Material based thermal energy storage for active building cooling: a Review

    Nitin .D. Patil


    Full Text Available Phase Change Materials (PCMs are "latent" thermal storage materials. They use chemical bonds to store and release heat. The thermal energy transfer occurs when a material changes from a solid to a liquid orfrom a liquid to a solid form. This is called a change in state or "phase." Initially, these solid-liquid PCMs perform like conventional storage materials; their temperature rises as they absorb solar heat. Unlike conventional heat storage materials, when PCMs reach the temperature at which they change phase (their melting point, they absorb large amounts of heat without getting hotter. When the ambient temperature in the space around the PCM material drops, the Phase Change Material solidifies, releasing its stored latent heat. PCMs absorb and emit heat while maintaining a nearly constant temperature. Within the human comfort and electronic-equipment tolerance range of 20°C to 35°C, latent thermal storage materials are very effective.They can be used for equalization of day & night temperature and for transport of refrigerated products. In the proposed project heat of fusion of Cacl2. 6H2o as PCM is used for cooling water during night and this cooled water is used as circulating medium trough fan coil unit, air trough FCU will get cooled by transferring heat to water and fresh & cool air will be thrown in a room. In the proposed project FREE COOLING & ACTIVE BUILDING COOLING concepts of Thermal Energy Storage are used in combine

  4. Molecularly imprinted polymer grafted to porous polyethylene frits: a new selective solid-phase extraction format.

    Barahona, Francisco; Turiel, Esther; Martín-Esteban, Antonio


    In this paper, a novel format for selective solid-phase extraction based on a molecularly imprinted polymer (MIP) is described. A small amount of MIP has been synthesized within the pores of commercial polyethylene (PE) frits and attached to its surface using benzophenone (BP), a photo-initiator capable to start the polymerisation from the surface of the support material. Key properties affecting the obtainment of a proper polymeric layer, such as polymerisation time and kind of cross-linker were optimised. The developed imprinted material has been applied as a selective sorbent for cleaning extracts of thiabendazole (TBZ), as model compound, from citrus samples. The use of different solvents for loading the analyte in the imprinted frits was investigated, as well as the binding capacity of the imprinted polymer. Imprinted frits showed good selectivity when loads were performed using toluene and a linear relationship was obtained for the target analyte up to 1000 ng of loaded analyte. Prepared composite material was applied to the SPE of TBZ in real samples extracts, showing an impressive clean-up ability. Calibrations showed good linearity in the concentration range of 0.05-5.00 μg g(-1), referred to the original solid sample, and the regression coefficients obtained were greater than 0.996. The calculated detection limit was 0.016 μg g(-1), low enough to satisfactory analysis of TBZ in real samples. RSDs at different spiking levels ranged below 15% in all the cases and imprinted frits were reusable without loss in their performance.

  5. 固相萃取-气相色谱法测定食品包装材料中邻苯二甲酸酯类物质%Determination of Phthalate Esters in Plastic Food Packing Materials by Solid Phase Extraction-Gas Chromatography

    曹小妹; 吴晓燕; 李挥; 张敬轩; 高文惠


    建立采用固相萃取-气相色谱法同时分析检测邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸丁基苄基酯(BBP)和邻苯二甲酸二-2-乙基己酯(DEHP)4种邻苯二甲酸酯类物质的方法。研究塑料包装材料中邻苯二甲酸酯类在水、65%乙醇、4%乙酸、正己烷4种模拟液中的溶出及利用固相萃取技术对浸出液进行富集的情况,考察气相色谱操作条件对4种邻苯二甲酸酯类物质分离的影响。结果表明,该方法具有良好的线性相关性,线性相关系数在0.9986~0.9994之间;回收率在80.63%~95.50%之间;DBP、BBP、DCHP和DEHP的检测限分别是0.050、0.010、0.055μg/mL和0.012μg/mL。该方法样品预处理简便,测定方法灵敏、可靠,可用于食品包装材料中邻苯二甲酸酯类的监测。%A method was developed by solid phase extraction-gas chromatography for the simultaneous determination of dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), dicyclohexyl phthalate (DCHP) and di-2-ethylhexyl phthalate (DEHP) in plastic food packing materials. The dissolution of phthalate esters from plastic packing materials into water, 65% alcohol, 4% acetic acid and n-hexane was studied. The enrichment of phthalate esters in extraction solution was conducted by solid phase extraction. The effect of gas chromatographic conditions on the separation of four phthalate esters was investigated. The results showed that the method had an excellent linear relationship with the correlation coefficient of 0.9986--0.9994. The recovery rates and detection limits of this method for DBP, BBP, DCHP and DEHP were 80.63% - 95.50%, and 0.050, 0.010, 0.055 and 0.012 μg/mL, respectively. This developed method is easy, sensitive and reliable, which can be used to analyze phthalate esters in plastic food packing materials.

  6. Effects of Microencapsulated Phase Change Material (MPCM) on Critical Heat Flux in Pool Boiling

    Park, Sung Dae; Kim, Seong Man; Kang, Sarah; Lee, Seung Won; Seo, Han; Bang, In Cheol [Ulsan National Institute of Science and Technology, Ulsan (Korea, Republic of)


    Thermal power is limited by critical heat flux (CHF) in the nuclear power plant. And the in-vessel retention by external reactor vessel cooling (IVR-ERVC) is applied in some nuclear power plants; AP600, AP1000, Loviisa and APR1400. The heat removal capacity of IVR-ERVC is also restricted by CHF. So, it is essential to get CHF margin to improve an economics and a safety of the plant. There are some typical approaches to enhance CHF: vibrating the heater or fluid, coating with porous media on the heater surface, applying an electric field. The recent study related to the CHF is focus on using the nanofluid. In this paper, the new approach was investigated by using the microencapsulated phase change material (MPCM). MPCM is the particles whose diameter is from 0.1{mu}m to 1000{mu}m. The MPCM consists of the core material and the shell material. The core material can be solid, liquid, gas or even the mixture. The solid paraffin is the best candidate as the core material due to its stable chemical and thermal properties. And the shell material is generally synthesized polymer of about several micrometers in thickness. The most interesting feature of the MPCM is that the latent heat associated with the solid-liquid phase change is related to the heat transfer. When the MPCM is dispersed into the carrier fluid, a kind of suspension named as microencapsulated phase change slurry (MPCS) is formed. The study on the MPCS was conducted in field of both the heat transfer fluids and energy storage media. It is inspired by the fact that the latent heat can serve distribution to the additional CHF margin. The purpose of this work is to confirm whether or not the CHF is enhanced

  7. CO2-Doped Diamond: A Potential Solid-State CO2 Laser Material?

    Tratt, D.


    This paper describes a novel concept for a solid-state CO subscript 2 laser medium which, by eschewing the gas-phase approach, may offer prospects for a compact, robust 9 - 11 (micro)m coherent source, coupled with the potentially superior frequency stability characteristics afforded by monolithic solid-state construction.

  8. Direct MD simulation of liquid-solid phase equilibria for two-component plasmas

    Schneider, A S; Horowitz, C J; Berry, D K


    We determine the liquid-solid phase diagram for carbon-oxygen plasma mixtures using two-phase MD simulations. We identified liquid, solid, and interface regions using a bond angle metric. To study finite size effects, we perform 55296 ion simulations and compare to earlier 27648 ion results. To help monitor non-equilibrium effects, we calculate diffusion constants $D_i$. We find that $D_O$ for oxygen ions in the solid is much smaller than $D_C$ for carbon ions and that both diffusion constants are 80 or more times smaller than diffusion constants in the liquid phase. There is excellent agreement between our phase diagram and that predicted by Medin and Cumming. This suggests that errors from finite size and non-equilibrium effects are small and that the carbon-oxygen phase diagram is now accurately known.

  9. Numerical Simulation of Erosion-Corrosion in the Liquid Solid Two-Phase Flow


    Erosion-corrosion of liquid-solid two-phase flow occurring in a pipe with sudden expansion in cross section is numerically simulated in this paper. The global model for erosion-corrosion process includes three main components: the liquid-solid two-phase flow model, erosion model and corrosion model. The Euierian-Lagranglan approach is used to simulate liquid-solid two-phase flow, while the stochastic trajectory model was adopted to obtain properties of particle phase. Two-way coupling effect between the fluid and the particle phase is considered in the model. The accuracy of the models is tested by the data in the reference. The comparison shows that the model is basically correct and feasible.

  10. Molecularly imprinted polymer/cryogel composites for solid-phase extraction of bisphenol A from river water and wine.

    Baggiani, Claudio; Baravalle, Patrizia; Giovannoli, Cristina; Anfossi, Laura; Giraudi, Gianfranco


    Superporous monolithic hydrogels (cryogel monoliths) are elastic, sponge-like materials that can be prepared in an aqueous medium through a cryotropic gelation technique. These monoliths show interesting properties for the development of high-throughput solid-phase extraction supports to treat large volumes of aqueous samples. In this work, a cryogel-supported molecularly imprinted solid-phase extraction approach for the endocrine disruptor bisphenol A (BPA) from river water and wine samples is presented. An imprinted polymer with molecular recognition properties for BPA was prepared in acetonitrile by thermal polymerization of a mixture of 4,4'-dihydroxy-2,2-diphenyl-1,1,1,3,3,3-trifluoropropane as a mimic template of BPA, 4-vinylpyridine and trimethylolpropane trimethacrylate in a molar ratio of 1 + 6 + 6. Fine imprinted particles (extraction approach to recover BPA from dilute aqueous samples with minimum pre-loading work-up. The optimized extraction protocol resulted in a reliable MISPE method suitable to selectively extract and preconcentrate BPA from river water and red wine samples, demonstrating the practical feasibility of cryogel-trapped imprinted polymers as solid-phase extraction materials.

  11. Fabrication of metal-organic frameworks and graphite oxide hybrid composites for solid-phase extraction and preconcentration of luteolin.

    Wang, Yang; Wu, Yichun; Ge, Huali; Chen, Huanhuan; Ye, Guiqin; Hu, Xiaoya


    A novel solid-phase extraction sorbent, metal-organic frameworks and graphite oxide hybrid composite, was prepared by a solvothermal technique. The morphology and properties of the resultant material were examined by Fourier transform infrared spectroscopy, X-ray diffraction and field emission scanning electron microscopy. To evaluate the extraction performance of the resultant sorbent, luteolin was chosen as a model analyte. The extraction conditions were optimized. Based on these, a convenient and efficient solid-phase extraction procedure for the determination of luteolin was established and the subsequent quantification step was performed by square wave anodic stripping voltammetry. Under the optimal conditions, the oxidation current increased linearly with increasing the concentration of luteolin in the range of 5.0 × 10(-9)-5.0 × 10(-7)molL(-1) with a correlation coefficient of 0.9983 and a detection limit of 7.9 × 10(-10)molL(-1). The relative standard deviation of seven successive scans was 4.20% for 5.0 × 10(-8)molL(-1) luteolin. This work not only proposes a useful method for sample pretreatment, but also reveals the great potential of metal-organic frameworks based hybrid materials as an excellent sorbent in solid-phase extraction.

  12. Thermal Diffusivity and Thermal Conductivity of Five Different Steel Alloys in the Solid and Liquid Phases

    Wilthan, B.; Schützenhöfer, W.; Pottlacher, G.


    The need for characterization of thermophysical properties of steel and nickel-based alloys was addressed in the FFG-Bridge Project 810999 in cooperation with a partner from industry, Böhler Edelstahl GmbH & Co KG. To optimize numerical simulations of production processes, such as remelting or plastic deformation, additional, and more accurate data were necessary for the alloys under investigation. With a fast ohmic pulse heating circuit system, the temperature-dependent specific electrical resistivity, density, and specific heat capacity for a set of five high alloyed steels were measured. Hence, using the Wiedemann-Franz law with a Lorenz number of , the thermal diffusivity and thermal conductivity could be calculated for the solid and liquid phases up to temperatures of 2500 K. This experimental approach is limited by the following requirements for the specimens: they have to be electrically conducting, the melting point has to be high enough for the implemented pyrometric temperature measurement, and one has to be able to draw wires of the material. The latter restriction is technologically challenging with some of the materials being very brittle. For all samples, electrical and temperature signals are recorded and a fast shadowgraph method is used to measure the volume expansion. For each material under investigation, a set of data including the chemical composition, the density at room temperature, solidus and liquidus temperatures, and the change of enthalpy, resistivity, density, thermal conductivity, and thermal diffusivity as a function of temperature is reported.

  13. Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

    Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon


    We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

  14. Perhydroazulene-based liquid-crystalline materials with smectic phases.

    Hussain, Zakir; Hopf, Henning; Eichhorn, S Holger


    New liquid-crystalline materials with a perhydroazulene core were synthesized and the stereochemistry of these compounds was investigated. The mesomorphic properties of the new LC compounds were investigated by differential scanning colorimetry, polarizing optical microscopy and X-ray diffraction. We report here on the LC properties of nonchiral materials, which predominantly exhibit smectic phases and display nematic phases only within narrow temperature ranges. The dependence of the mesogenic behavior of the new materials on the stereochemistry of the core system was also investigated. All newly synthesized compounds were fully characterized by the usual spectroscopic and analytical methods.

  15. Perhydroazulene-based liquid-crystalline materials with smectic phases

    Zakir Hussain


    Full Text Available New liquid-crystalline materials with a perhydroazulene core were synthesized and the stereochemistry of these compounds was investigated. The mesomorphic properties of the new LC compounds were investigated by differential scanning colorimetry, polarizing optical microscopy and X-ray diffraction. We report here on the LC properties of nonchiral materials, which predominantly exhibit smectic phases and display nematic phases only within narrow temperature ranges. The dependence of the mesogenic behavior of the new materials on the stereochemistry of the core system was also investigated. All newly synthesized compounds were fully characterized by the usual spectroscopic and analytical methods.

  16. New insights into the thermal behaviour of organic ionic plastic crystals: magnetic resonance imaging of polycrystalline morphology alterations induced by solid-solid phase transitions.

    Romanenko, Konstantin; Pringle, Jennifer M; O'Dell, Luke A; Forsyth, Maria


    Organic ionic plastic crystals (OIPCs) show strong potential as solid-state electrolytes for lithium battery applications, demonstrating promising electrochemical performance and eliminating the need for a volatile and flammable liquid electrolyte. The ionic conductivity (σ) in these systems has recently been shown to depend strongly on polycrystalline morphology, which is largely determined by the sample's thermal history. [K. Romanenko et al., J. Am. Chem. Soc., 2014, 136, 15638]. Tailoring this morphology could lead to conductivities sufficiently high for battery applications, so a more complete understanding of how phenomena such as solid-solid phase transitions can affect the sample morphology is of significant interest. Anisotropic relaxation of nuclear spin magnetisation provides a new MRI based approach for studies of polycrystalline materials at both a macroscopic and molecular level. In this contribution, morphology alterations induced by solid-solid phase transitions in triisobutyl(methyl)phosphonium bis(fluorosulfonyl)imide (P1444FSI) and diethyl(methyl)(isobutyl)phosphonium hexafluorophosphate (P1224PF6) are examined using magnetic resonance imaging (MRI), alongside nuclear magnetic resonance (NMR) spectroscopy, diffusion measurements and conductivity data. These observations are linked to molecular dynamics and structural behaviour crucial for the conductive properties of OIPCs. A distinct correlation is established between the conductivity at a given temperature, σ(T), and the intensity of the narrow NMR signal that is attributed to a mobile fraction, fm(T), of ions in the OIPC. To explain these findings we propose an analogy with the well-studied relationship between permeability (k) and void fraction (θ) in porous media, with k(θ) commonly quantified by a power-law dependence that can also be employed to describe σ(fm).

  17. Solid Phase Extraction for Monitoring of Occupational Exposure to Cr (III

    S.J. Shahtaheri


    Full Text Available Chromium is an important constituent widely used in different industrial processes for production of various synthetic materials. For evaluation of workers’ exposure to trace toxic metal of Cr (III, environmental and biological monitoring are essential processes, in which, preparation of samples is one of the most time-consuming and error-prone aspects prior to analysis. The use of solid-phase extraction (SPE has grown and is a fertile technique of sample preparation as it provides better results than those produced by liquid-liquid extraction (LLE. SPE using mini columns filled with XAD-4 resin was optimized regarding to sample pH, ligand concentration, loading flow rate, elution solvent, sample volume, elution volume, amount of resins, and sample matrix interferences. Chromium was retained on solid sorbent and was eluted with 2 M HNO3 followed by simple determination of analytes by using flame atomic absorption spectrometery. Obtained recoveries of metal ion were more than 92%. The optimized procedure was also validated with three different pools of spiked urine samples and showed a good reproducibility over six consecutive days as well as six within-day experiments. Through this study, suitable results were obtained for relative standard deviation, therefore, it is concluded that, this optimized method can be considered to be successful in simplifying sample preparation for trace residue analysis of Cr in different matrices for evaluation of occupational and environmental exposures. To evaluate occupational exposure to chromium, 16 urine samples were taken, prepared, and analyzed based on optimized procedure.

  18. Evaporation induced orientational order in soft solid phases of clays

    Lindbo Hansen, Elisabeth; Hemmen, Henrik; Dommersnes, Paul; Fossum, Jon Otto


    We demonstrate experimentally the possibility for promoting uniaxial orientational order in initially isotropic, soft solid dispersions of the synthetic clays Na-fluorohectorite and Laponite RD. We observe that strong orientational order can emerge from initially isotropic states when the samples are subjected to a slow concentration increase through evaporation of the dispersion water. During evaporation, there is a gradient in the order which, if evaporation is halted, slowly relaxes towards a uniform order throughout the samples. It is evident that the development of orientational order is not counterindicated by the viscoelastic nature of the samples, and that although the translational and likely also rotational diffusion of the particles is restricted in the soft solid state, the orientational degree of freedom can undergo a transition from a collectively random to an ordered state.

  19. New insights in Microbial Fuel Cells: novel solid phase anolyte

    Tommasi, Tonia; Salvador, Gian Paolo; Quaglio, Marzia


    For the development of long lasting portable microbial fuel cells (MFCs) new strategies are necessary to overcome critical issues such as hydraulic pump system and the biochemical substrate retrieval overtime to sustain bacteria metabolism. The present work proposes the use of a synthetic solid anolyte (SSA), constituted by agar, carbonaceous and nitrogen sources dissolved into diluted seawater. Results of a month-test showed the potential of the new SSA-MFC as a long lasting low energy consuming system.

  20. Solid-liquid phase diagram of disubstituted benzene systems

    黑恩成; 刘国杰


    The cooling curves of different compositions of the systems of ortho-chlorotoluene/para-chlorotoluene and ortho-nitrochlorobenzene/para-nitrochlorobenzene are carefully determined by the thermal analysis method. The crystals obtained are also tested. The conclusion that both systems are of simple eutectic diagram but not the solid solution diagram with a minimum melting point is confirmed. The characteristics of the diagram are explained according to the physical and thermodynarmc properties of the components.

  1. Phase transition of solid bismuth under high pressure

    Chen, Hai-Yan; Xiang, Shi-Kai; Yan, Xiao-Zhen; Zheng, Li-Rong; Zhang, Yi; Liu, Sheng-Gang; Bi, Yan


    As a widely used pressure calibrator, the structural phase transitions of bismuth from phase I, to phase II, to phase III, and then to phase V with increasing pressure at 300 K have been widely confirmed. However, there are different structural versions for phase III, most of which are determined by x-ray diffraction (XRD) technology. Using x-ray absorption fine structure (XAFS) measurements combined with ab initio calculations, we show that the proposed incommensurate composite structure of bismuth of the three configurations is the best option. An abnormal continuous increase of the nearest-neighbor distance of phase III with elevated pressure is also observed. The electronic structure transformation from semimetal to metal is responsible for the complex behavior of structure transformation. Project supported by the National Natural Science Foundation of China (Grant Nos. 10904133, 11304294, 11274281, 11404006, and U1230201), the Development Foundation of China Academy of Engineering Physics (Grant Nos. 2015B0101004, 2013B0401062, and 2012A0101001), the Research Foundation of the Laboratory of Shock Wave and Detonation, China (Grant No. 9140C670201140C67282).

  2. Effect of shear stress in ferroelectric solid solutions with coexisting phases

    Lu, Xiaoyan; Zhang, Hangbo; Zheng, Limei; Cao, Wenwu


    One common feature of ferroelectric solid solutions with large piezoelectricity is the coexistence of two or more phases. Due to the strain mismatch among coexisting phases, adaptive structures near the interfaces or domain walls develop to maintain the atomic coherency. Shear stresses commonly exist, especially when the domain size is small. The effect of shear stresses on phase morphology in Pb(Zr1-xTix)O3 solid solutions with compositions within the morphotropic phase boundary region was studied within the framework of Landau phenomenological theory. Our results show that the coexisting rhombohedral (R) and tetragonal (T) phases can be modified to form stable or metastable R-like and/or T-like monoclinic phases under shear stresses. Large stresses may also induce first order or second order phase transitions.

  3. Temperature and phase dependence of positron lifetimes in solid cyclohexane

    Eldrup, Morten Mostgaard


    The temperature dependence of position lifetimes in both the brittle and plastic phases of cyclohaxane has been examined. Long-lived components in both phases are associated with the formation of positronium (Ps). Two long lifetimes attributable to ortho-Ps are resolvable in the plastic phase....... The longer of these (≈ 2.5 ns), which is temperature dependent, is ascribed to ortho-Ps trapped at vacancies. The shorter lifetime (≈ 0.9 ns), shows little temperature dependence. In contrast to most other plastic crystals, no sigmoidal behaviour of the average ortho-Ps lifetime is observed. A possibility...

  4. Solid phase extraction of lactic acid from fermentation broth by anion-exchangeable silica confined ionic liquids.

    Bi, Wentao; Zhou, Jun; Row, Kyung Ho


    Three anion-exchangeable, silica-confined ionic liquids were synthesized for solid phase extraction of lactic acid from fermentation broth, followed by high-performance liquid chromatography coupled to ultraviolet detection. By comparing the adsorption isotherms of lactic acid on different silica-confined ionic liquids, interactions between the lactic acid and sorbents were investigated. The adsorbed amounts were then fitted into different adsorption isotherm equations; finally, the Langmuir equation was selected. Then the imidazolium silica with the highest adsorption capacity of lactic acid was packed into a cartridge for solid phase extraction. The loading volume of the cartridge was optimized by the Langmuir equation and geometry. After washing with distilled water and eluting with 0.25 mol L(-1) of an HCl solution, the lactic acid was separated from interference with a recovery yield of 91.9%. Furthermore, this kind of anion-exchangeable material exhibited potential for industrial applications and separation of other anionic bioactive compounds.

  5. Characterizaticr of Solid State Laser and Nonlinear Optical Materials.


    materials useful in the different methods for obtaining frequency agility: narrow line emitters with multiple lasing channels and nonlinear optical materials . In...codoped with two or more rare earth ions were studied and computers models developed to explain their spectral dynamics. The nonlinear optical materials investigated

  6. Solid-liquid phase equilibria of the Gaussian core model fluid.

    Mausbach, Peter; Ahmed, Alauddin; Sadus, Richard J


    The solid-liquid phase equilibria of the Gaussian core model are determined using the GWTS [J. Ge, G.-W. Wu, B. D. Todd, and R. J. Sadus, J. Chem. Phys. 119, 11017 (2003)] algorithm, which combines equilibrium and nonequilibrium molecular dynamics simulations. This is the first reported use of the GWTS algorithm for a fluid system displaying a reentrant melting scenario. Using the GWTS algorithm, the phase envelope of the Gaussian core model can be calculated more precisely than previously possible. The results for the low-density and the high-density (reentrant melting) sides of the solid state are in good agreement with those obtained by Monte Carlo simulations in conjunction with calculations of the solid free energies. The common point on the Gaussian core envelope, where equal-density solid and liquid phases are in coexistence, could be determined with high precision.

  7. Study of solid solution strengthening of alloying element with phase structure factors


    Using the empirical electron theory of solids and molecules (EET), the phase structure factors, nA and nB, of the carbon-containing structural units with mass fraction of carbon (wC) below 0.8% and the mono-alloy structural units with wC at 0.2% in austenite and martensite are calculated. The solid solution strengthening brought by C-containing interstitial solid solution and alloy-substitutional solid solution in γ-Fe and α-Fe is discussed at electron structural level. The coefficient (s) of solid solution strengthening is advanced according to the bonding force between atoms. The study shows that when the criterion is applied to the carbonaceous or alloying element-containing solid solution the results of calculation will coincide with the experimental result very well.

  8. Modeling the Reactions of Energetic Materials in the Condensed Phase

    Fried, L E; Manaa, M R; Lewis, J P


    High explosive (HE) materials are unique for having a strong exothermic reactivity, which has made them desirable for both military and commercial applications. Although the history of HE materials is long, condensed-phase properties are poorly understood. Understanding the condensed-phase properties of HE materials is important for determining stability and performance. Information regarding HE material properties (for example, the physical, chemical, and mechanical behaviors of the constituents in plastic-bonded explosive, or PBX, formulations) is necessary in efficiently building the next generation of explosives as the quest for more powerful energetic materials (in terms of energy per volume) moves forward. In addition, understanding the reaction mechanisms has important ramifications in disposing of such materials safely and cheaply, as there exist vast stockpiles of HE materials with corresponding contamination of earth and groundwater at these sites, as well as a military testing sites The ability to model chemical reaction processes in condensed phase energetic materials is rapidly progressing. Chemical equilibrium modeling is a mature technique with some limitations. Progress in this area continues, but is hampered by a lack of knowledge of condensed phase reaction mechanisms and rates. Atomistic modeling is much more computationally intensive, and is currently limited to very short time scales. Nonetheless, this methodology promises to yield the first reliable insights into the condensed phase processes responsible for high explosive detonation. Further work is necessary to extend the timescales involved in atomistic simulations. Recent work in implementing thermostat methods appropriate to shocks may promise to overcome some of these difficulties. Most current work on energetic material reactivity assumes that electronically adiabatic processes dominate. The role of excited states is becoming clearer, however. These states are not accessible in perfect

  9. Nature of hardness evolution in nanocrystalline NiTi shape memory alloys during solid-state phase transition

    Amini, Abbas; Cheng, Chun


    Due to a distinct nature of thermomechanical smart materials' reaction to applied loads, a revolutionary approach is needed to measure the hardness and to understand its size effect for pseudoelastic NiTi shape memory alloys (SMAs) during the solid-state phase transition. Spherical hardness is increased with depths during the phase transition in NiTi SMAs. This behaviour is contrary to the decrease in the hardness of NiTi SMAs with depths using sharp tips and the depth-insensitive hardness of traditional metallic alloys using spherical tips. In contrast with the common dislocation theory for the hardness measurement, the nature of NiTi SMAs' hardness is explained by the balance between the interface and the bulk energy of phase transformed SMAs. Contrary to the energy balance in the indentation zone using sharp tips, the interface energy was numerically shown to be less dominant than the bulk energy of the phase transition zone using spherical tips. PMID:23963305

  10. Nature of hardness evolution in nanocrystalline NiTi shape memory alloys during solid-state phase transition.

    Amini, Abbas; Cheng, Chun


    Due to a distinct nature of thermomechanical smart materials' reaction to applied loads, a revolutionary approach is needed to measure the hardness and to understand its size effect for pseudoelastic NiTi shape memory alloys (SMAs) during the solid-state phase transition. Spherical hardness is increased with depths during the phase transition in NiTi SMAs. This behaviour is contrary to the decrease in the hardness of NiTi SMAs with depths using sharp tips and the depth-insensitive hardness of traditional metallic alloys using spherical tips. In contrast with the common dislocation theory for the hardness measurement, the nature of NiTi SMAs' hardness is explained by the balance between the interface and the bulk energy of phase transformed SMAs. Contrary to the energy balance in the indentation zone using sharp tips, the interface energy was numerically shown to be less dominant than the bulk energy of the phase transition zone using spherical tips.

  11. Efficient Reformulation of Solid Phase Diffusion in Electrochemical-Mechanical Coupled Models for Lithium-Ion Batteries: Effect of Intercalation Induced Stresses

    De, S; Suthar, B; Rife, D; Sikha, G; Subramanian, VR


    Lithium-ion batteries are typically modeled using porous electrode theory coupled with various transport and reaction mechanisms with an appropriate discretization or approximation for the solid phase diffusion within the electrode particle. One of the major difficulties in simulating Li-ion battery models is the need for simulating solid-phase diffusion in the second radial dimension r within the particle. It increases the complexity of the model as well as the computation time/cost to a great extent. This is Particularly true for the inclusion of pressure induced diffusion inside particles experiencing volume change. A computationally efficient representation for solid-phase diffusion is discussed in this paper. The operating condition has a significant effect on the validity, accuracy, and efficiency of various approximations for the solid-phase transport governed by pressure induced diffusion. This paper introduces efficient methods for solid phase reformulation - (1) parabolic profile approach and (2) a mixed order finite difference method for approximating/representing solid-phase concentration variations within the active materials of porous electrodes for macroscopic models for lithium-ion batteries. (C) 2013 The Electrochemical Society. All rights reserved.

  12. Determination of Roxarsone in feeds using solid phase extraction and liquid chromatography with ultraviolet detection.

    Sapp, R E; Davidson, S


    A method is presented for detection and quantitation of Roxarsone in poultry feed by liquid chromatography. The drug is extracted by phosphate buffer and determined by solid phase extraction and reversed-phase liquid chromatography. Recoveries of the sample spikes and fortified field samples agree closely with those obtained by the standard spectrophotometric method.


    TANG Xuelin; QIAN Zhongdong; WU Yulin


    The dense solid-phase governing equations for two-phase flows are obtained by using the kinetic theory of gas molecules. Assuming that the solid-phase velocity distributions obey the Maxwell equations, the collision term for particles under dense two-phase flow conditions is also derived.In comparison with the governing equations of a dilute two-phase flow, the solid-particle's governing equations are developed for a dense turbulent solid-liquid flow by adopting some relevant terms from the dilute two-phase governing equations. Based on Cauchy-Helmholtz theorem and Smagorinsky model,a second-order dynamic sub-grid-scale (SGS) model, in which the sub-grid-scale stress is a function of both the strain-rate tensor and the rotation-rate tensor, is proposed to model the two-phase governing equations by applying dimension analyses. Applying the SIMPLEC algorithm and staggering grid system to the two-phase discretized governing equations and employing the slip boundary conditions on the walls, the velocity and pressure fields, and the volumetric concentration are calculated. The simulation results are in a fairly good agreement with experimental data in two operating cases in a conduit with a rectangular cross-section and these comparisons imply that these models are practical.

  14. Structure and dynamics of 1-butyl-3-methylimidazolium hexafluorophosphate phases on silica and laponite clay: from liquid to solid behavior.

    Castillo, M Rosa; Fraile, José M; Mayoral, José A


    Solid-state NMR experiments show that the behavior of supported 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid phases depends on the type of support and the phase thickness. A mobile nearly liquid phase is obtained on silica, on the basis of the line widths of the bands in (1)H, (31)P, and (13)C spectra. However, the mobility is somehow restricted, as shown by the possibility of using the cross-polarization technique, although with slow dynamics. On laponite clay, a layered material with a negatively charged surface, a truly solid phase is obtained at low coverage, whereas the increase in ionic liquid loading leads to a second liquid phase, as shown by the presence of two contributions with very different line widths. These two phases seem to coexist without exchange in the NMR time frame. Heteronuclear correlation experiments evidence different relative dispositions of the imidazolium-surface-PF(6) system, with only aromatic protons involved in all the interactions on silica but participation of the benzylic groups (N-CH(3) and/or N-CH(2)) in the case of laponite clay.

  15. Unconventional phase field simulations of transforming materials with evolving microstructures

    Jiang-Yu Li; Chi-Hou Lei; Liang-Jun Li; Yi-Chung Shu; Yun-Ya Liu


    Transforming materials with evolving microstructures is one of the most important classes of smart materials that have many potential technological applications,and an unconventional phase field approach based on the characteristic functions of transforming variants has been developed to simulate the formation and evolution of their microstructures.This approach is advantageous in its explicit material symmetry and energy well structure,minimal number of material coefficients,and easiness in coupling multiple physical processes and order parameters,and has been applied successfully to study the microstructures and macroscopic properties of shape memory alloys,ferroelectrics,ferromagnetic shape memory alloys,and multiferroic magnetoelectric crystals and films with increased complexity.In this topical review,the formulation of this unconventional phase field approach will be introduced in details,and its applications to various transforming materials will be discussed.Some examples of specific microstructures will also be presented.

  16. Jet engine with electromagnetic field excitation of expendable solid-state material

    Tsybin, O. Yu.; Makarov, S. B.; Ostapenko, O. N.


    Electromagnetic field action on a solid-state natural raw material is considered here in the context of producing a mechanical reactive momentum. We suggest the development of a jet engine that possesses fast control and low thrust based on desorption or sputtering of particles flow from a solid surface.

  17. Evaluation of single-walled carbon nanohorns as sorbent in dispersive micro solid-phase extraction

    Jimenez-Soto, Juan Manuel; Cardenas, Soledad [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain); Valcarcel, Miguel, E-mail: [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain)


    Highlights: Black-Right-Pointing-Pointer The potential of single walled carbon nanohorns in dispersive solid phase microextraction has been evaluated. Black-Right-Pointing-Pointer The method was characterized for the extraction of PAHs from waters. Black-Right-Pointing-Pointer Single walled carbon nanohorns were better extractant than carbon nanotubes and carbon nanocones. Black-Right-Pointing-Pointer The limits of detection were adequate for the target analytes in environmental waters. - Abstract: A new dispersive micro solid-phase extraction method which uses single-walled carbon nanohorns (SWNHs) as sorbent is proposed. The procedure combines the excellent sorbent properties of the nanoparticles with the efficiency of the dispersion of the material in the sample matrix. Under these conditions, the interaction with the analytes is maximized. The determination of polycyclic aromatic hydrocarbons was selected as model analytical problem. Two dispersion strategies were evaluated, being the functionalization via microwave irradiation better than the use of a surfactant. The extraction was accomplished by adding 1 mL of oxidized SWHNs (o-SWNHs) dispersion to 10 mL of water sample. After extraction, the mixture was passed through a disposable Nylon filter were the nanoparticles enriched with the PAHs were retained. The elution was carried out with 100 {mu}L of hexane. The limits of detection achieved were between 30 and 60 ng L{sup -1} with a precision (as repeatability) better than 12.5%. The recoveries obtained for the analytes in three different water samples were acceptable in all instances. The performance of o-SWNHs was favourably compared with that provided by carboxylated single-walled carbon nanotubes and thermally treated carbon nanocones.

  18. Density-functional theory of a lattice-gas model with vapour, liquid, and solid phases

    Prestipino, S.; Giaquinta, P. V.


    We use the classical version of the density-functional theory in the weighted-density approximation to build up the entire phase diagram and the interface structure of a two-dimensional lattice-gas model which is known, from previous studies, to possess three stable phases -- solid, liquid, and vapour. Following the common practice, the attractive part of the potential is treated in a mean-field-like fashion, although with different prescriptions for the solid and the fluid phases. It turns o...

  19. 76 FR 53897 - EPA Seeking Input Materials Measurement; Municipal Solid Waste (MSW), Recycling, and Source...


    ... From the Federal Register Online via the Government Publishing Office ENVIRONMENTAL PROTECTION AGENCY EPA Seeking Input Materials Measurement; Municipal Solid Waste (MSW), Recycling, and Source... management, recycling, measurement, data, data collection, construction and demolition (C&D)...


    V. A. Okovity


    Full Text Available The paper presents an oxide ceramic material with addition of solid lubricant which has good technological characteristics and which is able to form high wear-resistant plasma coatings with low friction coefficient.

  1. Thermodynamics and Kinetics of Phase Transformations in Hydrogen Storage Materials

    Ceder, Gerbrand; Marzari, Nicola


    The aim of this project is to develop and apply computational materials science tools to determine and predict critical properties of hydrogen storage materials. By better understanding the absorption/desorption mechanisms and characterizing their physical properties it is possible to explore and evaluate new directions for hydrogen storage materials. Particular emphasis is on the determination of the structure and thermodynamics of hydrogen storage materials, the investigation of microscopic mechanisms of hydrogen uptake and release in various materials and the role of catalysts in this process. As a team we have decided to focus on a single material, NaAlH{sub 4}, in order to fully be able to study the many aspects of hydrogen storage. We have focused on phase stability, mass transport and size-dependent reaction mechanisms in this material.

  2. Solid-phase microextraction for bioconcentration studies according to OECD TG 305

    Duering, Rolf-Alexander; Boehm, Leonard [Land Use and Nutrition (IFZ) Justus Liebig University Giessen, Institute of Soil Science and Soil Conservation, Research Centre for BioSystems, Giessen (Germany); Schlechtriem, Christian [Fraunhofer Institute for Molecular Biology and Applied Ecology (IME), Schmallenberg (Germany)


    An important aim of the European Community Regulation on chemicals and their safe use is the identification of (very) persistent, (very) bioaccumulative, and toxic substances. In other regulatory chemical safety assessments (pharmaceuticals, biocides, pesticides), the identification of such (very) persistent, (very) bioaccumulative, and toxic substances is of increasing importance. Solid-phase microextraction is especially capable of extracting total water concentrations as well as the freely dissolved fraction of analytes in the water phase, which is available for bioconcentration in fish. However, although already well established in environmental analyses to determine and quantify analytes mainly in aqueous matrices, solid-phase microextraction is still a rather unusual method in regulatory ecotoxicological research. Here, the potential benefits and drawbacks of solid-phase microextraction are discussed as an analytical routine approach for aquatic bioconcentration studies according to OECD TG 305, with a special focus on the testing of hydrophobic organic compounds characterized by log K{sub OW}> 5. (orig.)

  3. Thermal energy storage using phase change materials fundamentals and applications

    Fleischer, Amy S


    This book presents a comprehensive introduction to the use of solid‐liquid phase change materials to store significant amounts of energy in the latent heat of fusion. The proper selection of materials for different applications is covered in detail, as is the use of high conductivity additives to enhance thermal diffusivity. Dr. Fleischer explores how applications of PCMS have expanded over the past 10 years to include the development of high efficiency building materials to reduce heating and cooling needs, smart material design for clothing, portable electronic systems thermal management, solar thermal power plant design and many others. Additional future research directions and challenges are also discussed.

  4. Detecting Lesch-Nyhan syndrome by solid phase primer extension

    Shumaker, J.M.; Caskey, C.T. [Baylor College of Medicine, Houston, TX (United States); Metspalu, A.


    A mutation detection method based upon the wild type human HPRT sequence is presented for identification of Lesch Nyhan syndrome. The technique consists of performing a biotinlyated PCR amplification of the region of interest, followed by isolation and purification of single stranded template using magnetic separation. Allele-specific primers are annealed adjacent to the potential mutation site on the template. A terminal fluorescent deoxynucleotide addition is performed with a DNA template-dependent polymerase to distinguish between the mutant and wild-type sequence. The products are purified from unincorporated ddNTPs, eluted and finally analyzed on an ABI 373 to identify the mutation. The length of an extension primer is used as a position signature for mutations. The fidelity of nucleotide incorporation provides an excellent signal-to-noise ratio for the detection of nine HPRT mutations within eight cell lines. This method should detect all types of mutations except for repeated sequences that are longer than the primers. Moreover, the method is being extended to a solid support assay, whereby the extension primers are attached to a two-dimensional glass surface. Following extension, the solid support is analyzed for radioactive incorporation. We have shown the sequence determination of a five base region of a wild-type sequence and two different HPRT mutations. As more dense oligonucleotide arrays are produced, this method could be extended to sequence the complete coding region of HPRT.

  5. Pentaerythrityltetramine scaffolds for solid-phase combinatorial chemistry.

    Virta, Pasi; Leppänen, Marika; Lönnberg, Harri


    Straightforward synthesis for two pentaerythrityltetramine precursors, 2,2-bis(azidomethyl)propane-1,3-diamine (1) and 2-[N-(allyloxycarbonyl)aminomethyl]-2-azidomethylpropane-1,3-diamine (2), has been described. Both propane-1,3-diamines have been attached by reductive amination to a solid-supported backbone amide linker derived from 4-(4-formyl-3,5-dimethoxyphenoxy)butyric acid. The presence of the two methoxy substituents on the linker is essential to avoid cross-linking between two linkers. The remaining free primary amino group of the propane-1,3-diamine moiety may then be selectively acylated with an appropriately protected amino acid using conventional N,N-dicyclohexylcarbodiimide/1-hydroxybenzotriazole (DCC/HOBt) activation without any interference by the secondary amino function. The latter group may be subsequently acylated by an anhydride method. Sequential reduction of the azido group and removal of the allyloxycarbonyl protection from 2 allow further coupling of two different amino acids, and hence, this handle may be utilized in construction of branched structures containing four different amino acids or peptides. Solid-supported 1 may, in turn, be used for the synthesis of similar constructs containing two identical branches. It is worth noting that no acid-labile protecting groups are required in this approach, and hence, this dimension may be saved for the cleavage of the linker. The applicability of the scaffolds to library synthesis has been demonstrated by preparation of 11 pentaerythrityl-branched tetra- and octapeptides.

  6. Structure and electronic properties and phase stabilities of the Cd(1-x)Zn(x)S solid solution in the range of 0≤x≤1.

    Lu, Jibao; Dai, Ying; Guo, Meng; Wei, Wei; Ma, Yandong; Han, Shenghao; Huang, Baibiao


    As an excellent bandgap-engineering material, the Cd(1-x)Zn(x)S solid solution, is found to be an efficient visible light response photocatalyst for water splitting, but few theoretical studies have been performed on it. A better characterization of the composition dependence of the physical and optical properties of this material and a thorough understanding of the bandgap-variation mechanism are necessary to optimize the design of high-efficience photocatalysts. In order to get an insight into these problems, we systematically investigated the crystal structure, the phase stability, and the electronic structures of the Cd(1-x)Zn(x)S solid solution by means of density functional theory calculations. The most energetically favorable arrangement of the Cd, Zn, S atoms and the structural disorder of the solid solution are revealed. The phase diagram of the Cd(1-x)Zn(x)S solid solution is calculated based on regular-solution model and compared with the experimental data. This is the first report on the calculated phase diagram of this solid solution, and can give guidance for the experimental synthesis of this material. Furthermore, the variation of the electronic structures versus x and its mechanism are elaborated in detail, and the experimental bandgap as a function of x is well predicted. Our findings provide important insights into the experimentally observed structural and electronic properties, and can give theoretical guidelines for the further design of the Cd(1-x)Zn(x)S solid solution.

  7. Stability of phases in (Ba, Gd)MnO3 solid solution system

    Migaku Kobayashi; Hidenori Tamura; Hiromi Nakano; Hirohisa Satoh; Naoki Kamegashira


    The existing phases in BaxGd1-xMnO3 solid solution system (0≦x≦1) were studied by analyzing the detailed crystal structure of each composition from the results of the Rietveld method using powder X-ray diffraction data. For a small substitution of Ba for Gd (0≦x<0.1), the orthorhombic phase with a perovskite type structure (Pnma space group) was stably formed and this fact was supported by the electron diffraction data. There existed an intermediate phase of Ba0.33Gd0.67MnO3, which was characterized as the tetragonal phase with perovskite structure. The composition range of this phase was narrow and almost line compound. Between the regions of these phases, there existed two-phase region. There was also a two-phase region between the intermediate tetragonal phase and BaMnO3. Measurement of electrical conductivities of these orthorhombic solid solutions and tetragonal phases showed semiconducting behaviors for both phases and the existence of the phase transition at high temperature for the orthorhombic phase. The transition temperature decreased as the Ba content increased.

  8. Crystalline-to-plastic phase transitions in molecularly thin n-dotriacontane films adsorbed on solid surfaces

    Cisternas, Edgardo; Corrales, T. P.; del Campo, V.;


    Crystalline-to-rotator phase transitions have been widely studied in bulk hydrocarbons, in particular in normal alkanes. But few studies of these transitions deal with molecularly thin films of pure n-alkanes on solid substrates. In this work, we were able to grow dotriacontane (n-C32H66) films...... identify with a solid-solid phase transition. At higher coverages, we observed additional steps in the ellipsometric signal that we identify with a solid-solid phase transition in multilayer islands (similar to 333 K) and with the transition to the rotator phase in bulk crystallites (similar to 337 K...

  9. Rapidly Activated Dynamic Phase Transitions in Nonlinear Solids


    I Form Approv# edAD -A263 601 AiENTA11ON PAGE- f____________18 1. AGENCY USE ONLY (Lea"e blaWk 12. REPORT DATE 13. REPORT TYPE AND OATES COVEREO Feb...phase transforming media during high energy impact. Conversion of mechanical energy to thermal ener- gy has been studied by means of an extended theory...and Phase Structures in General Media , R. Fosdick, E. Dunn & M. Slemrod eds., IMA volume series, Springer- Verlag. Song, J. and T. L. Pence (1992

  10. Two-phase anaerobic digestion of vegetable market waste fraction of municipal solid waste and development of improved technology for phase separation in two-phase reactor.

    Majhi, Bijoy Kumar; Jash, Tushar


    Biogas production from vegetable market waste (VMW) fraction of municipal solid waste (MSW) by two-phase anaerobic digestion system should be preferred over the single-stage reactors. This is because VMW undergoes rapid acidification leading to accumulation of volatile fatty acids and consequent low pH resulting in frequent failure of digesters. The weakest part in the two-phase anaerobic reactors was the techniques applied for solid-liquid phase separation of digestate in the first reactor where solubilization, hydrolysis and acidogenesis of solid organic waste occur. In this study, a two-phase reactor which consisted of a solid-phase reactor and a methane reactor was designed, built and operated with VMW fraction of Indian MSW. A robust type filter, which is unique in its implementation method, was developed and incorporated in the solid-phase reactor to separate the process liquid produced in the first reactor. Experiments were carried out to assess the long term performance of the two-phase reactor with respect to biogas production, volatile solids reduction, pH and number of occurrence of clogging in the filtering system or choking in the process liquid transfer line. The system performed well and was operated successfully without the occurrence of clogging or any other disruptions throughout. Biogas production of 0.86-0.889m(3)kg(-1)VS, at OLR of 1.11-1.585kgm(-3)d(-1), were obtained from vegetable market waste, which were higher than the results reported for similar substrates digested in two-phase reactors. The VS reduction was 82-86%. The two-phase anaerobic digestion system was demonstrated to be stable and suitable for the treatment of VMW fraction of MSW for energy generation.

  11. Ultrathin two-dimensional inorganic materials: new opportunities for solid state nanochemistry.

    Sun, Yongfu; Gao, Shan; Lei, Fengcai; Xiao, Chong; Xie, Yi


    CONSPECTUS: The ultimate goal of solid state chemistry is to gain a clear correlation between atomic, defect, and electronic structure and intrinsic properties of solid state materials. Solid materials can generally be classified as amorphous, quasicrystalline, and crystalline based on their atomic arrangement, in which crystalline materials can be further divided into single crystals, microcrystals, and nanocrystals. Conventional solid state chemistry mainly focuses on studying single crystals and microcrystals, while recently nanocrystals have become a hot research topic in the field of solid state chemistry. As more and more nanocrystalline materials have been artificially fabricated, the solid state chemistry for studying those nanosolids has become a new subdiscipline: solid state nanochemistry. However, solid state nanochemistry, usually called "nanochemistry" for short, primarily studies the microstructures and macroscopic properties of a nanomaterial's aggregation states. Due to abundant microstructures in the aggregation states, it is only possible to build a simple but imprecise correlation between the microscopic morphology and the macroscopic properties of the nanostructures. Notably, atomically thin two-dimensional inorganic materials provide an ideal platform to establish clear structure-property relationships in the field of solid state nanochemistry, thanks to their homogeneous dispersion without the assistance of a capping ligand. In addition, their atomic structures including coordination number, bond length, and disorder degree of the examined atoms can be clearly disclosed by X-ray absorption fine structure spectroscopy. Also, their more exposed interior atoms would inevitably induce the formation of various defects, which would have a non-negligible effect on their physicochemical properties. Based on the obtained atomic and defect structural characteristics, density-functional calculations are performed to study their electronic structures

  12. Multilayer Pressure Vessel Materials Testing and Analysis. Phase 1

    Cardinal, Joseph W.; Popelar, Carl F.; Page, Richard A.


    To provide NASA a comprehensive suite of materials strength, fracture toughness and crack growth rate test results for use in remaining life calculations for aging multilayer pressure vessels, Southwest Research Institute (R) (SwRI) was contracted in two phases to obtain relevant material property data from a representative vessel. This report describes Phase 1 of this effort which includes a preliminary material property assessment as well as a fractographic, fracture mechanics and fatigue crack growth analyses of an induced flaw in the outer shell of a representative multilayer vessel that was subjected to cyclic pressure test. SwRI performed this Phase 1 effort under contract to the Digital Wave Corporation in support of their contract to Jacobs ATOM for the NASA Ames Research Center.

  13. Counterposition and negative phase velocity in uniformly moving dissipative materials

    Mackay, Tom G [School of Mathematics and Maxwell Institute for Mathematical Sciences, University of Edinburgh, Edinburgh EH9 3JZ (United Kingdom); Lakhtakia, Akhlesh [NanoMM-Nanoengineered Metamaterials Group, Department of Engineering Science and Mechanics, Pennsylvania State University, University Park, PA 16802-6812 (United States)], E-mail:, E-mail:


    We considered the phenomena of counterposition and negative phase velocity, which are relevant to certain metamaterials and certain astrophysical scenarios. The Lorentz transformations of electric and magnetic fields were implemented to study (i) the refraction of linearly polarized plane waves into a half-space occupied by a uniformly moving material and (ii) the traversal of linearly polarized Gaussian beams through a uniformly moving slab. Motion was taken to occur tangentially to the interface(s) and in the plane of incidence. The moving materials were assumed to be isotropic, homogeneous and dissipative dielectric materials from the perspective of a co-moving observer. Two different moving materials were considered: from the perspective of a co-moving observer, material A supports planewave propagation with only positive phase velocity, whereas material B supports planewave propagation with both positive and negative phase velocity, depending on the polarization state. For both materials A and B, the sense of the phase velocity and whether or not counterposition occurred, as perceived by a non-co-moving observer, could be altered by varying the observer's velocity. Furthermore, the lateral position of a beam upon propagating through a uniformly moving slab made of material A, as perceived by a non-co-moving observer, could be controlled by varying the observer's velocity. In particular, at certain velocities, the transmitted beam emerged from the slab laterally displaced in the direction opposite to the direction of incident beam. The transmittances of a uniformly moving slab made of material B were very small and the energy density of the transmitted beam was largely concentrated in the direction normal to the slab, regardless of the observer's velocity.

  14. Positronium in solid phases of n-alkane binary mixtures

    Zgardzińska, B.; Goworek, T.


    Highlights: • Rotator phase in even alkanes C{sub n}H{sub 2n+2} with n ⩽ 20 appears in mixed samples only. • Interlamellar gap width is the same for shorter chain alkane concentration x and 1 − x. • Excess electron trapping diminishes with broadening of alkane chain distribution Δn. - Abstract: Binary mixtures of even-numbered normal alkanes C{sub n}H{sub 2n+2} and C{sub n+2}H{sub 2n+6} with n ⩽ 18 were investigated by positron annihilation spectroscopy. Formation of the rotator phase was observed in mixed structures, while no such a phase in neat alkanes in this range of n was found. Phase diagrams for n = 18 and n = 16 are very similar to the diagrams for binary mixtures of odd-numbered alkanes. The effect of positronium formation with trapped excess electrons weakens with decreasing n, at low n values the time constant of Ps rise contains the component much shorter than 1 h.

  15. All rights reserved Development of Headspace Solid-Phase ...


    Pesticide Residues in Fruit and Vegetable Samples using OFAT Design. *. 1,2. LUKMAN BOLA ... phase microextraction parameters (fiber coating type, extraction temperature and time, pH, salt addition ... production of food (Bakırcı, et al. 2014 ...

  16. SANS study of phase separation in solid {sup 3}He-{sup 4}He

    Koster, J.P.; Nagler, S.E.; Adams, E.D. [Florida Univ., Gainesville, FL (United States). Dept. of Physics; Wignall, G.D. [Oak Ridge National Lab., TN (United States). Solid State Div.


    Small angle neutron scattering has been used to study phase separation in a quantum alloy, solid {sup 3}He{sub x}-{sup 4}He{sub 1{minus}x}. The onset of phase separation is marked by a dramatic increase in the measured scattering. A simple interpretation of the results suggests that the late-stage phase separation kinetics are dominated by an increase in the concentration of {sup 3}He atoms in preexisting precipitate regions.

  17. A new method to study complex materials in solid state chemistry: application to chalcogenide materials

    Lippens, P. E.; Olivier-Fourcade, J.; Jumas, J. C.


    We show that a combined application of Mössbauer spectroscopy and other experimental tools such as X-ray photoelectron spectroscopy, X-ray absorption spectroscopy and nuclear magnetic resonance provides a coherent picture of the local electronic structure in chalcogenide materials. In order to develop this idea we propose an analysis of the Sn, Sb and Te local electronic structures for three different systems of materials. The first example concerns the In Sn S system. We show that Li insertion in In16Sn4S32 leads to changes of the Sn oxidation states from Sn(IV) to Sn(II). The second example concerns materials of the Tl Sb S system. We show that variations of the 121Sb Mössbauer isomer shift and surface of the first peak of the X-ray absorption spectra at the Sb LIII edge can be linearly correlated because of the main influence of the Sb 5s electrons. This is explained by changes in the local environment of the Sb atoms. The last example concerns the crystalline phases of the Tl Sn Te system. The formal oxidation numbers of the Te atoms are determined from 125Te Mössbauer spectroscopy and X-ray photoelectron spectroscopy. They are related to the different types of bonds involving the Te atoms in the Tl Sn Te compounds.

  18. Thermal Performance of Microencapsulated Phase Change Material Survey


    ER D C TR -0 8 -4 Basic Research/Military Construction Thermal Performance of Microencapsulated Phase Change Material Slurry Jorge L...distribution is unlimited. Basic Research/Military Construction ERDC TR-08-4 March 2008 Thermal Performance of Microencapsulated Phase Change... microencapsulated PCM (MPCM) slurries is enhanced significantly, even when using low volume fractions. MPCM slurries have potential to decrease costs and improve

  19. Thermal Performance of Microencapsulated Phase Change Material Slurry


    ER D C TR -0 8 -4 Basic Research/Military Construction Thermal Performance of Microencapsulated Phase Change Material Slurry Jorge L...distribution is unlimited. Basic Research/Military Construction ERDC TR-08-4 March 2008 Thermal Performance of Microencapsulated Phase Change... microencapsulated PCM (MPCM) slurries is enhanced significantly, even when using low volume fractions. MPCM slurries have potential to decrease costs and improve

  20. Cu Binding to Iron Oxide-Organic Matter Coprecipitates in Solid and Dissolved Phases

    Vadas, T. M.; Koenigsmark, F.


    Recent studies indicate that Cu is released from wetlands following storm events. Assymetrical field flow field fractionation (AF4) analyses as well as total and dissolved metal concentration measurements suggest iron oxide-organic matter complexes control Cu retention and release. Coprecipitation products of Fe oxide and organic matter were prepared under conditions similar to the wetland to assess Cu partitioning to and availability from solid phases that settle from solution as well as phases remaining suspended. Cu coprecipitation and sorption to organomineral precipitation solids formed at different Fe:organic carbon (OC) ratios were compared for net Cu removal and extractability. As more humic acid was present during precipitation of Fe, TEM images indicated smaller Fe oxide particles formed within an organic matrix as expected. In coprecipitation reactions, as the ratio of Fe:OC decreased, more Cu was removed from solution at pH 5.5 and below. However, in sorption reactions, there was an inhibition of Cu removal at low OC concentrations. As the pH increased from 5.5 to 7 and as solution phase OC concentration increased, more Cu remained dissolved in both coprecipitation and sorption reactions. The addition of Ca2+, glycine, histidine and citric acid or lowering the pH resulted in more extractable Cu from the coprecipitation compared with the sorption reactions. The variations in Cu extraction were likely due to a combination of a more amorphous structure in CPT products, and the relative abundance of available Fe oxide or OC binding sites. Suspended Fe oxide-organic matter coprecipitates were assessed using AF4 coupled to online TOC analysis and ICP-MS. In laboratory prepared samples, Cu was observed in a mixture of small 1-5 nm colloids of Fe oxide-organic matter precipitates, but the majority was observed in larger organic matter colloids and were not UV absorbing, suggesting more aliphatic carbon materials. In field samples, up to 60% of the dissolved Cu