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Sample records for sensitive solid phase

  1. Solid phase assays

    International Nuclear Information System (INIS)

    Reese, M.G.; Johnson, L.R.; Ransom, D.K.

    1980-01-01

    In a solid phase assay for quantitative determination of biological and other analytes, a sample such as serum is contacted with a receptor for the analyte being assayed, the receptor being supported on a solid support. No tracer for the analyte is added to the sample before contacting with the receptor; instead the tracer is contacted with the receptor after unbound analyte has been removed from the receptor. The assay can be otherwise performed in a conventional manner but can give greater sensitivity. (author)

  2. Ion-selective solid-phase electrode sensitive to ammonium ions

    International Nuclear Information System (INIS)

    Vlasov, Yu.G.; Milonova, M.S.; Antonov, P.P.; Bychkov, E.A.; Ehfa, A.Ya.

    1983-01-01

    Ammonium phosphomolybdate is investigated for the purpose of using it as membrane material of ammonium-selective solid-phase electrodes. Estimation of proton mobility and ion conductivity of ammonium phosphomolybdate is performed

  3. Solid phase radioimmunoassays

    International Nuclear Information System (INIS)

    Wide, L.

    1977-01-01

    Solid phase coupled antibodies were introduced to facilitate the separation of bound and free labelled ligand in the competitive inhibition radioimmunoassay. Originally, the solid matrix used was in the form of small particles and since then a number of different matrices have been used such as very fine powder particles, gels, paper and plastic discs, magnetic particles and the inside surface of plastic tubes. The coupling of antibodies may be that of a covalent chemical binding, a strong physical adsorbtion, or an immunological binding to a solid phase coupled antigen. New principles of radioimmunoassay such as the solid phase sandwich techniques and the immunoradiometric assay were developped from the use of solid phase coupled antigens and antibodies. The solid phase sandwich techniques are reagent excess methods with a very wide applicability. Several of the different variants of solid phase techniques are suitable for automation. Advantages and disadvantages of solid phase radioimmunoassays when compared with those using soluble reagents are discussed. (orig.) [de

  4. Solid phase radioimmunoassays for human C-reactive protein

    International Nuclear Information System (INIS)

    Shine, B.; Beer, F.C. de; Pepys, M.B.

    1981-01-01

    Two new, rapid and sensitive radioimmunoassays for human C-reactive protein (CRP) have been established using antiserum coupled to magnetizable cellulose particles, which facilitate phase separation. A single antibody method, using solid phase anti-CRP, provides a sensitivity of 50 μg/l with a 1-h incubation time and intra- and inter-assay coefficients of variation of 10%. A double antibody method, using fluid phase rabbit anti-CRP serum and solid phase sheep anti-rabbit IgG serum, provides a sensitivity of 3 μg/l with an overnight incubation and intra- and inter-assay coefficients of variation of 10%. Among 468 sera from normal adult volunteer blood donors the median CRP concentration was 800 μg/l, interquartile range 340-1700 μg/l and range 70-29,000 μg/l. Ninety percent of samples contained less than 3 mg/l and 99% less than 10 mg/l. Low levels (14-650 μg/l) of CRP were detected both in amniotic fluids and in cerebrospinal fluids. (Auth.)

  5. Liquid-phase and solid-phase radioimmunoassay with herpes simplex virus type 1 nucleocapsids

    International Nuclear Information System (INIS)

    Bystricka, M.; Rajcani, J.; Libikova, H.; Sabo, A.; Foeldes, O.; Sadlon, J.

    1985-01-01

    Liquid-phase radioimmunoassay and solid-phase radioimmunoassay are described using 125 I-labelled or immobilized nucleocapsids (NC) of herpes simplex virus (HSV) type1. These techniques appeared sensitive and specific for quantitation of HSV-NC antigens and corresponding antibodies. (author)

  6. Evaluation of a solid-phase RIA technique and a solid-phase ELISA technique for demonstrating hepatitis-B surface antigen

    International Nuclear Information System (INIS)

    Vranckx, R.; Cole, J.; Peetermans, M.

    1978-01-01

    The sensitivities of a solid-phase radioimmunoassay (RIA), a solid-phase enzyme immunoassay (ELISA) and a haemagglutination test (RPHA) for the detection of the hepatitis-B surface antigen (HBsAg) were compared (1) by screening a panel of 300 sera (97 positives and 203 negatives), and (2) by titrating serial dilutions of 10 positive sera. Ninety-seven sera were positive by RIA, 95% were detected by ELISA and 81% were detected by RPHA. In the serial dilutions, the average end-points of the titrations were 0.005ng/ml for RIA, 0.01ng/ml for ELISA and 0.04 ng/ml for RPHA. It can be concluded that the sensitivity of the ELISA test is intermediate between that of the RIA and the RPHA. The ELISA and the RPHA tests seem to be a little more sensitive for the detection of subtype ay than for the detection of subtype ad. (author)

  7. Solid phase radioimmunoassay for HBe Ag and anti-HBe

    Energy Technology Data Exchange (ETDEWEB)

    Froesner, G G; Deinhardt, F [Muenchen Univ. (Germany, F.R.). Inst. fuer Hygiene und Medizinische Mikrobiologie; Sugg, U [Tuebingen Univ. (Germany, F.R.). Abt. fuer Transfusionswesen mit Blutbank; Haas, H [Staedtische Krankenanstalten Esslingen (Germany, F.R.). Zentrallabor; Overby, R L [Abbott Labs., North Chicago, IL (USA)

    1978-04-01

    A highly sensitive solid phase radioimmunoassay for the detection of hepatitis Be-antigen (HBeAg) and anti-HBe is described. Iodine-125 labelled anti-HBe is used as a tracer. The assay is about 500 foLd more sensitive than immunodiffusion.

  8. Temperature sensitive molecularly imprinted microspheres for solid-phase dispersion extraction of malachite green, crystal violet and their leuko metabolites

    International Nuclear Information System (INIS)

    Tan, Lei; Chen, Kuncai; He, Rong; Peng, Rongfei; Huang, Cong

    2016-01-01

    This article demonstrates the feasibility of an alternative strategy for producing temperature sensitive molecularly imprinted microspheres (MIMs) for solid-phase dispersion extraction of malachite green, crystal violet and their leuko metabolites. Thermo-sensitive MIMs can change their structure following temperature stimulation. This allows capture and release of target molecules to be controlled by temperature. The fabrication technique provides surface molecular imprinting in acetonitrile using vinyl modified silica microspheres as solid supports, methacrylic acid and N-isopropyl acrylamide as the functional monomers, ethyleneglycol dimethacrylate as the cross-linker, and malachite green as the template. After elution of the template, the MIMs can be used for fairly group-selective solid phase dispersion extraction of malachite green, crystal violet, leucomalachite green, and leucocrystal violet from homogenized fish samples at a certain temperature. Following centrifugal separation of the microspheres, the analytes were eluted with a 95:5 mixture of acetonitrile and formic acid, and then quantified by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) with isotope internal calibration. The detection limits for malachite green, crystal violet and their metabolites typically are 30 ng·kg −1 . Positive samples were identified by UHPLC-MS/MS in the positive ionization mode with multiple reaction monitoring. The method was applied to the determination of the dyes and the respective leuko dyes in fish samples, and accuracy and precision were validated by comparative analysis of the samples by using aluminum neutral columns. (author)

  9. Solid state phase change materials for thermal energy storage in passive solar heated buildings

    Science.gov (United States)

    Benson, D. K.; Christensen, C.

    1983-11-01

    A set of solid state phase change materials was evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol, pentaglycerine and neopentyl glycol. Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature within the range from less than 25 deg to 188 deg. Thermophysical properties such as thermal conductivity, density and volumetric expansion were measured. Computer simulations were used to predict the performance of various Trombe wall designs incorporating solid state phase change materials. Optimum performance was found to be sensitive to the choice of phase change temperatures and to the thermal conductivity of the phase change material. A molecular mechanism of the solid state phase transition is proposed and supported by infrared spectroscopic evidence.

  10. Solid-phase reductive amination for glycomic analysis.

    Science.gov (United States)

    Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

    2017-04-15

    Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

  11. Micro solid-phase radioimmunoassay for detection of herpesvirus type-specific antibody: specificity and sensitivity

    Energy Technology Data Exchange (ETDEWEB)

    Adler-Storthz, K.; Matson, D.O.; Adam, E.; Dreesman, G.R. (Baylor Univ., Houston, TX (USA). Coll. of Medicine)

    1983-02-01

    The specificity and sensitivity of a micro solid-phase radioimmunoassay (micro-SPRIA) that detects type-specific IgG antibody to herpes simplex virus types 1 and 2 (HSV1 and HSV2) were evaluated. Glycoproteins VP123 (molecular weight, 123,000) of HSV1 and VP119 (molecular weight, 119,000) of HSV2 were found to display the greatest degree of antigenic type-specificity of several HSV antigens tested with the micro-SPRIA technique. When testing a group of sera, negative for anti-HSV antibodies by microneutralization, in the micro-SPRIA, a range of negative reactivities was noted, suggesting that cut-points should be determined for each antigen preparation. The micro-SPRIA detected appropriate antibody activity in patients with recurrent infection and a marked agreement was noted in comparison to detection of anti-HSV antibodies measured with the microneutralization test. The type-specificity of the micro-SPRIA was substantiated by the independence of test results using VP119 and VP123 antigens for a random group of positive sera. The assay is rapid, specific, and sensitive and allows the testing of multiple serum samples with a standardized set of reagents.

  12. Radioimmuoassay study of antidigitoxin antibodies in liquid phase and after coupling on a solid phase

    International Nuclear Information System (INIS)

    Collignon, A.; German, A.; Scherrmann, J.M.; Bourdon, R.

    1983-01-01

    Antidigitoxin antibodies prepared by immunizing rabbits with a digitoxin-bovine serum albumin conjugate have been studied by radioimmunoassay in the native serum (homogeneous phase antibodies) and after coupling on glass beads (heterogeneous phase antibodies). Homogeneous phase antibodies present a satisfactory titer and affinity constant and react very specifically with digitoxin. Fixation of antibodies on a solid phase induce a loss of their immunoreactivity as it is showed by modification of the inhibition curves, by a greater sensitivity to the chemical structure of the tracer and by a decrease of the affinity constant. Reactionnal kinetic and sensitivity to the incubation temperature are not modified. Heterogeneous phase antibodies present a greater stability. Both antibodies types can be used for a digitoxin radioimmunoassay [fr

  13. Double antibody solid-phase radioimmunoassay for staphylococcal enterotoxin A

    International Nuclear Information System (INIS)

    Lindroth, S.; Niskanen, A.

    1977-01-01

    A double antibody solid-phase (DASP) radioimmunoassay for staphylococcal enterotoxin A is described. In the assay the antigen-antibody complex is precipitated by anti-rabbit serum which is adsorbed onto a solid carrier (cellulose). The method is sensitive to 200 pg of enterotoxin. It was possible to detect a little as 2-5 ng of enterotoxin A/ml food extract from minced meat and sausage. Enterotoxins B and C were not found to inhibit the uptake of labled enterotoxin A at a level which might distort the results of the enterotoxin A assay. The DASP technique is sensitive, rapid, and easy to perform and thus compares favorably with other radioimmunoassays for enterotoxin. (orig.) [de

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

    DEFF Research Database (Denmark)

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

    1996-01-01

    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...... reduced compared to the conventional chemical cleavage method (CCM), and even by using a uniformly labelled probe, the exact position and nature of the mutation can be revealed. The SpCCM is suitable for automatization using a workstation to carry out the reactions and a fluorescent detection-based DNA...

  15. On the sensitivity of FPPE - TWRC method in thermal effusivity investigations of solids

    International Nuclear Information System (INIS)

    Dadarlat, Dorin; Streza, Mihaela; Pop, Mircea N; Tosa, Valer

    2009-01-01

    The front detection configuration (FPPE) together with the thermal-wave-resonator-cavity (TWRC) method was used for direct measurement of the thermal effusivity of solid materials inserted as backings in the FPPE detection cell. It was demonstrated that the normalized phase of the FPPE signal has an oscillating dependence as a function of sample's thickness. The paper presents experimental results on solid materials, with various values of thermal effusivity (Cu, brass, steel, bakelite, wood). A study of the sensitivity of the technique for different liquid/backing effusivity ratios is performed. The highest sensitivity was obtained when investigating solids with values of thermal effusivity not far from the effusivity of the liquid layer of the detection cell.

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

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, A R

    2007-06-01

    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.

  17. Solid-solid phase transitions in Fe nanowires induced by axial strain

    International Nuclear Information System (INIS)

    Sandoval, Luis; Urbassek, Herbert M

    2009-01-01

    By means of classical molecular-dynamics simulations we investigate the solid-solid phase transition from a bcc to a close-packed crystal structure in cylindrical iron nanowires, induced by axial strain. The interatomic potential employed has been shown to be capable of describing the martensite-austenite phase transition in iron. We study the stress versus strain curves for different temperatures and show that for a range of temperatures it is possible to induce a solid-solid phase transition by axial strain before the elasticity is lost; these transition temperatures are below the bulk transition temperature. The two phases have different (non-linear) elastic behavior: the bcc phase softens, while the close-packed phase stiffens with temperature. We also consider the reversibility of the transformation in the elastic regimes, and the role of the strain rate on the critical strain necessary for phase transition.

  18. Development of a solid-phase assay for measurement of proteolytic enzyme activity

    International Nuclear Information System (INIS)

    Varani, J.; Johnson, K.; Kaplan, J.

    1980-01-01

    A solid-phase, plate assay was developed for the measurement of proteolytic enzyme activity. In this assay procedure, radiolabeled substrates were dried onto the surface of microtiter wells. Following drying, the wells were washed two times with saline to remove the nonadherent substrate. When proteolytic enzymes were added to the wells, protein hydrolysis occurred, releasing radioactivity into the supernatant fluid. The amount of protein hydrolysis that occurred was reflected by the amount of radioactivity in the supernatant fluid. When 125 I-hemoglobin was used as the substrate, it was as susceptible to hydrolysis by trypsin in the solid-phase assay as it was in solution in a standard assay procedure. Protease activity from a variety of sources (including from viable cells as well as from extracellular sources) were also able to hydrolyze the hemoglobin on the plate. 125 I-Labeled serum albumen, fibrinogen, and rat pulmonary basement membrane were also susceptible to hydrolysis by trypsin in the solid phase. When [ 14 C]elastin was dried onto the plate, it behaved in a similar manner to elastin in solution. It was resistant to hydrolysis by nonspecific proteases such as trypsin and chymotrypsin but was highly susceptible to hydrolysis by elastase. The solid-phase plate assay has several features which recommended it for routine use. It is as sensitive as standard tube assays (and much more sensitive than routinely used colormetric assays). It is quick and convenient; there are no precipitation, centrifugation, or filtration steps. In addition, very small volumes of radioactive wastes are generated. Another advantage of the solid-phase plate assay is the resistance of the dried substrates to spontaneous breakdown and to microbial contamination. Finally, this assay is suitable for use with viable cells as well as for extracellular proteases

  19. Radiation sensitive solid state devices

    International Nuclear Information System (INIS)

    Shannon, J.M.; Ralph, J.E.

    1975-01-01

    A solid state radiation sensitive device is described employing JFETs as the sensitive elements. Two terminal construction is achieved by using a common conductor to capacitively couple to the JFET gate and to one of the source and drain connections. (auth)

  20. Solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Jensen, Knud Jørgen

    2013-01-01

    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....

  1. Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

    Science.gov (United States)

    Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

    2017-03-04

    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.

  2. Preparation and characterization of a novel polymeric based solid-solid phase change heat storage material

    International Nuclear Information System (INIS)

    Xi Peng; Gu Xiaohua; Cheng Bowen; Wang Yufei

    2009-01-01

    Here we reported a two-step procedure for preparing a novel polymeric based solid-solid phase change heat storage material. Firstly, a copolymer monomer containing a polyethylene glycol monomethyl ether (MPEG) phase change unit and a vinyl unit was synthesized via the modification of hydrogen group of MPEG. Secondly, by copolymerization of the copolymer monomer and phenyl ethylene, a novel polymeric based solid-solid phase change heat storage material was prepared. The composition, structure and properties of the novel polymeric based solid-solid phase change material were characterized by IR, 1 H NMR, DSC, WAXD, and POM, respectively. The results show that the novel polymeric based solid-solid phase change material possesses of excellent crystal properties and high phase change enthalpy.

  3. Mechanism and microstructures in Ga2O3 pseudomartensitic solid phase transition.

    Science.gov (United States)

    Zhu, Sheng-Cai; Guan, Shu-Hui; Liu, Zhi-Pan

    2016-07-21

    Solid-to-solid phase transition, although widely exploited in making new materials, challenges persistently our current theory for predicting its complex kinetics and rich microstructures in transition. The Ga2O3α-β phase transformation represents such a common but complex reaction with marked change in cation coordination and crystal density, which was known to yield either amorphous or crystalline products under different synthetic conditions. Here we, via recently developed stochastic surface walking (SSW) method, resolve for the first time the atomistic mechanism of Ga2O3α-β phase transformation, the pathway of which turns out to be the first reaction pathway ever determined for a new type of diffusionless solid phase transition, namely, pseudomartensitic phase transition. We demonstrate that the sensitivity of product crystallinity is caused by its multi-step, multi-type reaction pathway, which bypasses seven intermediate phases and involves all types of elementary solid phase transition steps, i.e. the shearing of O layers (martensitic type), the local diffusion of Ga atoms (reconstructive type) and the significant lattice dilation (dilation type). While the migration of Ga atoms across the close-packed O layers is the rate-determining step and yields "amorphous-like" high energy intermediates, the shearing of O layers contributes to the formation of coherent biphase junctions and the presence of a crystallographic orientation relation, (001)α//(201[combining macron])β + [120]α//[13[combining macron]2]β. Our experiment using high-resolution transmission electron microscopy further confirms the theoretical predictions on the atomic structure of biphase junction and the formation of (201[combining macron])β twin, and also discovers the late occurrence of lattice expansion in the nascent β phase that grows out from the parent α phase. By distinguishing pseudomartensitic transition from other types of mechanisms, we propose general rules to predict the

  4. Solid phase 125I labelled radioimmunoassay for spermidine

    International Nuclear Information System (INIS)

    Zhao Shimin

    1991-01-01

    Using 125 I labelled monoclonal antibody against spermidine and solid phase antigen spermidine-bovine serum albumin conjugate, the radioimmunoassay for spermidine was developed. The sensitivity of this method was about 8 times higher than that of liquid phase 14 C labelled spermidine radioimmunoassay, reaching detection limit of 10 ng/ml (0.5 ng/tube). The working range of standard curve was 0-10 5 ng/ml. The new method was suitable for spermidine measurements in saliva, stomach fluid, and cerebrospinal fluid. The coefficients of variation (CV) of within and between-assay were 4% and 13%, respectively. Preliminary clinical measurements showed that the spermidine levels in saliva of cancer patients and in cerebrospinal fluid of leukemia patients were significantly elevated

  5. Multiplexed Colorimetric Solid-Phase Extraction

    Science.gov (United States)

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

    2009-01-01

    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).

  6. Solid Phase Radioimmunoassay for Measuring Serum Prolactin Using Antibody Coupled Magnetizable Particles

    International Nuclear Information System (INIS)

    El-Bayoumy, A.S.A.

    2012-01-01

    The objective of the present work was to prepare solid phase radioimmunoassay (RIA) reagents. Development as well as optimization and validation of RIA system using solid phase magnetic particles for the measurement of prolactin (PRL) in human serum are described. The production of polyclonal antibodies was carried out by immunizing three Balb/C mice intraperitoneal through primary injection and two booster doses. Low density magnetizable cellulose iron oxide particles have been used to couple covalently to the IgG fraction of polyclonal anti-prolactin using carbonyl diimidazole activation method and applied as a solid phase separating agent for RIA of serum prolactin. Preparation of 125 I-PRL tracer was prepared using lactoperoxidase method and it was purified by gel filtration using sephadex G-100. The PRL standards were prepared using a highly purified PRL antigen with assay buffer as standard matrix. Optimization and validation of the assay were carried out. The results obtained provide a low cost, simple, sensitive, specific and accurate RIA system of prolactin based on magnetizable solid phase separation. These magnetic particles retain their characteristics during storage for 6 months at 4 degree C. In conclusion, this assay could be used as a useful diagnostic tool for pituitary dysfunction and possible reproductive disability.

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

    Science.gov (United States)

    Bharadwaj, Atul S; Singh, Yashwant

    2017-03-01

    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)=ε(σ/r)^{n}, where parameter n measures softness of the potential. We find that for 1/nfcc) structure while 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.

  8. Solid-solid phase change thermal storage application to space-suit battery pack

    Science.gov (United States)

    Son, Chang H.; Morehouse, Jeffrey H.

    1989-01-01

    High cell temperatures are seen as the primary safety problem in the Li-BCX space battery. The exothermic heat from the chemical reactions could raise the temperature of the lithium electrode above the melting temperature. Also, high temperature causes the cell efficiency to decrease. Solid-solid phase-change materials were used as a thermal storage medium to lower this battery cell temperature by utilizing their phase-change (latent heat storage) characteristics. Solid-solid phase-change materials focused on in this study are neopentyl glycol and pentaglycerine. Because of their favorable phase-change characteristics, these materials appear appropriate for space-suit battery pack use. The results of testing various materials are reported as thermophysical property values, and the space-suit battery operating temperature is discussed in terms of these property results.

  9. Ultrasensitive microfluidic solid-phase ELISA using an actuatable microwell-patterned PDMS chip.

    Science.gov (United States)

    Wang, Tanyu; Zhang, Mohan; Dreher, Dakota D; Zeng, Yong

    2013-11-07

    Quantitative detection of low abundance proteins is of significant interest for biological and clinical applications. Here we report an integrated microfluidic solid-phase ELISA platform for rapid and ultrasensitive detection of proteins with a wide dynamic range. Compared to the existing microfluidic devices that perform affinity capture and enzyme-based optical detection in a constant channel volume, the key novelty of our design is two-fold. First, our system integrates a microwell-patterned assay chamber that can be pneumatically actuated to significantly reduce the volume of chemifluorescent reaction, markedly improving the sensitivity and speed of ELISA. Second, monolithic integration of on-chip pumps and the actuatable assay chamber allow programmable fluid delivery and effective mixing for rapid and sensitive immunoassays. Ultrasensitive microfluidic ELISA was demonstrated for insulin-like growth factor 1 receptor (IGF-1R) across at least five orders of magnitude with an extremely low detection limit of 21.8 aM. The microwell-based solid-phase ELISA strategy provides an expandable platform for developing the next-generation microfluidic immunoassay systems that integrate and automate digital and analog measurements to further improve the sensitivity, dynamic ranges, and reproducibility of proteomic analysis.

  10. Application of a sepharose bead immunofluorescence assay and a solid-phase radioimmunoassay to the bovine leukemia virus system

    International Nuclear Information System (INIS)

    Fiebach, H.; Uckert, W.; Micheel, B.

    1982-01-01

    Several fluorescence assays with bovine leukemia virus (BLV) conjugated to activated Sepharose 4B were used for the detection of BLV and anti-BLV antibodies. These tests were compared with a solid-phase radioimmunoassay and found to be in the same sensitivity range. Sepharose bead immunofluorescence assay and solid-phase radioimmunoassay can be applied to the diagnosis of BLV infection in cattle. (author)

  11. Application of a sepharose bead immunofluorescence assay and a solid-phase radioimmunoassay to the bovine leukemia virus system

    Energy Technology Data Exchange (ETDEWEB)

    Fiebach, H.; Uckert, W.; Micheel, B. (Akademie der Wissenschaften der DDR, Berlin. Zentralinstitut fuer Krebsforschung)

    Several fluorescence assays with bovine leukemia virus (BLV) conjugated to activated Sepharose 4B were used for the detection of BLV and anti-BLV antibodies. These tests were compared with a solid-phase radioimmunoassay and found to be in the same sensitivity range. Sepharose bead immunofluorescence assay and solid-phase radioimmunoassay can be applied to the diagnosis of BLV infection in cattle.

  12. Sensitivity enhancement for nitrophenols using cationic surfactant-modified activated carbon for solid-phase extraction surface-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Chen, Y C; Tsai, M F

    2000-01-01

    Previous work has demonstrated that a combination of solid-phase extraction with surface-assisted laser desorption/ionization (SPE-SALDI) mass spectrometry can be applied to the determination of trace nitrophenols in water. An improved method to lower the detection limit of this hyphenated technique is described in this present study. Activated carbon powder is used as both the SPE adsorbent and the SALDI solid in the analysis by SPE-SALDI. The surface of the activated carbon is modified by passing an aqueous solution of a cationic surfactant through the SPE cartridge. The results demonstrate that the sensitivity for nitrophenols in the analysis by SPE-SALDI can be improved by using cationic surfactants to modify the surface of the activated carbon. The detection limit for nitrophenols is about 25 ppt based on a signal-to-noise ratio of 3 by sampling from 100 mL of solution. Copyright 2000 John Wiley & Sons, Ltd.

  13. Solid-phase peptide quantitation assay using labeled monoclonal antibody and glutaraldehyde fixation

    International Nuclear Information System (INIS)

    Kasprzyk, P.G.; Cuttitta, F.; Avis, I.; Nakanishi, Y.; Treston, A.; Wong, H.; Walsh, J.H.; Mulshine, J.L.

    1988-01-01

    A solid-phase radioimmunoassay utilizing iodinated peptide-specific monoclonal antibody as a detection system instead of labeled peptide has been developed. Regional specific monoclonal antibodies to either gastrin-releasing peptide or gastrin were used as models to validate the general application of our modified assay. Conditions for radioactive labeling of the monoclonal antibody were determined to minimize oxidant damage, which compromises the sensitivity of other reported peptide quantitation assays. Pretreatment of 96-well polyvinyl chloride test plates with a 5% glutaraldehyde solution resulted in consistent retention of sufficient target peptide on the solid-phase matrix to allow precise quantitation. This quantitative method is completed within 1 h of peptide solid phasing. Pretreatment of assay plates with glutaraldehyde increased binding of target peptide and maximized antibody binding by optimizing antigen presentation. The hypothesis that glutaraldehyde affects both peptide binding to the plate and orientation of the peptide was confirmed by analysis of several peptide analogs. These studies indicate that peptide binding was mediated through a free amino group leaving the carboxy-terminal portion of the target peptide accessible for antibody binding. It was observed that the length of the peptide also affects the amount of monoclonal antibody that will bind. Under the optimal conditions, results from quantitation of gastrin-releasing peptide in relevant samples agree well with those from previously reported techniques. Thus, we report here a modified microplate assay which may be generally applied for the rapid and sensitive quantitation of peptide hormones

  14. Combinatorial Solid-Phase Synthesis of Balanol Analogues

    DEFF Research Database (Denmark)

    Nielsen, John; Lyngsø, Lars Ole

    1996-01-01

    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...

  15. Surface phase transitions in cu-based solid solutions

    Science.gov (United States)

    Zhevnenko, S. N.; Chernyshikhin, S. V.

    2017-11-01

    We have measured surface energy in two-component Cu-based systems in H2 + Ar gas atmosphere. The experiments on solid Cu [Ag] and Cu [Co] solutions show presence of phase transitions on the surfaces. Isotherms of the surface energy have singularities (the minimum in the case of copper solid solutions with silver and the maximum in the case of solid solutions with cobalt). In both cases, the surface phase transitions cause deficiency of surface miscibility: formation of a monolayer (multilayer) (Cu-Ag) or of nanoscale particles (Cu-Co). At the same time, according to the volume phase diagrams, the concentration and temperature of the surface phase transitions correspond to the solid solution within the volume. The method permits determining the rate of diffusional creep in addition to the surface energy. The temperature and concentration dependence of the solid solutions' viscosity coefficient supports the fact of the surface phase transitions and provides insights into the diffusion properties of the transforming surfaces.

  16. Indirect solid-phase immunosorbent assay for detection of arenavirus antigens and antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, A P; Rezapkin, G V; Dzagurova, T K; Tkachenko, E A [Institute of Poliomyelitis anU Viral Encephalities of the U.S.S.R. Academy of Medical Sciences, Moscow

    1984-05-01

    Indirect enzyme-linked immunosorbent assay (ELISA) and solid phase radioimmunoassay (SPRIA) using either enti-human or anti-mouse IgG labelled with horseradish peroxidase and /sup 125/I, respectively, were developed for the detection of Junin, Machupo, Tacaribe, Amapari, Tamiami, Lassa and LCM arenaviruses. Both methods allow high sensitivity detection of arenavirus antigens and antibodies.

  17. Phase-sensitive flow cytometer

    Energy Technology Data Exchange (ETDEWEB)

    Steinkamp, J.A.

    1992-12-31

    This report describes phase-sensitive flow cytometer (FCM) which provides additional FCM capability to use the fluorescence lifetime of one or more fluorochromes bound to single cells to provide additional information regarding the cells. The resulting fluorescence emission can be resolved into individual fluorescence signals if two fluorochromes are present or can be converted directly to a decay lifetime from a single fluorochrome. The excitation light for the fluorochromes is modulated to produce an amplitude modulated fluorescence pulse as the fluorochrome is excited in the FCM. The modulation signal also forms a reference signal that is phase-shifted a selected amount for subsequent mixing with the output modulated fluorescence intensity signal in phase-sensitive detection circuitry. The output from the phase-sensitive circuitry is then an individual resolved fluorochrome signal or a single fluorochrome decay lifetime, depending on the applied phase shifts.

  18. Solid phase transformations

    CERN Document Server

    Čermák, J

    2008-01-01

    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

  19. Rapid and sensitive determination of major polyphenolic components in Euphoria longana Lam. seeds using matrix solid-phase dispersion extraction and UHPLC with hybrid linear ion trap triple quadrupole mass spectrometry.

    Science.gov (United States)

    Rathore, Atul S; Sathiyanarayanan, L; Deshpande, Shreekant; Mahadik, Kakasaheb R

    2016-11-01

    A rapid and sensitive method for the extraction and determination of four major polyphenolic components in Euphoria longana Lam. seeds is presented for the first time based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry. Matrix solid-phase dispersion method was designed for the extraction of Euphoria longana seed constituents and compared with microwave-assisted extraction and ultrasonic-assisted extraction methods. An Ultra high performance liquid chromatography with hybrid triple quadrupole linear ion-trap mass spectrometry method was developed for quantitative analysis in multiple-reaction monitoring mode in negative electrospray ionization. The chromatographic separation was accomplished using an ACQUITY UPLC BEH C 18 (2.1 mm × 50 mm, 1.7 μm) column with gradient elution of 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. The developed method was validated with acceptable linearity (r 2 > 0.999), precision (RSD ≤ 2.22%) and recovery (RSD ≤ 2.35%). The results indicated that matrix solid-phase dispersion produced comparable extraction efficiency compared with other methods nevertheless was more convenient and time-saving with reduced requirements on sample and solvent volumes. The proposed method is rapid and sensitive in providing a promising alternative for extraction and comprehensive determination of active components for quality control of Euphoria longana products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Solid-Solid Vacuum Regolith Heat-Exchanger for Oxygen Production, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — This SBIR Phase-1 project will demonstrate the feasibility of using a novel coaxial counterflow solid-solid heat exchanger to recover heat energy from spent regolith...

  1. New Solid Phases for Estimation of Hormones by Radioimmunoassay Technique

    International Nuclear Information System (INIS)

    Sheha, R.R.; Ayoub, H.S.M.; Shafik, M.

    2013-01-01

    The efforts in this study were initiated to develop and validate new solid phases for estimation of hormones by radioimmunoassay (RIA). The study argued the successful application of different hydroxy apatites (HAP) as new solid phases for estimation of Alpha fetoprotein (AFP), Thyroid Stimulating hormone (TSH) and Luteinizing hormone (LH) in human serum. Hydroxy apatites have different alkali earth elements were successfully prepared by a well-controlled co-precipitation method with stoichiometric ratio value 1.67. The synthesized barium and calcium hydroxy apatites were characterized using XRD and Ftir and data clarified the preparation of pure structures of both BaHAP and CaHAP with no evidence on presence of other additional phases. The prepared solid phases were applied in various radioimmunoassay systems for separation of bound and free antigens of AFP, TSH and LH hormones. The preparation of radiolabeled tracer for these antigens was carried out using chloramine-T as oxidizing agent. The influence of different parameters on the activation and coupling of the used apatite particles with the polyclonal antibodies was systematically investigated and the optimum conditions were determined. The assay was reproducible, specific and sensitive enough for regular estimation of the studied hormones. The intra-and inter-assay variation were satisfactory and also the recovery and dilution tests indicated an accurate calibration. The reliability of these apatite particles had been validated by comparing the results that obtained by using commercial kits. The results finally authenticates that hydroxyapatite particles would have a great potential to address the emerging challenge of accurate quantitation in laboratory medical application

  2. Comparison of solid and liquid-phase bioassays using ecoscores to assess contaminated soils

    Energy Technology Data Exchange (ETDEWEB)

    Lors, Christine [Universite Lille Nord de France, 1bis rue Georges Lefevre, 59044 Lille Cedex (France); Ecole des Mines de Douai, LGCgE-MPE-GCE, 941 rue Charles-Bourseul, 59500 Douai (France); Centre National de Recherche sur les Sites et Sols Pollues, 930 Boulevard Lahure, BP 537, 59505 Douai Cedex (France); Ponge, Jean-Francois, E-mail: ponge@mnhn.fr [Museum National d' Histoire Naturelle, Departement Ecologie et Gestion de la Biodiversite, CNRS UMR 7179, 4 Avenue du Petit-Chateau, 91800 Brunoy (France); Martinez Aldaya, Maite [Museum National d' Histoire Naturelle, Departement Ecologie et Gestion de la Biodiversite, CNRS UMR 7179, 4 Avenue du Petit-Chateau, 91800 Brunoy (France); Damidot, Denis [Universite Lille Nord de France, 1bis rue Georges Lefevre, 59044 Lille Cedex (France); Ecole des Mines de Douai, LGCgE-MPE-GCE, 941 rue Charles-Bourseul, 59500 Douai (France)

    2011-10-15

    Bioassays on aqueous and solid phases of contaminated soils were compared, belonging to a wide array of trophic and response levels and using ecoscores for evaluating ecotoxicological and genotoxicological endpoints. The method was applied to four coke factory soils contaminated mainly with PAHs, but also to a lesser extent by heavy metals and cyanides. Aquatic bioassays do not differ from terrestrial bioassays when scaling soils according to toxicity but they are complementary from the viewpoint of ecological relevance. Both aquatic and terrestrial endpoints are strongly correlated with concentrations of 3-ring PAHs. This evaluation procedure allows us to propose a cost-effective battery which embraces a wide array of test organisms and response levels: it includes two rapid bioassays (Microtox) and springtail avoidance), a micronucleus test and three bioassays of a longer duration (algal growth, lettuce germination and springtail reproduction). This battery can be recommended for a cost-effective assessment of polluted/remediated soils. - Highlights: > Comparison of liquid- and solid-phase bioassays on contaminated soils, using ecoscores. > Complementarity of liquid- and solid-phase bioassays for the evaluation of environmental hazards. > Proposal for a restricted battery of 5 most sensitive tests. > Use of this restricted battery for a cost-effective assessment of polluted/remediated soils. - Aqueous and solid phases of contaminated soils give similar results in terms of toxicity but are complementary for the evaluation of environmental hazards by ecoscores.

  3. Solid-phase spectrophotometry

    International Nuclear Information System (INIS)

    Brykina, G.D.; Marchenko, D.Yu.; Shpigun, O.A.

    1995-01-01

    Solid-phase spectrophotometry (SPS), which is based on the direct measurement of light absorption of an ion exchanger containing a substance of interest, was reviewed. Since 1976, it has been known that aborbance of an ion exchanger is directly proportional to the concentration of a particular ion in solution. A similar dependence can also be followed for other sorbents, as well as for foams, membranes, films, etc., which do not exhibit ion exchange properties. One can use absorption, diffuse reflection, and luminescence spectra parameters as an analytical signal. Thus, SPS of ion exchangers is among the analytical techniques that combine the sorption concentration and surface determination of the substance of interest. This review summarizes the advancements in SPS over the last six years and demonstrates the prospects for its development. Special attention is paid to experimental methods for measuring solid-phase absorption and to the basic procedures of sample preparation, including new ones. These two facets are of great importance for obtaining precise results and extending the capabilities of SPS

  4. Detection and specifity of class specific antibodies to whole bacteria cells using a solid phase radioimmunoassay

    Energy Technology Data Exchange (ETDEWEB)

    Czerkinsky, C.; Rees, A.S.; Bergimeier, L.A.; Challacombe, S.J. (Guy' s Hospital Medical and Dental Schools, London (UK))

    1983-07-01

    A solid phase radioimmunoassay has been developed which can be used for the detection of isotype specific antibodies to whole bacteria and other particulate antigens, and is applicable to a variety of species. Bacteria are bound to the solid phase by the use either of antibodies, or of methyl glyoxal. Both methods result in a sensitive and reproducible assay, and bacteria do not appear to desorb from the solid phase. The specificity of antibodies to whole bacteria was examined by absorption of antisera with various species of bacteria and retesting, or by determining the binding of antisera to various bacteria bound to the solid phase. Both methods revealed specificity for the bacteria examined. Inhibition studies showed that antibodies to Streptococcus mutans whole cells could be inhibited by purified cell surface antigens glucosyltransferase and antigen I/II, but only minimally by lipoteichoic acid, c polysaccharide or dextran. In murine antisera antibodies of the IgG, IgM, and IgA classes could be detected at amounts of less than 1 ng/ml.

  5. Anti-glomerular basement membrane autoantibodies in the Brown Norway rat: detection by a solid-phase radioimmunoassay

    International Nuclear Information System (INIS)

    Bowman, C.; Peters, D.K.; Lockwood, C.M.

    1983-01-01

    A solid-phase radioimmunoassay (RIA) is described for the detection of IgG autoantibodies to glomerular basement membrane (GBM) induced in the Brown Norway rat by mercuric chloride. The assay involves the adsorption of a collagenase digest of GBM to plastic microtitre plates and detection of bound antibody with affinity purified radiolabelled rabbit anti-rat IgG. Comparison with existing immunofluorescence methods for detection of anti-GBM antibody showed that the solid-phase RIA is highly sensitive, allowing detection of antibody in solutions with as low as 0.5 ng protein/ml. The assay is suitable for detection of anti-GBM antibody both in serum and in eluates from nephritic kidneys. The assay proved to be specific in competitive studies of inhibition brought about by GBM, keyhole limpet antigen and ovalbumin. This solid-phase RIA is reproducible, robust and easy to perform. (Auth.)

  6. Wax Precipitation Modeled with Many Mixed Solid Phases

    DEFF Research Database (Denmark)

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

    2005-01-01

    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......-temperature and low-temperature forms, are pure. Model calculations compare well with the data of Pauly et al. for C18 to C30 waxes precipitating from n-decane solutions. (C) 2004 American Institute of Chemical Engineers....

  7. Sensitive Quantification of Cannabinoids in Milk by Alkaline Saponification-Solid Phase Extraction Combined with Isotope Dilution UPLC-MS/MS.

    Science.gov (United States)

    Wei, Binnian; McGuffey, James E; Blount, Benjamin C; Wang, Lanqing

    2016-01-01

    Maternal exposure to marijuana during the lactation period-either active or passive-has prompted concerns about transmission of cannabinoids to breastfed infants and possible subsequent adverse health consequences. Assessing these health risks requires a sensitive analytical approach that is able to quantitatively measure trace-level cannabinoids in breast milk. Here, we describe a saponification-solid phase extraction approach combined with ultra-high-pressure liquid chromatography-tandem mass spectrometry for simultaneously quantifying Δ9-tetrahydrocannabinol (THC), cannabidiol (CBD), and cannabinol (CBN) in breast milk. We demonstrate for the first time that constraints on sensitivity can be overcome by utilizing alkaline saponification of the milk samples. After extensively optimizing the saponification procedure, the validated method exhibited limits of detections of 13, 4, and 66 pg/mL for THC, CBN, and CBD, respectively. Notably, the sensitivity achieved was significantly improved, for instance, the limits of detection for THC is at least 100-fold more sensitive compared to that previously reported in the literature. This is essential for monitoring cannabinoids in breast milk resulting from passive or nonrecent active maternal exposure. Furthermore, we simultaneously acquired multiple reaction monitoring transitions for 12 C- and 13 C-analyte isotopes. This combined analysis largely facilitated data acquisition by reducing the repetitive analysis rate for samples exceeding the linear limits of 12 C-analytes. In addition to high sensitivity and broad quantitation range, this method delivers excellent accuracy (relative error within ±10%), precision (relative standard deviation <10%), and efficient analysis. In future studies, we expect this method to play a critical role in assessing infant exposure to cannabinoids through breastfeeding.

  8. Solid - solid and solid - liquid phase transitions of iron and iron alloys under laser shock compression

    Science.gov (United States)

    Harmand, M.; Krygier, A.; Appel, K.; Galtier, E.; Hartley, N.; Konopkova, Z.; Lee, H. J.; McBride, E. E.; Miyanishi, K.; Nagler, B.; Nemausat, R.; Vinci, T.; Zhu, D.; Ozaki, N.; Fiquet, G.

    2017-12-01

    An accurate knowledge of the properties of iron and iron alloys at high pressures and temperatures is crucial for understanding and modelling planetary interiors. While Earth-size and Super-Earth Exoplanets are being discovered in increasingly large numbers, access to detailed information on liquid properties, melting curves and even solid phases of iron and iron at the pressures and temperatures of their interiors is still strongly limited. In this context, XFEL sources coupled with high-energy lasers afford unique opportunities to measure microscopic structural properties at far extreme conditions. Also the achievable time resolution allows the shock history and phase transition mechanisms to be followed during laser compression, improving our understanding of the high pressure and high strain experiments. Here we present recent studies devoted to investigate the solid-solid and solid-liquid transition in laser-shocked iron and iron alloys (Fe-Si, Fe-C and Fe-O alloys) using X-ray diffraction and X-ray diffuse scattering. Experiment were performed at the MEC end-station of the LCLS facility at SLAC (USA). Detection of the diffuse scattering allowed the identification of the first liquid peak position along the Hugoniot, up to 4 Mbar. The time resolution shows ultrafast (between several tens and several hundreds of picoseconds) solid-solid and solid-liquid phase transitions. Future developments at XFEL facilities will enable detailed studies of the solid and liquid structures of iron and iron alloys as well as out-of-Hugoniot studies.

  9. Multiple solid-phase microextraction

    NARCIS (Netherlands)

    Koster, EHM; de Jong, GJ

    2000-01-01

    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

  10. Comparison of solid and liquid-phase bioassays using ecoscores to assess contaminated soils

    International Nuclear Information System (INIS)

    Lors, Christine; Ponge, Jean-Francois; Martinez Aldaya, Maite; Damidot, Denis

    2011-01-01

    Bioassays on aqueous and solid phases of contaminated soils were compared, belonging to a wide array of trophic and response levels and using ecoscores for evaluating ecotoxicological and genotoxicological endpoints. The method was applied to four coke factory soils contaminated mainly with PAHs, but also to a lesser extent by heavy metals and cyanides. Aquatic bioassays do not differ from terrestrial bioassays when scaling soils according to toxicity but they are complementary from the viewpoint of ecological relevance. Both aquatic and terrestrial endpoints are strongly correlated with concentrations of 3-ring PAHs. This evaluation procedure allows us to propose a cost-effective battery which embraces a wide array of test organisms and response levels: it includes two rapid bioassays (Microtox) and springtail avoidance), a micronucleus test and three bioassays of a longer duration (algal growth, lettuce germination and springtail reproduction). This battery can be recommended for a cost-effective assessment of polluted/remediated soils. - Highlights: → Comparison of liquid- and solid-phase bioassays on contaminated soils, using ecoscores. → Complementarity of liquid- and solid-phase bioassays for the evaluation of environmental hazards. → Proposal for a restricted battery of 5 most sensitive tests. → Use of this restricted battery for a cost-effective assessment of polluted/remediated soils. - Aqueous and solid phases of contaminated soils give similar results in terms of toxicity but are complementary for the evaluation of environmental hazards by ecoscores.

  11. Development of solid phase radioimmunoassay using antibody coupled magnetizable particles for measurement of progesterone in human serum

    International Nuclear Information System (INIS)

    Mehany, N.L.

    2007-01-01

    The aim of the present study was to prepare solid phase radioimmunoassay (RIA) reagents. Development as well as optimization and validation of RIA system using solid phase magnetic particles for the measurement of progesterone in human serum are described. The production of polyclonal antibodies was carried out by immunizing five white New-Zealand rabbits subcutaneously. Low density magnetizable cellulose iron oxide particles have been used to couple covalently to the IgG fraction of polyclonal anti-progesterone using carbonyl diimidazole activation method and applied as a solid phase separating agent for RIA of serum progesterone. 125 I-progesterone tracer was prepared using chloramine-T and iodogen oxidation methods and purified using high performance liquid chromatography. The progesterone standards were prepared using highly purified progesterone powder with hormone free serum as standard matrix. Optimization and validation of the assay were carried out. The results obtained provide a low cost, simple, sensitive, specific and accurate RIA system of progesterone based on magnetizable solid phase separation. This may be extremely helpful in diagnosis and proper management of ovulation during childbearing years

  12. The detection and specifity of class specific antibodies to whole bacteria cells using a solid phase radioimmunoassay

    International Nuclear Information System (INIS)

    Czerkinsky, C.; Rees, A.S.; Bergimeier, L.A.; Challacombe, S.J.

    1983-01-01

    A solid phase radioimmunoassay has been developed which can be used for the detection of isotype specific antibodies to whole bacteria and other particulate antigens, and is applicable to a variety of species. Bacteria are bound to the solid phase by the use either of antibodies, or of methyl glyoxal. Both methods result in a sensitive and reproducible assay, and bacteria do not appear to desorb from the solid phase. The specificity of antibodies to whole bacteria was examined by absorption of antisera with various species of bacteria and retesting, or by determining the binding of antisera to various bacteria bound to the solid phase. Both methods revealed specificity for the bacteria examined. Inhibition studies showed that antibodies to Streptococcus mutans whole cells could be inhibited by purified cell surface antigens glucosyltransferase and antigen I/II, but only minimally by lipoteichoic acid, c polysaccharide or dextran. In murine antisera antibodies of the IgG, IgM, and IgA classes could be detected at amounts of less than 1 ng/ml. (author)

  13. Effect of solids, caloric content on dual-phase gastric emptying

    Energy Technology Data Exchange (ETDEWEB)

    Van Den Maegdenbergh, V.; Urbain, J.L.; Siegel, J.A.; Mortelmans, L.; De Roo, M. (Univ. Hospital Gasthuisberg, Leuven (Belgium) Temple Univ. Hospital, Philadelphia, PA (USA))

    1990-03-01

    The dual-phase gastric emptying technique is routinely employed to determine the differential emptying of solids and liquids in a wide spectrum of gastrointestinal diseases. Composition, acidity, volume, caloric density, physical form and viscosity of the test means have been shown to be important determinants for the quantitative evaluation of gastric emptying. In this study, the authors have evaluated the effect of increasing the caloric content of the solid portion of a physiologic test mean on both solid and liquid emptying kinetics in health male volunteers. They observed that increasing solid caloric content delayed emptying of both solids and liquids. For the solid phase, the delay was accounted for by a longer lag phase and decrease in emptying rate; for liquids a longer emptying rate was also obtained. They conclude that modification of the caloric content of the solid portion of a meal not only affects the emptying of the solid phase but also alters the emptying of the liquid component of the meal.

  14. Phase stability in wear-induced supersaturated Al-Ti solid solution

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, Y.; Yokoyama, K. [Dept. of Functional Machinery Mechanics Shinshu Univ., Ueda (Japan); Hosoda, H. [Precision and Intelligence Lab., Tokyo Inst. of Tech., Nagatsuta, Midori-ku, Yokohama (Japan)

    2002-07-01

    Al-Ti supersaturated solid solutions were introduced by wear testing and the rapid quenching of an Al/Al{sub 3}Ti composite (part of an Al/Al{sub 3}Ti functionally graded material) that was fabricated using the centrifugal method. The phase stability of the supersaturated solid solution was studied through systematic annealing of the supersaturated solid solution. It was found that the Al-Ti supersaturated solid solution decomposed into Al and Al{sub 3}Ti intermetallic compound phases during the heat treatment. The Al-Ti supersaturated solid solutions fabricated were, therefore, not an equilibrium phase, and thus decomposed into the equilibrium phases during heat treatment. It was also found that heat treatment leads to a significant hardness increase for the Al-Ti supersaturated solid solution. Finally, it was concluded that formation of the wear-induced supersaturated solid solution layer was a result of severe plastic deformation. (orig.)

  15. Hyperbranched quasi-1D nanostructures for solid-state dye-sensitized solar cells.

    Science.gov (United States)

    Passoni, Luca; Ghods, Farbod; Docampo, Pablo; Abrusci, Agnese; Martí-Rujas, Javier; Ghidelli, Matteo; Divitini, Giorgio; Ducati, Caterina; Binda, Maddalena; Guarnera, Simone; Li Bassi, Andrea; Casari, Carlo Spartaco; Snaith, Henry J; Petrozza, Annamaria; Di Fonzo, Fabio

    2013-11-26

    In this work we demonstrate hyperbranched nanostructures, grown by pulsed laser deposition, composed of one-dimensional anatase single crystals assembled in arrays of high aspect ratio hierarchical mesostructures. The proposed growth mechanism relies on a two-step process: self-assembly from the gas phase of amorphous TiO2 clusters in a forest of tree-shaped hierarchical mesostructures with high aspect ratio; oriented crystallization of the branches upon thermal treatment. Structural and morphological characteristics can be optimized to achieve both high specific surface area for optimal dye uptake and broadband light scattering thanks to the microscopic feature size. Solid-state dye sensitized solar cells fabricated with arrays of hyperbranched TiO2 nanostructures on FTO-glass sensitized with D102 dye showed a significant 66% increase in efficiency with respect to a reference mesoporous photoanode and reached a maximum efficiency of 3.96% (among the highest reported for this system). This result was achieved mainly thanks to an increase in photogenerated current directly resulting from improved light harvesting efficiency of the hierarchical photoanode. The proposed photoanode overcomes typical limitations of 1D TiO2 nanostructures applied to ss-DSC and emerges as a promising foundation for next-generation high-efficiency solid-state devices comprosed of dyes, polymers, or quantum dots as sensitizers.

  16. Practical application of solid phase spectrophotometry in analysis of materials and goods of mining and metallurgy

    International Nuclear Information System (INIS)

    Duan Qunzhang

    1999-01-01

    The author reviewed recent development and practical application of solid phase spectrophotometry in analysis of materials and goods of mining-metallurgy. Separation and preconcentration and conditions of coloring determination, sensitivity and range of detection, as well as interference of corresponding method are discussed

  17. Visualizing a dilute vortex liquid to solid phase transition in a Bi2Sr2CaCu2O8 single crystal

    International Nuclear Information System (INIS)

    Shaw, Gorky; Mandal, Pabitra; Banerjee, S S; Tamegai, T

    2012-01-01

    Using high-sensitivity magneto-optical imaging, we find evidence for a jump in local vortex density associated with a vortex liquid to vortex solid phase transition just above the lower critical field in a single crystal of Bi 2 Sr 2 CaCu 2 O 8 . We find that the regions of the sample where the jump in vortex density occurs are associated with low screening currents. In the field–temperature vortex phase diagram, we identify phase boundaries demarcating a dilute vortex liquid phase and the vortex solid phase. The phase diagram also identifies a coexistence regime of the dilute vortex liquid and solid phases and shows the effect of pinning on the vortex liquid to vortex solid phase transition line. We find that the phase boundary lines can be fitted to the theoretically predicted expression for the low-field portion of the phase boundary delineating a dilute vortex solid from a vortex liquid phase. We show that the same theoretical fit can be used to describe the pinning dependence of the low-field phase boundary lines provided that the dependence of the Lindemann number on pinning strength is considered. (paper)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-06-24

    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.

  19. Phase-space evolution of x-ray coherence in phase-sensitive imaging.

    Science.gov (United States)

    Wu, Xizeng; Liu, Hong

    2008-08-01

    X-ray coherence evolution in the imaging process plays a key role for x-ray phase-sensitive imaging. In this work we present a phase-space formulation for the phase-sensitive imaging. The theory is reformulated in terms of the cross-spectral density and associated Wigner distribution. The phase-space formulation enables an explicit and quantitative account of partial coherence effects on phase-sensitive imaging. The presented formulas for x-ray spectral density at the detector can be used for performing accurate phase retrieval and optimizing the phase-contrast visibility. The concept of phase-space shearing length derived from this phase-space formulation clarifies the spatial coherence requirement for phase-sensitive imaging with incoherent sources. The theory has been applied to x-ray Talbot interferometric imaging as well. The peak coherence condition derived reveals new insights into three-grating-based Talbot-interferometric imaging and gratings-based x-ray dark-field imaging.

  20. Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow

    NARCIS (Netherlands)

    Roes, A.W.M.; van Swaaij, Willibrordus Petrus Maria

    1979-01-01

    Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow, a promising new countercurrent operation, was evaluated using residence time distribution (RTD) experiments. The column was packed with dumped Pall rings, the gas phase was air at ambient conditions and the solid

  1. Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

    Science.gov (United States)

    Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

    2007-11-15

    The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

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

    Directory of Open Access Journals (Sweden)

    Xiaoyan Lu

    2016-10-01

    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.

  3. Application of solid-phase microextraction in analytical toxicology.

    Science.gov (United States)

    Pragst, Fritz

    2007-08-01

    Solid-phase microextraction (SPME) is a miniaturized and solvent-free sample preparation technique for chromatographic-spectrometric analysis by which the analytes are extracted from a gaseous or liquid sample by absorption in, or adsorption on, a thin polymer coating fixed to the solid surface of a fiber, inside an injection needle or inside a capillary. In this paper, the present state of practical performance and of applications of SPME to the analysis of blood, urine, oral fluid and hair in clinical and forensic toxicology is reviewed. The commercial coatings for fibers or needles have not essentially changed for many years, but there are interesting laboratory developments, such as conductive polypyrrole coatings for electrochemically controlled SPME of anions or cations and coatings with restricted-access properties for direct extraction from whole blood or immunoaffinity SPME. In-tube SPME uses segments of commercial gas chromatography (GC) capillaries for highly efficient extraction by repeated aspiration-ejection cycles of the liquid sample. It can be easily automated in combination with liquid chromatography but, as it is very sensitive to capillary plugging, it requires completely homogeneous liquid samples. In contrast, fiber-based SPME has not yet been performed automatically in combination with high-performance liquid chromatography. The headspace extractions on fibers or needles (solid-phase dynamic extraction) combined with GC methods are the most advantageous versions of SPME because of very pure extracts and the availability of automatic samplers. Surprisingly, substances with quite high boiling points, such as tricyclic antidepressants or phenothiazines, can be measured by headspace SPME from aqueous samples. The applicability and sensitivity of SPME was essentially extended by in-sample or on-fiber derivatization. The different modes of SPME were applied to analysis of solvents and inhalation narcotics, amphetamines, cocaine and metabolites

  4. Using reweighting and free energy surface interpolation to predict solid-solid phase diagrams

    Science.gov (United States)

    Schieber, Natalie P.; Dybeck, Eric C.; Shirts, Michael R.

    2018-04-01

    Many physical properties of small organic molecules are dependent on the current crystal packing, or polymorph, of the material, including bioavailability of pharmaceuticals, optical properties of dyes, and charge transport properties of semiconductors. Predicting the most stable crystalline form at a given temperature and pressure requires determining the crystalline form with the lowest relative Gibbs free energy. Effective computational prediction of the most stable polymorph could save significant time and effort in the design of novel molecular crystalline solids or predict their behavior under new conditions. In this study, we introduce a new approach using multistate reweighting to address the problem of determining solid-solid phase diagrams and apply this approach to the phase diagram of solid benzene. For this approach, we perform sampling at a selection of temperature and pressure states in the region of interest. We use multistate reweighting methods to determine the reduced free energy differences between T and P states within a given polymorph and validate this phase diagram using several measures. The relative stability of the polymorphs at the sampled states can be successively interpolated from these points to create the phase diagram by combining these reduced free energy differences with a reference Gibbs free energy difference between polymorphs. The method also allows for straightforward estimation of uncertainties in the phase boundary. We also find that when properly implemented, multistate reweighting for phase diagram determination scales better with the size of the system than previously estimated.

  5. Heterogeneous Ferroelectric Solid Solutions Phases and Domain States

    CERN Document Server

    Topolov, Vitaly

    2012-01-01

    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.

  6. Development Of Solid Phase Radioimmunoassay Using Antibody Coupled Cellulose Particles For Measurement Of Prolactin In Human Serum

    International Nuclear Information System (INIS)

    Abdel-Ghany, I.Y.

    2013-01-01

    The objective of the present study was to prepare solid phase radioimmunoassay (RIA) reagents. Development as well as optimization and validation of RIA system using solid phase cellulose particles for the measurement of prolactin (PRL) in human serum were described. The production of polyclonal antibodies was carried out by immunizing three Balb/C mice intraperitoneal through primary injection and two booster doses. The activation of cellulose particles using 1,1-carbonyl diimidazole (CDI) and coupling of these solid phase particles with IgG fraction of mouse anti-PRL were carried out. Preparation of 125 I-PRL tracer was prepared using lactoperoxidase method then purified by gel filtration using sephadex G-100. The PRL standards were prepared using a highly purified PRL antigen with assay buffer as standard matrix. Optimization and validation of the assay were carried out. The results obtained provide a low cost, simple, sensitive, specific and accurate RIA system of prolactin based on solid phase separation. These cellulose particles retain their characteristics during storage for 6 months at 4 degree C. In conclusion, this assay could be used as a useful diagnostic tool for pituitary dysfunctions and possible reproductive disability

  7. Solid-phase single molecule biosensing using dual-color colocalization of fluorescent quantum dot nanoprobes

    Science.gov (United States)

    Liu, Jianbo; Yang, Xiaohai; Wang, Kemin; Wang, Qing; Liu, Wei; Wang, Dong

    2013-10-01

    The development of solid-phase surface-based single molecule imaging technology has attracted significant interest during the past decades. Here we demonstrate a sandwich hybridization method for highly sensitive detection of a single thrombin protein at a solid-phase surface based on the use of dual-color colocalization of fluorescent quantum dot (QD) nanoprobes. Green QD560-modified thrombin binding aptamer I (QD560-TBA I) were deposited on a positive poly(l-lysine) assembled layer, followed by bovine serum albumin blocking. It allowed the thrombin protein to mediate the binding of the easily detectable red QD650-modified thrombin binding aptamer II (QD650-TBA II) to the QD560-TBA I substrate. Thus, the presence of the target thrombin can be determined based on fluorescent colocalization measurements of the nanoassemblies, without target amplification or probe separation. The detection limit of this assay reached 0.8 pM. This fluorescent colocalization assay has enabled single molecule recognition in a separation-free detection format, and can serve as a sensitive biosensing platform that greatly suppresses the nonspecific adsorption false-positive signal. This method can be extended to other areas such as multiplexed immunoassay, single cell analysis, and real time biomolecule interaction studies.The development of solid-phase surface-based single molecule imaging technology has attracted significant interest during the past decades. Here we demonstrate a sandwich hybridization method for highly sensitive detection of a single thrombin protein at a solid-phase surface based on the use of dual-color colocalization of fluorescent quantum dot (QD) nanoprobes. Green QD560-modified thrombin binding aptamer I (QD560-TBA I) were deposited on a positive poly(l-lysine) assembled layer, followed by bovine serum albumin blocking. It allowed the thrombin protein to mediate the binding of the easily detectable red QD650-modified thrombin binding aptamer II (QD650-TBA II) to

  8. Integration of Solid-phase Extraction with Electrothermal Atomic Absorption Spectrometry for Determination of Trace Elements

    OpenAIRE

    NUKATSUKA, Isoshi; OHZEKI, Kunio

    2006-01-01

    An enrichment step in a sample treatment is essential for trace analysis to improve the sensitivity and to eliminate the matrix of the sample. Solid-phase extraction (SPE) is one of the widely used enrichment technique. Electrothermal atomic absorption spectrometry (ETAAS) is a well-established determination technique for trace elements. The integration of SPE with ETAAS leads to further improvement of sensitivity, an automation of the measurement and the economy in the sample size, amounts o...

  9. New solid phase radioimmunoassay (CLB-RIA) for the detection of hepatitis-B antigen and antibody

    Energy Technology Data Exchange (ETDEWEB)

    Duimel, W J [Centraal Laboratorium van de Bloedtransfusiedienst, Amsterdam; Brummelhuis, H G.J.

    1975-07-01

    A new competitive solid phase radioimmunoassay (CLB-RIA) has been developed for the detection of HBAg and HBAb in human serum and plasma. In the assay, sheep antibodies to HBAg, covalently linked to an insoluble carrier, highly purified /sup 125/I labelled HBAg and the serum or plasma sample are incubated for 20 h at room temperature. After incubation, the bound and the free fraction of the tracer are separated by centrifugation. The presence of both HBAg and HBAb results in a decrease of the amount of bound tracer, when compared with a negative control serum. Differentiation between HBAg and HBAb requires the use of another type of radioimmunoassay. For this purpose a sandwich solid phase radioimmunoassay, for the detection of HBAb only, has been developed (CLB-AURIA). In this, assay-purified HBAg is covalently linked to an insoluble carrier. Using a mixture of both immunosorbents (insolubilized HBAg and HBAb), it is possible to detect and to distinguish HBAg and HBAb in one single solid phase radioimmunoassay (CLB-MIRIA). The influence of three parameters on the CLB-RIA, the incubation time, the amount of tracer and the effect of Tween-20 has been studied. The sensitivity of the described solid phase CLB-RIA for the detection of HBAg is comparable to that of other radioimmunoassays reported in literature; its specificity is very high.

  10. The Gaseous Phase as a Probe of the Astrophysical Solid Phase Chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Abou Mrad, Ninette; Duvernay, Fabrice; Isnard, Robin; Chiavassa, Thierry; Danger, Grégoire, E-mail: gregoire.danger@univ-amu.fr [Aix-Marseille Université, PIIM UMR-CNRS 7345, F-13397 Marseille (France)

    2017-09-10

    In support of space missions and spectroscopic observations, laboratory experiments on ice analogs enable a better understanding of organic matter formation and evolution in astrophysical environments. Herein, we report the monitoring of the gaseous phase of processed astrophysical ice analogs to determine if the gaseous phase can elucidate the chemical mechanisms and dominant reaction pathways occurring in the solid ice subjected to vacuum ultra-violet (VUV) irradiation at low temperature and subsequently warmed. Simple (CH{sub 3}OH), binary (H{sub 2}O:CH{sub 3}OH, CH{sub 3}OH:NH{sub 3}), and ternary ice analogs (H{sub 2}O:CH{sub 3}OH:NH{sub 3}) were VUV-processed and warmed. The evolution of volatile organic compounds in the gaseous phase shows a direct link between their relative abundances in the gaseous phase, and the radical and thermal chemistries modifying the initial ice composition. The correlation between the gaseous and solid phases may play a crucial role in deciphering the organic composition of astrophysical objects. As an example, possible solid compositions of the comet Lovejoy are suggested using the abundances of organics in its comae.

  11. A Novel Phase-Locking-Free Phase Sensitive Amplifier based Regenerator

    DEFF Research Database (Denmark)

    Kjøller, Niels-Kristian; Røge, Kasper Meldgaard; Guan, Pengyu

    2016-01-01

    We propose a scheme for phase regeneration of optical binary phase-shift keying (BPSK) data signals based on phase sensitive amplification without active phase-locking. A delay interferometer (DI) is used to convert a BPSK signal impaired by noise to an amplitude modulated signal followed by cross......-locked pumps. As a result, active phase-stabilization is avoided. A proof-of-principle experiment is carried out with a dual-pump degenerate phase sensitive amplifier (PSA), demonstrating regeneration for a 10 Gb/s non-return-to-zero differential BPSK (NRZ-DPSK) data signal degraded by a sinusoidal phase...

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

    DEFF Research Database (Denmark)

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

    2009-01-01

    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...

  13. Role of nanoparticles in analytical solid phase microextraction (SPME)

    NARCIS (Netherlands)

    Zielinska, K.; Leeuwen, van H.P.

    2013-01-01

    Solid phase microextraction (SPME) is commonly used to measure the free concentration of fairly hydrophobic substances in aqueous media on the basis of their partitioning between sample solution and a solid phase. Here we study the role of nanoparticles that may sorb the analyte in the sample

  14. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    International Nuclear Information System (INIS)

    Herrero Latorre, C.; Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.

    2012-01-01

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► 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.

  15. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [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)

    2012-10-24

    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.

  16. Analytical study of solids-gas two phase flow

    International Nuclear Information System (INIS)

    Hosaka, Minoru

    1977-01-01

    Fundamental studies were made on the hydrodynamics of solids-gas two-phase suspension flow, in which very small solid particles are mixed in a gas flow to enhance the heat transfer characteristics of gas cooled high temperature reactors. Especially, the pressure drop due to friction and the density distribution of solid particles are theoretically analyzed. The friction pressure drop of two-phase flow was analyzed based on the analytical result of the single-phase friction pressure drop. The calculated values of solid/gas friction factor as a function of solid/gas mass loading are compared with experimental results. Comparisons are made for Various combinations of Reynolds number and particle size. As for the particle density distribution, some factors affecting the non-uniformity of distribution were considered. The minimum of energy dispersion was obtained with the variational principle. The suspension density of particles was obtained as a function of relative distance from wall and was compared with experimental results. It is concluded that the distribution is much affected by the particle size and that the smaller particles are apt to gather near the wall. (Aoki, K.)

  17. Materials research for passive solar systems: Solid-state phase-change materials

    Science.gov (United States)

    Benson, D. K.; Webb, J. D.; Burrows, R. W.; McFadden, J. D. O.; Christensen, C.

    1985-03-01

    A set of solid-state phase-change materials is being evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol (C5H12O4), pentaglycerinve (C5H12O3), and neopentyl glycol (C5H12O2). Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature between 25 C and 188 C, and have latent heats of transformation etween 20 and 70 cal/g. Transformation temperatures, specific heats, and latent heats of transformation have been measured for a number of these materials. Limited cyclic experiments suggest that the solid solutions are stable. These phase-change materials exhibit large amounts of undercooling; however, the addition of certain nucleating agents as particulate dispersions in the solid phase-change material greatly reduces this effect. Computer simulations suggest that the use of an optimized solid-state phase-change material in a Trombe wall could provide better performance than a concrete Trombe wall four times thicker and nine times heavier.

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

    Science.gov (United States)

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

    2016-05-01

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

  19. Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

    International Nuclear Information System (INIS)

    Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho

    1991-01-01

    The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing 99m Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

  20. Study on confirmation of Solid-Meal Lag Phase of Gastric Emptying

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Ji Young; Lee, Kyoung Soo; Kim, Chang Guhn; Juhng, Seon Kwan; Won, Jong Jin; Nah, Yong Ho [Wonkwang University School of Medicine, Iksan (Korea, Republic of)

    1991-07-15

    The purpose of this study was to examine the existence of a lag phase of gastric emptying of solid meals. We studied solid phase gastric emptying in 26 normal subject using continuous data acquisition for 30 minutes. Each ingested a 300 g meal containing {sup 99m}Tc-labeled scrambled egg (solid 150 g, milk 150 ml). Lag phase was determined by 1) inspection of the gastric emptying curve 2) time to a 2% decrease in stomach activity 3) the time of visual appearance of duodenal activity on computer image. We concluded that solid meal lag phase exist.

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

    Directory of Open Access Journals (Sweden)

    Wojda Marta

    2014-01-01

    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. A competitive solid-phase radioimmunoassay for quantitation of the major allergen of Parietaria pollen

    International Nuclear Information System (INIS)

    Corbi, A.L.; Ayuso, R.; Lombardero, M.; Duffort, O.; Carreira, J.

    1985-01-01

    A competitive solid-phase radioimmunoassay has been developed for quantitation of the major allergen of Parietaria judaica pollen. The assay is based on: (1) the ability of AC/1.1 monoclonal antibody to bind specifically to the P. judaica major allergen, and (2) the ability of crude pollen extracts or purified allergen to inhibit the binding of 125 I-labelled allergen to solid-phase-bound AC/1.1 monoclonal antibody. The assay is sensitive enough to detect as little as 10 ng of allergen. A good correlation is found when the results obtained are compared with those produced by RAST inhibition (r = 0.95; P < 0.001). Thus, this method can also be used for the estimation of the allergenic activity of P. judaica pollen extracts. The assay is easily completed in 2 h, allowing simultaneous analysis of a number of extracts. (Auth.)

  3. Detection of viral antigens by solid phase radioimmunoassay on polyethylene film

    Energy Technology Data Exchange (ETDEWEB)

    Prokudina, E N; Semenova, N P; Zhdanov, V M

    1986-04-01

    Polyethylene film, without any pretreatment, may serve as a solid phase (SP) for RIA. Viral antigens (HBsAg, and influenza virus) are detected by SP-RIA on the film with a sensitivity of about 2-3 ng/ml or 40-60 pg/assay. The use of polyethylene film allows one to record RIA autographically. The use of micro amounts of reagents and specimens tested is an added advantage. No special equipment is necessary, the method is inexpensive, easy to perform and may be used for mass screening. (Auth.). 7 refs.; 4 figs.

  4. Extração em fase sólida (SPE e micro extração em fase sólida (SPME de piretróides em água Solid-phase extraction (SPE and solid-phase microextraction of pyrethroids in water

    Directory of Open Access Journals (Sweden)

    Wilma Regina Barrionuevo

    2001-04-01

    Full Text Available The pyrethroids bifenthrin, permethrin, cypermethrin and deltamethrin were extracted by solid phase extraction (SPE and solid phase microextraction (SPME. The analysis were performed on a gas chromatograph with electron capture detection (GC-ECD. Octadecil Silano-C18, Florisil and Silica stationary phases were studied for SPE. Better results were obtained for Florisil which gave recoveries from 80% to 108%. Pyrethroids extraction by SPME showed a linear response and a detection limit of 10 pg ml-1. Although the data showed that the two extraction methods were able to isolate the pesticide residues from water samples, the best results were obtained by using SPME which is more sensitive, faster, cheeper, being a more useful technique for the analysis of pyrethroids in drinking water.

  5. Evaluation of natural toxicity on MICROTOX solid-phase test. The pelitic normalization

    International Nuclear Information System (INIS)

    Onorati, F.; Pellegrini, D.; Ausili, A.

    1999-01-01

    In sediment toxicity testing Microtox solid-phase test (SPT) is one of the most used and standardised bioassay. Nevertheless, its real sensitivity and discriminatory power is still unclear, because of several interferences principally related to the matrix composition. Using reference sediments, characterised with chemical and physical analysis, it was possible to find a significant relationship between their natural toxicity and the pelitic fraction that allows to estimate the natural component of the acute toxicity in contaminated samples. This relationship arrows a more sensitive and valid interpretation than raw data and it is used to develop a sediment toxicity index (STI) based on radio to reference (RTR) concept, applicable to harbour contaminated samples [it

  6. Amino-modified diamond as a durable stationary phase for solid-phase extraction.

    Science.gov (United States)

    Saini, Gaurav; Yang, Li; Lee, Milton L; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

    2008-08-15

    We report the formation of a highly stable amino stationary phase on diamond and demonstrate its use in solid-phase extraction (SPE). This process consists of spontaneous and self-limiting adsorption of polyallylamine (PAAm) from aqueous solution onto oxidized diamond. Thermal curing under reduced pressure or chemical cross-linking with a diepoxide was shown to fix the polymer to the particles. The resulting adsorbents are stable under even extreme pH conditions (from at least pH 0-14) and significantly more stable than a commercially available amino SPE adsorbent. Coated diamond particles were characterized by X-ray photoelectron spectroscopy (XPS) and diffuse reflectance Fourier transform-infrared spectroscopy (DRIFT). Model silicon surfaces were characterized by spectroscopic ellipsometry and wetting. Solid-phase extraction was demonstrated using cholesterol, hexadecanedioic acid, and palmitoyloleoylphosphatidylcholine as analytes, and these results were compared to those obtained with commercially available materials. Breakthrough curves indicate that, as expected, porous diamond particles have higher analyte capacity than nonporous solid particles.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1984-05-01

    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. N-Acyliminium Intermediates in Solid-Phase Synthesis

    DEFF Research Database (Denmark)

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

    2010-01-01

    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...

  9. Solid-phase synthesis of molecularly imprinted nanoparticles.

    Science.gov (United States)

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

    2016-03-01

    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.

  10. Phase sensitive multichannel OCT

    International Nuclear Information System (INIS)

    Trasischker, W.

    2015-01-01

    The main aim of this thesis was to develop and improve phase sensitive, multichannel methods for optical coherence tomography (OCT) using light in the 840 nm and 1040 nm regime. Conventional OCT provides purely structural information by illuminating the sample by one beam and recording the backscattered signal with one detection channel. Combination of this approach with a raster scan enables the acquisition of 2D and 3D structural information with a resolution in the micrometer regime. However, sometimes additional image contrast or information is desired. Amongst other approaches, this can be provided by a phase sensitive analysis of the interference pattern. Combining phase sensitivity with the illumination of the sample by more than one beam and/or by recording the data using more than one data acquisition channel allows for even more enhanced imaging. While phase sensitive OCT gives access to additional contrast and information, multichannel OCT can provide higher imaging speed, scan eld size and exible dierential measurements. Amongst the dierential, phase sensitive approaches, Doppler OCT (DOCT) and polarization sensitive OCT (PS-OCT) are two of the most promising OCT modalities. While the former targets information on the movement of backscattering particles, the latter measures alterations of the polarization state of the light induced by the sample. Both techniques provide additional image contrast and are, due to the non-invasive and fast character of OCT, well suited for in vivo imaging of the human eye. In the course of this thesis, two dierent multichannel, phase sensitive OCT systems will be presented. First, a D-OCT system with three dierent sampling beams is described. With a central wavelength of 840 nm these three beams are emitted by three individual laser sources. This eectively eliminates any cross talk and provides the full depth range for each channel. Furthermore, by illuminating the sample from three dierent directions, the absolute

  11. Evaluation of a solid phase R.I.A. technique and solid phase E.L.I.S.A. technique for the demonstration of hepatitis B surface antigen

    International Nuclear Information System (INIS)

    Vranckx, R.; Cole, J.; Peetermans, M.

    1977-01-01

    We compared the sensitivity of a solidphase radio-immunoassay (R.I.A.), a solid-phase enzyme-immunoassay (E.L.I.S.A.) and a hemagglutination test (R.P.H.A.) for the detection of the HBs Ag in two ways: 1) by screening a panel of 300 sera (97 positives and 203 negatives) 2) by titrating serial dilutions of 10 positive sera. Ninety seven sera were positive by R.I.A., 95% were detected by E.L.I.S.A. and 81% were detected by R.P.H.A. In the serial dilutions the average end points of the titration were for R.I.A. 0.005 ng/ml, for E.L.I.S.A. 0,01 ng/ml and for R.P.H.A. 0.04 ng/ml. It can be concluded that the sensitivity of the E.L.I.S.A. test is intermediate between the sensitivity of the R.I.A. and the sensitivity of the R.P.H.A. The E.L.I.S.A. and the R.P.H.A. tests seam to be a little more sensitive for the detection of subtype ay than the detection of subtype ad. (orig.) [de

  12. Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction.

    Science.gov (United States)

    Chen, YiQuan; Cheng, Xian; Mo, Fan; Huang, LiMei; Wu, Zujian; Wu, Yongning; Xu, LiangJun; Fu, FengFu

    2016-04-01

    A simple dispersive solid-phase extraction (DSPE) used to extract and preconcentrate ultra-trace MeHg, EtHg and Hg(2+) from water sample, and a sensitive method for the simultaneous analysis of MeHg, EtHg and Hg(2+) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) with field-amplified sample stacking injection (FASI) were first reported in this study. The DSPE used thiol cotton particles as adsorbent, and is simple and effective. It can be used to extract and preconcentrate ultra-trace mercury compounds in water samples within 30 min with a satisfied recovery and no mercury species alteration during the process. The FASI enhanced the sensitivity of CE-ICP-MS with 25-fold, 29-fold and 27-fold for MeHg, EtHg and Hg(2+) , respectively. Using FASI-CE-ICP-MS together with DSPE, we have successfully determined ultra-trace MeHg, EtHg and Hg(2+) in tap water with a limits of quantification (LOQs) of 0.26-0.45 pg/mL, an RSD (n = 3) mercury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Solid phase extraction membrane

    Science.gov (United States)

    Carlson, Kurt C [Nashville, TN; Langer, Roger L [Hudson, WI

    2002-11-05

    A wet-laid, porous solid phase extraction sheet material that contains both active particles and binder and that possesses excellent wet strength is described. The binder is present in a relatively small amount while the particles are present in a relatively large amount. The sheet material is sufficiently strong and flexible so as to be pleatable so that, for example, it can be used in a cartridge device.

  14. Solid phase syntheses of oligoureas

    Energy Technology Data Exchange (ETDEWEB)

    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)

    1997-02-19

    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.

  15. All solid-state SBS phase conjugate mirror

    Science.gov (United States)

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

    1999-03-09

    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.

  16. Solid-phase radioimmunoassay of immunoglobulins G, A and M: applicability in analysis of sucrose gradients

    Energy Technology Data Exchange (ETDEWEB)

    Eriksen, E F; Danielsen, H [Aarhus Kommunehospital (Denmark). Medical Department C; Johansen, A S [Aarhus Univ. (Denmark). Institute of Medical Biochemistry; Larsson, L I [Unit of Histochemistry, University Institute of Pathology, Copenhagen, Denmark

    1984-01-01

    A simple and sensitive solid-phase radioimmunoassay for the detection of immunoglobulins G, A and M in sucrose gradients is described. The solid-phase consisted of immunoglobulins adsorbed to polystyrene tubes. Using buffers without detergent and /sup 125/I-labeled sheep anti-rabbit IgA as radioligand, the assay was able to detect 0.8 ng per tube in the IgG assay and 1.6 ng per tube in the IgA and IgM assays. Standard curves with antigen dissolved in 10% and 32% sucrose were superimposable and did not deviate from standard curves with antigen dissolved in buffer without sucrose. Using these techniques on ultracentrifugation samples from patients with systemic lupus erythematosus, Schoenlein-Henoch nephritis and IgA glorulonephritis is was possible to detect both immunoglobulin fragments and immunoglobulin aggregates at the same time without prior dialysis of the samples.

  17. Solid-Phase S-Alkylation Promoted by Molecular Sieves.

    Science.gov (United States)

    Calce, Enrica; Leone, Marilisa; Mercurio, Flavia Anna; Monfregola, Luca; De Luca, Stefania

    2015-11-20

    A solid-phase S-alkylation procedure to introduce chemical modification on the cysteine sulfhydryl group of a peptidyl resin is reported. The reaction is promoted by activated molecular sieves and consists of a solid-solid process, since both the catalyst and the substrate are in a solid state. The procedure was revealed to be efficient and versatile, particularly when used in combination with the solution S-alkylation approach, allowing for the introduction of different molecular diversities on the same peptide molecule.

  18. A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium

    International Nuclear Information System (INIS)

    Nakao, Ryuji; Halldin, Christer

    2013-01-01

    A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. Methods: This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Results: Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for 11 C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Conclusion: Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma

  19. Linkage of biomolecules to solid phases for immunoassay

    International Nuclear Information System (INIS)

    Chapman, R.S.

    1998-01-01

    Topics covered by this lecture include a brief review of the principal methods of linkage of biomolecules to solid phase matrices. Copies of the key self explanatory slides are presented as figures together with reprints of two publications by the author dealing with a preferred chemistry for the covalent linkage of antibodies to hydroxyl and amino functional groups and the effects of changes in solid phase matrix and antibody coupling chemistry on the performance of a typical excess reagent immunoassay for thyroid stimulating hormone

  20. Phase diagram of a Lennard-Jones solid

    International Nuclear Information System (INIS)

    Choi, Y.; Ree, T.; Ree, F.H.

    1993-01-01

    A phase diagram of a Lennard-Jones solid at kT/ε≥0.8 is constructed by our recent perturbation theory. It shows the stability of the face-centered-cubic phase except within a small pressure and temperature domain, where the hexagonal-close packed phase may occur. The theory predicts anharmonic contributions to the Helmholtz free energy (important to the crystal stability) in good agreement with Monte Carlo data

  1. Biological treatment of soils contaminated with hydrophobic organics using slurry and solid phase techniques

    International Nuclear Information System (INIS)

    Cassidy, D.P.; Irvine, R.L.

    1995-01-01

    Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurry is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bioslurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay load contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the ate and extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies

  2. MOLECULARLY IMPRINTED SOLID PHASE EXTRACTION FOR TRACE ANALYSIS OF DIAZINON IN DRINKING WATER

    Directory of Open Access Journals (Sweden)

    M. Rahiminejad ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani ، F. Golbabaei

    2009-04-01

    Full Text Available Amongst organophosphate pesticides, the one most widely used and common environmental contaminant is diazinon; thus methods for its trace analysis in environmental samples must be developed. Use of diazinon imprinted polymers such as sorbents in solid phase extraction, is a prominent and novel application area of molecular imprinted polymers. For diazinon extraction, high performance liquid chromatography analysis was demonstrated in this study. During optimization of the molecular imprinted solid phase extraction procedure for efficient solid phase extraction of diazinon, Plackett-Burman design was conducted. Eight experimental factors with critical influence on molecular imprinted solid phase extraction performance were selected, and 12 different experimental runs based on Plackett-Burman design were carried out. The applicability of diazinon imprinted polymers as the sorbent in solid phase extraction, presented obtained good recoveries of diazinon from LC-grade water. An increase in pH caused an increase in the recovery on molecular imprinted solid phase extraction. From these results, the optimal molecular imprinted solid phase extraction procedure was as follows: solid phase extraction packing with 100 mg diazinon imprinted polymers; conditioning with 5 mL of methanol and 6 mL of LC-grade water; sample loading containing diazinon (pH=10; washing with 1 mL of LC-grade water, 1 mL LC- grade water containing 30% acetonitrile and 0.5 mL of acetonitrile, respectively; eluting with 1 mL of methanol containing 2% acetic acid. The percentage recoveries obtained by the optimized molecular imprinted solid phase extraction were more than 90% with drinking water spiked at different trace levels of diazinon. Generally speaking, the molecular imprinted solid phase extraction procedure and subsequent high performance liquid chromatography analysis can be a relatively fast and proper approach for qualitative and quantitative analysis of diazinon in

  3. Phase-field model of vapor-liquid-solid nanowire growth

    Science.gov (United States)

    Wang, Nan; Upmanyu, Moneesh; Karma, Alain

    2018-03-01

    We present a multiphase-field model to describe quantitatively nanowire growth by the vapor-liquid-solid (VLS) process. The free-energy functional of this model depends on three nonconserved order parameters that distinguish the vapor, liquid, and solid phases and describe the energetic properties of various interfaces, including arbitrary forms of anisotropic γ plots for the solid-vapor and solid-liquid interfaces. The evolution equations for those order parameters describe basic kinetic processes including the rapid (quasi-instantaneous) equilibration of the liquid catalyst to a droplet shape with constant mean curvature, the slow incorporation of growth atoms at the droplet surface, and crystallization within the droplet. The standard constraint that the sum of the phase fields equals unity and the conservation of the number of catalyst atoms, which relates the catalyst volume to the concentration of growth atoms inside the droplet, are handled via separate Lagrange multipliers. An analysis of the model is presented that rigorously maps the phase-field equations to a desired set of sharp-interface equations for the evolution of the phase boundaries under the constraint of force balance at three-phase junctions (triple points) given by the Young-Herring relation that includes torque term related to the anisotropy of the solid-liquid and solid-vapor interface excess free energies. Numerical examples of growth in two dimensions are presented for the simplest case of vanishing crystalline anisotropy and the more realistic case of a solid-liquid γ plot with cusped minima corresponding to two sets of (10 ) and (11 ) facets. The simulations reproduce many of the salient features of nanowire growth observed experimentally, including growth normal to the substrate with tapering of the side walls, transitions between different growth orientations, and crawling growth along the substrate. They also reproduce different observed relationships between the nanowire growth

  4. Solid phase microextraction.

    Science.gov (United States)

    Pawliszyn, J

    2001-01-01

    Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

  5. Mesoporous TiO{sub 2} nanoparticles for highly sensitive solid-phase microextraction of organochlorine pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Shuqin; Xie, Lijun; Zheng, Juan; Jiang, Ruifeng; Zhu, Fang; Luan, Tiangang; Ouyang, Gangfeng, E-mail: cesoygf@mail.sysu.edu.cn

    2015-06-09

    Highlights: • Mesoporous TiO{sub 2} nanoparticles were synthesized and characterized. • A novel SPME fiber was fabricated with silicone sealant film and TiO{sub 2} powder. • The fiber exhibited excellent extraction performance to OCPs. • The fiber was used for analysis of OCPs in real water samples. - Abstract: Mesoporous TiO{sub 2} nanoparticles were synthesized with the hydrothermal method and characterized by powder X-ray diffraction (PXRD) and transmission electron microscope (TEM). Then a superior solid-phase microextraction (SPME) fiber was fabricated by sequentially coating the stainless steel fiber with silicone sealant film and mesoporous TiO{sub 2} powder. The developed fiber possessed a homogeneous surface and a long life-span up to 100 times at direct immersing (DI) extraction mode. Under the optimized conditions, the extraction efficiencies of the self-made 17 μm TiO{sub 2} fiber for six organochlorine pesticides (OCPs) were higher than those of the two commercial fibers (65 μm PDMS/DVB and 85 μm PA fibers) which were much thicker than the former. As for analytical performance, low detection limits (0.08–0.60 ng L{sup −1}) and wide linearity (5–5000 ng L{sup −1}) were achieved under the optimal conditions. The repeatabilities (n = 5) for single fiber were between 2.8 and 12.3%, while the reproducibilities (n = 3) of fiber-to-fiber were in the range of 3.7–15.7%. The proposed fiber was successfully applied to the sensitive analysis of OCPs in real water samples and four of the six analytes were detected from the rainwater and the lake water samples.

  6. Direct solid-phase radioimmunoassay for the detection of Aujeszky's disease antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Doeller, G; Jakubik, J

    1980-06-01

    A direct solid-phase radioimmunoassy (dRIA) was developed in order to demonstrate antibodies against Aujeszky's disease virus (ADV) in sera obtained from pigs and rabbits. In the presence of guinea-pig complement the above test is 160-fold to 1500-fold more sensitive than the neutralization test (NT) and 320-fold to 150 000-fold more sensitive than sera obtained from an ADV-infected farm, which were found to be negative in the complement assisted NT. It is possible to test a single dilution of unknown serum by dRIA by comparing same with a standard curve and to make a statement regarding its ADV-specific binding capacity to /sup 125/I-labelled ADV antigen. The advantages of dRIA in comparison to the indirect RIA and the advantages and disadvantages with regard to ELISA were discussed.

  7. Quantitation of complement factor D in human serum by a solid-phase radioimmunoassay

    Energy Technology Data Exchange (ETDEWEB)

    Barnum, S R; Niemann, M A; Kearney, J F; Volanakis, J E [Alabama Univ., Birmingham (USA)

    1984-03-16

    A sensitive solid-phase radioimmunoassay is described which quantitates human D to 1-2 ng/ml. The assay was used to measure the concentration of D in normal and acute-phase sera and sera from individuals with systemic lupus erythematosus. All 3 groups of sera had comparable levels of D with mean values of 1.8, 2.3 and 2.5 ..mu..g/ml, respectively. Also tested were sera decomplemented in vitro by activators of the classical and alternative pathways. The results indicated that D is not depleted by alternative or classical pathway activation. However, heat inactivation (56/sup 0/C, 30 min) of serum resulted in almost complete loss of antigenic D.

  8. Phase-sensitive optical processing in silicon waveguides

    DEFF Research Database (Denmark)

    Petermann, Klaus; Gajda, A.; Dziallas, Claudia

    2015-01-01

    Parametric optical signal processing is reviewed for silicon nano-rib-waveguides with a reverse-biased pin-junction. Phase-sensitive parametric amplification with a phase-sensitive extinction of more than 20 dB has been utilized for the regeneration of DPSK signals...

  9. Solid-phase immunoradiometric assay for serum amyloid A protein using magnetisable cellulose particles

    International Nuclear Information System (INIS)

    De Beer, F.C.; Dyck, R.F.; Pepys, M.B.

    1982-01-01

    An immunoradiometric assay for human serum amyloid A protein (SAA) was developed using magnetisable cellulose particles as the solid phase. Rabbit antiserum to SAA was raised by immunization with SAA isolated from acute-phase serum by gel filtration in formic acid. The antiserum was rendered monospecific for SAA by solid-phase immunoabsorption with normal human serum, which contains only traces of SAA, and some was coupled covalently to the cellulose particles. Immunopurified anti-SAA antibodies were isolated from the monospecific anti-SAA serum by binding to, and elution from insolubilized acute-phase serum and were radiolabelled with 125 I. The assay was calibrated with an acute phase serum which contained 6000 times more SAA than normal sera with the lowest detectable level of SAA, and an arbitrary value of 6000 U/l was assigned to this standard. Sera were tested in the native, undenatured state and there was no increase in SAA immunoreactivity following alkali treatment or heating. The assay range was from 1-2000 U/l so that all SAA levels above 6 U/l could be measured on a single (1:6) dilution of serum. The intra- and interassay coefficients of variation were 11.7 and 15.0% respectively. Among 100 healthy normal subjects (50 male, 50 female) the median SAA level was 9 U/l, range <1-100, with 93% below 20 U/l and only 2% below the lower limit of sensitivity of the assay (1 U/l). (Auth.)

  10. Phase Noise Tolerant QPSK Receiver Using Phase Sensitive Wavelength Conversion

    DEFF Research Database (Denmark)

    Da Ros, Francesco; Xu, Jing; Lei, Lei

    2013-01-01

    A novel QPSK receiver based on a phase noise reduction pre-stage exploiting PSA in a HNLF and balanced detection is presented. Receiver sensitivity improvement over a conventional balanced receiver is demonstrated.......A novel QPSK receiver based on a phase noise reduction pre-stage exploiting PSA in a HNLF and balanced detection is presented. Receiver sensitivity improvement over a conventional balanced receiver is demonstrated....

  11. Finite-deformation phase-field chemomechanics for multiphase, multicomponent solids

    Science.gov (United States)

    Svendsen, Bob; Shanthraj, Pratheek; Raabe, Dierk

    2018-03-01

    The purpose of this work is the development of a framework for the formulation of geometrically non-linear inelastic chemomechanical models for a mixture of multiple chemical components diffusing among multiple transforming solid phases. The focus here is on general model formulation. No specific model or application is pursued in this work. To this end, basic balance and constitutive relations from non-equilibrium thermodynamics and continuum mixture theory are combined with a phase-field-based description of multicomponent solid phases and their interfaces. Solid phase modeling is based in particular on a chemomechanical free energy and stress relaxation via the evolution of phase-specific concentration fields, order-parameter fields (e.g., related to chemical ordering, structural ordering, or defects), and local internal variables. At the mixture level, differences or contrasts in phase composition and phase local deformation in phase interface regions are treated as mixture internal variables. In this context, various phase interface models are considered. In the equilibrium limit, phase contrasts in composition and local deformation in the phase interface region are determined via bulk energy minimization. On the chemical side, the equilibrium limit of the current model formulation reduces to a multicomponent, multiphase, generalization of existing two-phase binary alloy interface equilibrium conditions (e.g., KKS). On the mechanical side, the equilibrium limit of one interface model considered represents a multiphase generalization of Reuss-Sachs conditions from mechanical homogenization theory. Analogously, other interface models considered represent generalizations of interface equilibrium conditions consistent with laminate and sharp-interface theory. In the last part of the work, selected existing models are formulated within the current framework as special cases and discussed in detail.

  12. Analysis of microcontaminants in aqueous samples by fully automated on-line solid-phase extraction-gas chromatography-mass selective detection.

    NARCIS (Netherlands)

    Louter, A.J.H.; van Beekvelt, C.A.; Cid Montanes, P.; Slobodník, J.; Vreuls, J.J.; Brinkman, U.A.T.

    1996-01-01

    The trace-level analysis of unknown organic pollutants in water requires the use of fast and sensitive methods which also provide structural information. In the present study, an on-line technique was used which combines sample preparation by means of solid-phase extraction (SPE) on a small

  13. Biogasification of solid wastes by two-phase anaerobic fermentation

    International Nuclear Information System (INIS)

    Ghosh, S.; Vieitez, E.R.; Liu, T.; Kato, Y.

    1997-01-01

    Municipal, industrial and agricultural solid wastes, and biomass deposits, cause large-scale pollution of land and water. Gaseous products of waste decomposition pollute the air and contribute to global warming. This paper describes the development of a two-phase fermentation system that alleviates methanogenic inhibition encountered with high-solids feed, accelerates methane fermentation of the solid bed, and captures methane (renewable energy) for captive use to reduce global warming. The innovative system consisted of a solid bed reactor packed with simulated solid waste at a density of 160 kg/m 3 and operated with recirculation of the percolated culture (bioleachate) through the bed. A rapid onset of solids hydrolysis, acidification, denitrification and hydrogen gas formation was observed under these operating conditions. However, these fermentative reactions stopped at a total fatty acids concentration of 13,000 mg/l (as acetic) at pH 5, with a reactor head-gas composition of 75 percent carbon dioxide, 20 percent nitrogen, 2 percent hydrogen and 3 percent methane. Fermentation inhibition was alleviated by moving the bioleachate to a separate methane-phase fermenter, and recycling methanogenic effluents at pH 7 to the solid bed. Coupled operation of the two reactors promoted methanogenic conversion of the high-solids feed. (author)

  14. Phase Sensitive Amplification using Parametric Processes in Optical Fibers

    DEFF Research Database (Denmark)

    Kang, Ning

    . Further, phase sensitive parametric processes in a nano-engineered silicon waveguide have been measured experimentally for the first time. Numerical optimizations show that with reduced waveguide propagation loss and reduced carrier life time, larger signal phase sensitive extinction ratio is achievable......Phase sensitive amplification using the parametric processes in fiber has the potential of delivering high gain and broadband operation with ultralow noise. It is able to regenerate both amplitude and phase modulated signals, simultaneously, with the appropriate design. This thesis concerns...... types. The regeneration capability of PSAs on phase encoded signal in an optical link has been optimized. Flat-top phase sensitive profile has been synthesized. It is able to provide simultaneous amplitude and phase noise squeezing, with enhanced phase noise margin compared to conventional designs...

  15. solid phase extraction method for selective determination

    African Journals Online (AJOL)

    FATOKI

    determination of phthalate ester plasticizers in rivers and marine water samples. Of the ... samples that receive effluent from industries that use phthalate esters. ... Keywords Phthalates, Plasticizers, Solid Phase Gas Chromatography.

  16. Biological treatment of soils contaminated with hydrophobic organics using slurry- and solid-phase techniques

    Science.gov (United States)

    Cassidy, Daniel H.; Irvine, Robert L.

    1995-10-01

    Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurrying is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bio-slurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay loam contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the rate an extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies. Results showed that slurrying for 1.5 hours at a water content less than saturation markedly increased the rate and extent of contaminant biodegradation in the solid phase bioreactors compared with soil having no slurry pretreatment. Slurrying the soil at or above its saturation moisture content resulted in lengthy dewatering times which prohibited aeration, thereby delaying the onset of biological treatment in the solid phase bioreactors. Results also showed that properly operated periodic aeration can provide less volatile contaminant removal and a grater fraction of biological contaminant removal than continuous aeration.

  17. The Pictet-Spengler reaction in solid-phase combinatorial chemistry

    DEFF Research Database (Denmark)

    Nielsen, Thomas E; Diness, Frederik; Meldal, Morten

    2003-01-01

    The Pictet-Spengler reaction is an important reaction for the generation of tetrahydro-beta-carbolines and tetrahydroisoquinoline ring systems, which exhibit a range of biological and pharmacological properties. This review covers the solid-phase Pictet-Spengler reaction, as employed in solid...

  18. Phase 2, Solid waste retrieval strategy

    International Nuclear Information System (INIS)

    Johnson, D.M.

    1994-01-01

    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

  19. Phase 2, Solid waste retrieval strategy

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, D.M.

    1994-09-29

    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.

  20. [Simultaneous determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography].

    Science.gov (United States)

    Liu, Min; Li, Xiaolin; Bie, Wei; Wang, Minglin; Feng, Qian

    2011-02-01

    A new method was established for the determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol-water (1:1, v/v) and purified by a solid phase extraction column. Then, the chromatographic separation was achieved on a Luna C18 column by linear gradient elution. The mobile phase was 10 mmol/L ammonium acetate-acetonitrile (containing 1% acetic acid). The results showed that the 15 industrial synthetic dyes can be separated efficiently. The recoveries of the 15 industrial synthetic dyes spiked in condiment were between 84.6% and 114.2% with the relative standard deviations of 0.9% - 10.3%. The limits of detection of this method was 0.05 - 0.18 mg/kg for the 15 industrial synthetic dyes. The method is simple, sensitive, accurate, repeatable and can be used for simultaneous determination of the 15 illegally added industrial synthetic dyes.

  1. Negligible depletion solid-phase microextraction with radiolabeled analytes to study free concentrations and protein binding : an example with [3H]Estradiol

    NARCIS (Netherlands)

    Heringa, M.B.; Pastor, D.; Algra, J.; Vaes, W.H.J.; Hemmens, J.L.M.

    2002-01-01

    A new method is presented that enables sensitive measurement of free concentrations of radiolabeled ligands. Additionally, protein binding of radiochemicals in complex matrixes can be determined with this new technique that combines negligible depletion solid-phase microextraction (nd-SPME) with

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

    Science.gov (United States)

    Faccenda, Manuele; Dal Zilio, Luca

    2017-01-01

    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

  3. Phase transitions in solids under high pressure

    CERN Document Server

    Blank, Vladimir Davydovich

    2013-01-01

    Phase equilibria and kinetics of phase transformations under high pressureEquipment and methods for the study of phase transformations in solids at high pressuresPhase transformations of carbon and boron nitride at high pressure and deformation under pressurePhase transitions in Si and Ge at high pressure and deformation under pressurePolymorphic α-ω transformation in titanium, zirconium and zirconium-titanium alloys Phase transformations in iron and its alloys at high pressure Phase transformations in gallium and ceriumOn the possible polymorphic transformations in transition metals under pressurePressure-induced polymorphic transformations in АIBVII compoundsPhase transformations in AIIBVI and AIIIBV semiconductor compoundsEffect of pressure on the kinetics of phase transformations in iron alloysTransformations during deformation at high pressure Effects due to phase transformations at high pressureKinetics and hysteresis in high-temperature polymorphic transformations under pressureHysteresis and kineti...

  4. Solid Phase Extraction and Spectrophotometric Determination of ...

    African Journals Online (AJOL)

    NJD

    2005-04-15

    Apr 15, 2005 ... to the economy and has significant industrial applications. The development of a ... Waters Solid Phase Extraction (SPE) device (the device can carry out twenty ... HPLC grade dimethyl formamide (DMF) (Fisher. Corporation ...

  5. Pressure Effects on Solid State Phase Transformation of Aluminium Bronze in Cooling Process

    International Nuclear Information System (INIS)

    Hai-Yan, Wang; Jian-Hua, Liu; Gui-Rong, Peng; Yan, Chen; Yu-Wen, Liu; Fei, Li; Wen-Kui, Wang

    2009-01-01

    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

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

    African Journals Online (AJOL)

    All rights reserved. ... 1Department of Pharmacology, 2Department of Applied Science, 3Police Forensic Science Center 10, Yala 95000, 4Natural ... Purpose: To develop a solid phase extraction (SPE) method that utilizes reverse-phase high.

  7. A multi-phase equation of state for solid and liquid lead

    International Nuclear Information System (INIS)

    Robinson, C.M.

    2004-01-01

    This paper considers a multi-phase equation of state for solid and liquid lead. The thermodynamically consistent equation of state is constructed by calculating separate equations of state for the solid and liquid phases. The melt curve is the curve in the pressure, temperature plane where the Gibb's free energy of the solid and liquid phases are equal. In each phase a complete equation of state is obtained using the assumptions that the specific heat capacity is constant and that the Grueneisen parameter is proportional to the specific volume. The parameters for the equation of state are obtained from experimental data. In particular they are chosen to match melt curve and principal Hugoniot data. Predictions are made for the shock pressure required for melt to occur on shock and release

  8. KAJIAN ADSORPSI ION LOGAM Cr(VI OLEH ADSORBEN KOMBINASI ARANG AKTIF SEKAM PADI DAN ZEOLIT MENGGUNAKAN METODE SOLID-PHASE SPECTROPHOTOMETRY (SPS

    Directory of Open Access Journals (Sweden)

    Sulistyo Saputro

    2016-10-01

      This study aims to study the use of activated rice husk charcoal and zeolite as combination adsorbents to adsorb Cr(VI metal ions; the effect of the combination adsorbents of activated rice husk charcoal and zeolite’s compositions to adsorb Cr(VI metal ions; and the sensitivity of solid-phase spectrophotometry (SPS as a method to determine the reduced levels of Cr(VI metal ions in the level of 15μ"> g/L. The activated rice husk charcoal used were obtained through the activation process by soaking in a solution of ZnCl2 10% while the zeolite with a solution of H2SO4 10%. The contacting process of the adsorbents with Cr(VI metal ions was done by varying the compositions of the activated rice husk charcoal and zeolite adsorbent, 1:1, 1:2, 1:3, and 2:1. The data analysis of the Cr(VI level used solid-phase spectrophotometry (SPS method. Characterization of activated rice husk charcoal and zeolite used FTIR. The results showed that: (1 a combination of activated rice husk charcoal and zeolite can be used as adsorbent to adsorb Cr(VI metal ions with the adsorption capacity was 0,28 15μ"> g/g; (2 the optimum composition of adsorbents was 1:2 with the percentage of absorption was 40,99%; (3 solid-phase spectrophotometry (SPS is a sensitive method to determine the reduced levels of Cr(VI in the level of 15μ"> g/L with the limit of detection (LOD was 0,021 15μ"> g/L.   Keywords: adsorption, Cr(VI,  activated  rice husk charcoal,  zeolite, solid-phase spectrophotometry

  9. Solid-phase equilibria on Pluto's surface

    Science.gov (United States)

    Tan, Sugata P.; Kargel, Jeffrey S.

    2018-03-01

    Pluto's surface is covered by volatile ices that are in equilibrium with the atmosphere. Multicomponent phase equilibria may be calculated using a thermodynamic equation of state and, without additional assumptions, result in methane-rich and nitrogen-rich solid phases. The former is formed at temperature range between the atmospheric pressure-dependent sublimation and condensation points, while the latter is formed at temperatures lower than the sublimation point. The results, calculated for the observed 11 μbar atmospheric pressure and composition, are consistent with recent work derived from observations by New Horizons.

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

    DEFF Research Database (Denmark)

    Nielsen, Thomas Eiland

    2009-01-01

    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...... with significant structural complexity and diversity. This review describes some of the most systematic solid-phase approaches that are potentially suited for pharmaceutical applications, that is, the methods described are useful for the synthesis of compound collections, and exhibit tunable stereochemistry...

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

    Science.gov (United States)

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

    2017-06-01

    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 CH 4 kgVS fed -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.

  12. On the study of the solid-solid phase transformation of TlBiTe2

    International Nuclear Information System (INIS)

    Chrissafis, K.; Vinga, E.S.; Paraskevopoulos, K.M.; Polychroniadis, E.K.

    2003-01-01

    The narrow gap semiconductor TlBiTe 2 undergoes a solid-solid phase transformation from the rhombohedral (D 3d ) to the cubic (O h ) phase. The present paper deals with the study of this phase transformation combining the results of Differential Scanning Calorimetry (DSC) and Transmission Electron Microscopy (TEM). It has been found that during heating the transformation is an athermal activated process, which can be described only by a combination of more than one processes while during cooling it exhibits an expectable thermal hysteresis due to the volume difference. The results of the kinetic analysis combined with the electron microscopy findings, supported also by the Fourier Transform Infrared (FTIR) spectroscopy ones, lead to the conclusion that TlBiTe 2 undergoes a multiple-step, displacive, martensitic type transformation. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

  13. SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE ...

    African Journals Online (AJOL)

    SOLID-PHASE PEPTIDE SYNTHESIS OF ISOTOCIN WITH AMIDE OF ASPARAGINE PROTECTED WITH 1-TETRALINYL. TRIFLUOROMETHANESULPHONIC ACID (TFMSA) DEPROTECTION, CLEAVAGE AND AIR OXIDATION OF MERCAPTO GROUPS TO DISULPHIDE.

  14. Solid-State NMR Investigation of Drug-Excipient Interactions and Phase Behavior in Indomethacin-Eudragit E Amorphous Solid Dispersions.

    Science.gov (United States)

    Lubach, Joseph W; Hau, Jonathan

    2018-02-20

    To investigate the nature of drug-excipient interactions between indomethacin (IMC) and methacrylate copolymer Eudragit® E (EE) in the amorphous state, and evaluate the effects on formulation and stability of these amorphous systems. Amorphous solid dispersions containing IMC and EE were spray dried with drug loadings from 20% to 90%. PXRD was used to confirm the amorphous nature of the dispersions, and DSC was used to measure glass transition temperatures (T g ). 13 C and 15 N solid-state NMR was utilized to investigate changes in local structure and protonation state, while 1 H T 1 and T 1ρ relaxation measurements were used to probe miscibility and phase behavior of the dispersions. T g values for IMC-EE solid dispersions showed significant positive deviations from predicted values in the drug loading range of 40-90%, indicating a relatively strong drug-excipient interaction. 15 N solid-state NMR exhibited a change in protonation state of the EE basic amine, with two distinct populations for the EE amine at -360.7 ppm (unprotonated) and -344.4 ppm (protonated). Additionally, 1 H relaxation measurements showed phase separation at high drug load, indicating an amorphous ionic complex and free IMC-rich phase. PXRD data showed all ASDs up to 90% drug load remained physically stable after 2 years. 15 N solid-state NMR experiments show a change in protonation state of EE, indicating that an ionic complex indeed forms between IMC and EE in amorphous solid dispersions. Phase behavior was determined to exhibit nanoscale phase separation at high drug load between the amorphous ionic complex and excess free IMC.

  15. Bioinspired magnetite synthesis via solid precursor phases

    NARCIS (Netherlands)

    Lenders, J.J.M.; Mirabello, G.; Sommerdijk, N.A.J.M.

    2016-01-01

    Living organisms often exploit solid but poorly ordered mineral phases as precursors in the biomineralization of their inorganic body parts. Generally speaking, such precursor-based approaches allow the organisms-without the need of high supersaturation levels-to accumulate significant quantities of

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

    Science.gov (United States)

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

    2014-11-01

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

  17. Sensitive beam-bunch phase detector

    Energy Technology Data Exchange (ETDEWEB)

    Takeuchi, S; Shepard, K W

    1984-11-15

    A sensitive heavy-ion beam-bunch phase detector has been developed by first examining the relationship between the sensitivity of an rf resonant cavity as a particle bunch detector and the shunt impedance of the same cavity as an accelerating structure. Then the various high shunt impedance rf cavities previously developed for accelerating heavy ions were evaluated for use as bunch detectors. A spiral-loaded geometry was chosen, built, and tested with beam. The sensitivity obtained, 14 V per electrical nA of beam, is a factor 3 higher than previously reported. (orig.).

  18. Sensitive beam-bunch phase detector

    Energy Technology Data Exchange (ETDEWEB)

    Takeuchi, S; Shepard, K W [Argonne National Lab., IL (USA). Physics Div.

    1984-11-15

    A sensitive heavy-ion beam-bunch phase detector has been developed by first examining the relationship between the sensitivity of an RF resonant cavity as a particle bunch detector and the shunt impedance of the same cavity as an accelerating structure. Then the various high shunt impedance RF cavities previously developed for accelerating heavy ions were evaluated for use as bunch detectors. A spiral-loaded geometry was chosen, built, and tested with beam. The sensitivity obtained, 14 ..mu.. V per electrical nA of beam, is a factor 3 higher than previously reported.

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

    OpenAIRE

    Matovic, M.

    2007-01-01

    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. For a proper description of the crystallization process the equilibrium approach is insufficient and a kinetic approach is actually required. In this work, we show that during slow crystallizatio...

  20. Solid-phase route to Fmoc-protected cationic amino acid building blocks

    DEFF Research Database (Denmark)

    Clausen, Jacob Dahlqvist; Linderoth, Lars; Nielsen, Hanne Mørck

    2012-01-01

    Diamino acids are commonly found in bioactive compounds, yet only few are commercially available as building blocks for solid-phase peptide synthesis. In the present work a convenient, inexpensive route to multiple-charged amino acid building blocks with varying degree of hydrophobicity...... was developed. A versatile solid-phase protocol leading to selectively protected amino alcohol intermediates was followed by oxidation to yield the desired di- or polycationic amino acid building blocks in gram-scale amounts. The synthetic sequence comprises loading of (S)-1-(p-nosyl)aziridine-2-methanol onto...... of simple neutral amino acids as well as analogs displaying high bulkiness or polycationic side chains was prepared. Two building blocks were incorporated into peptide sequences using microwave-assisted solid-phase peptide synthesis confirming their general utility....

  1. Unitized solid phase immunoassay kit and method

    International Nuclear Information System (INIS)

    1975-01-01

    A unitized solid phase kit for radioimmunoassay is disclosed. All of the necessary assay reagents are incorporated into a single tube wherein all phases of the assay procedure are performed, requiring only the addition of the patient's sample. Antibody is bound to the tube surface while labelled antigen is also present but unbound. Storage in the absence of air and water results in the stabilization of the reagents such that the system can be stored for long periods

  2. A novel hybrid metal-organic framework-polymeric monolith for solid-phase microextraction.

    Science.gov (United States)

    Lin, Chen-Lan; Lirio, Stephen; Chen, Ya-Ting; Lin, Chia-Her; Huang, Hsi-Ya

    2014-03-17

    This study describes the fabrication of a novel hybrid metal-organic framework- organic polymer (MOF-polymer) for use as a stationary phase in fritless solid-phase microextraction (SPME) for validating analytical methods. The MOF-polymer was prepared by using ethylene dimethacrylate (EDMA), butyl methacrylate (BMA), and an imidazolium-based ionic liquid as porogenic solvent followed by microwave-assisted polymerization with the addition of 25 % MOF. This novel hybrid MOF-polymer was used to extract penicillin (penicillin G, penicillin V, oxacillin, cloxacillin, nafcillin, dicloxacillin) under different conditions. Quantitative analysis of the extracted penicillin samples using the MOF-organic polymer for SPME was conducted by using capillary electrochromatography (CEC) coupled with UV analysis. The penicillin recovery was 63-96.2 % with high reproducibility, sensitivity, and reusability. The extraction time with the proposed fabricated SPME was only 34 min. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Solid-phase microextraction

    DEFF Research Database (Denmark)

    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...... of SPME were examined for halogenated and non-halogenated volatile hydrocarbons, and a standard method for their quantitative analysis in aqueous samples was developed and validated in inter-laboratory studies on the basis of reference material and in comparison with the traditional methods....... The influences of some possible interferences on the SPME process were examined, and new SPME probes were tested for the in situ monitoring of groundwater pollutants. Inter-laboratory studies were carried out also for the validation of SPME for the quantitative analysis of organochlorine, organonitrogen...

  4. Phase segregation in cerium-lanthanum solid solutions

    NARCIS (Netherlands)

    Belliere, V.; Joorst, G; Stephan, O; de Groot, FMF; Weckhuysen, BM

    2006-01-01

    Electron energy-loss spectroscopy (EELS) in combination with scanning transmission electron microscopy ( STEM) reveals that the La enrichment at the surface of cerium-lanthanum solid solutions is an averaged effect and that segregation occurs in a mixed oxide phase. This separation occurs within a

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

    DEFF Research Database (Denmark)

    Baatrup, G; Jonsson, H; Sjöholm, A

    1988-01-01

    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...

  6. Biological nitrate removal from water and wastewater by solid-phase denitrification process.

    Science.gov (United States)

    Wang, Jianlong; Chu, Libing

    2016-11-01

    Nitrate pollution in receiving waters has become a serious issue worldwide. Solid-phase denitrification process is an emerging technology, which has received increasing attention in recent years. It uses biodegradable polymers as both the carbon source and biofilm carrier for denitrifying microorganisms. A vast array of natural and synthetic biopolymers, including woodchips, sawdust, straw, cotton, maize cobs, seaweed, bark, polyhydroxyalkanoate (PHA), polycaprolactone (PCL), polybutylene succinate (PBS) and polylactic acid (PLA), have been widely used for denitrification due to their good performance, low cost and large available quantities. This paper presents an overview on the application of solid-phase denitrification in nitrate removal from drinking water, groundwater, aquaculture wastewater, the secondary effluent and wastewater with low C/N ratio. The types of solid carbon source, the influencing factors, the microbial community of biofilm attached on the biodegradable carriers, the potential adverse effect, and the cost of denitrification process are introduced and evaluated. Woodchips and polycaprolactone are the popular and competitive natural plant-like and synthetic biodegradable polymers used for denitrification, respectively. Most of the denitrifiers reported in solid-phase denitrification affiliated to the family Comamonadaceae in the class Betaproteobacteria. The members of genera Diaphorobacter, Acidovorax and Simplicispira were mostly reported. In future study, more attention should be paid to the simultaneous removal of nitrate and toxic organic contaminants such as pesticide and PPCPs by solid-phase denitrification, to the elucidation of the metabolic and regulatory relationship between decomposition of solid carbon source and denitrification, and to the post-treatment of the municipal secondary effluent. Solid-phase denitrification process is a promising technology for the removal of nitrate from water and wastewater. Copyright © 2016

  7. Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

    International Nuclear Information System (INIS)

    Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

    2004-01-01

    A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

  8. Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

    Science.gov (United States)

    Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

    2018-01-26

    The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Solid-solid synthesis and structural phase transition process of SmF3

    Science.gov (United States)

    Yan, Qi-Cao; Guo, Xing-Min

    2018-04-01

    Mazes of contradictory conclusions have been obtained by previous researches about structural phase transition process of SmF3. In this paper, the single crystals of SmF3 (hexagonal and orthorhombic) were prepared by solid-solid synthesis, which have shown gradual changes in crystal growth modes with the increase temperature and holding time. Furthermore, we propose the phase transition process of in SmF3. Hexagonal symmetry of SmF3 (space group Pnma) was prepared firstly by heating Sm2O3 and NH4HF2 over 40 min at 270 °C. And then orthorhombic symmetry of SmF3 (space group P63mc) was obtained by heating hexagonal symmetry over 10 h at 650 °C. The reaction of SmF3 (hexagonal) = SmF3 (orthorhombic) is extremely sluggish at a low temperature (less than 650 °C), which was seen as a Mixed Grown Region.

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

    Science.gov (United States)

    Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele

    2014-07-07

    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.

  11. Solid-phase microextraction for bioconcentration studies according to OECD TG 305

    Energy Technology Data Exchange (ETDEWEB)

    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)

    2012-12-15

    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.)

  12. Simulating Solid-Solid Phase Transition in Shape-Memory Alloy Microstructure by Face-Offsetting Method

    International Nuclear Information System (INIS)

    Bellur Ramaswamy, Ravi S.; Tortorelli, Daniel A.; Fried, Eliot; Jiao Xiangmin

    2008-01-01

    Advances in the understanding of martensitic transformations (diffusionless, solid-solid phase transformations) have been instrumental to the recent discovery of new low hysteresis alloys. However, some key fundamental issues must be better understood to design still better alloys. Restricting attention to antiplane shear, we use finite element analysis to model the shape-memory alloy microstructure within the Abeyaratne-Knowles continuum thermomechanical framework and use an interface kinetic relation of the kind proposed by Rosakis and Tsai. Geometric singularities and topological changes associated with microstructural evolution pose significant numerical challenges. We address such challenges with a recently developed front-tracking scheme called the face-offsetting method (FOM) to explicitly model phase interfaces. Initial results demonstrate the effectiveness of FOM in resolving needle-like twinned microstructures

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

    Science.gov (United States)

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

    2017-03-01

    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 (C 18 ) 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.

  14. Solid phase radioimmunoassays using labelled antibodies: a conceptual framework for designing assays

    International Nuclear Information System (INIS)

    Kalmakoff, J.; Parkinson, A.J.; Crawford, A.M.; Williams, B.R.G.

    1977-01-01

    A simple theoretical model for the antigen-antibody reaction is presented and used to evaluate the optimum conditions for designing solid phase radioimmunoassays (RIA) using labelled antibodies. Both theoretical and experimental data are presented, using a wide variety of antigens and their corresponding antibodies. The types of RIA described include the direct, the indirect, the direct sandwich assays for detecting either antigen or antibody. The experimental results confirm in a semiquantitative manner that the greatest sensitivity of the RIA is achieved when the smallest amount of labelled antibody is used, that whenever possible the antigen/antibody ratio should be greater than unity(>1), and that the formation of the antigen-antibody complex is dependent on the mass action effect

  15. C18, C8, and perfluoro reversed phases on diamond for solid-phase extraction.

    Science.gov (United States)

    Saini, Gaurav; Wiest, Landon A; Herbert, David; Biggs, Katherine N; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

    2009-04-17

    In spite of advances in solid-phase extraction (SPE) technology there are certain disadvantages to current SPE silica-based, column packings. The pH range over which extraction can occur is limited and each column is generally only used once. New diamond-based reversed SPE phases (C(18), C(8), and perfluorinated) were developed in our laboratories. Studies were done which show that these phases do not have the same limitations as traditional silica-based stationary phases. The synthesis and properties of these diamond-based phases are presented, and the stability, percent recovery, and column capacity are given for the C(18) phase.

  16. Influence of Calcium on Microbial Reduction of Solid Phase Uranium (VI)

    International Nuclear Information System (INIS)

    Liu, Chongxuan; Jeon, Byong-Hun; Zachara, John M.; Wang, Zheming

    2007-01-01

    The effect of calcium on microbial reduction of a solid phase U(VI), sodium boltwoodite (NaUO2SiO3OH · 1.5H2O), was evaluated in a culture of a dissimilatory metal-reducing bacterium (DMRB), Shewanella oneidensis strain MR-1. Batch experiments were performed in a non-growth bicarbonate medium with lactate as electron donor at pH 7 buffered with PIPES. Calcium increased both the rate and extent of Na-boltwoodite dissolution by increasing its solubility through the formation of a ternary aqueous calcium-uranyl-carbonate species. The ternary species, however, decreased the rates of microbial reduction of aqueous U(VI). Laser-induced fluorescence spectroscopy (LIFS) and transmission electron microscopy (TEM) revealed that microbial reduction of solid phase U(VI) is a sequentially coupled process of Na-boltwoodite dissolution, U(VI) aqueous speciation, and microbial reduction of dissolved U(VI) to U(IV) that accumulated on bacterial surfaces/periplasm. The overall rates of microbial reduction of solid phase U(VI) can be described by the coupled rates of dissolution and microbial reduction that were both influenced by calcium. The results demonstrated that dissolved U(VI) concentration during microbial reduction was a complex function of solid phase U(VI) dissolution kinetics, aqueous U(VI) speciation, and microbial activity

  17. A solid phase radioimmunoassay for free triiodothyronine in serum: assay development and validation

    International Nuclear Information System (INIS)

    Liu Fangyan; Zhou Meiying; Yin Linxiang; Yang Jianzhong; Hua Chenglin

    1999-01-01

    A solid phase radioimmunoassay for free triiodothyronine in serum was developed based on double-antibody coated tubes. The method was turned out to be reliable with good reproducibility, higher sensitivity and easy performance. The measurable range of FT 3 in serum was 1.2 to 38 pmol/L. The mean coefficients of variation within and between assays were 1.79%∼3.18% and 4.72%∼9.31%, respectively. The FT 3 concentrations in euthyroid serum as determined by this method were 2.8 to 7.8 pmol/L. The FT 3 values determined by this new method correlated well with those measured by a commercial radioimmunoassay (r = 0.853)

  18. Solid phase tube radioimmunoassay for digoxin detection

    International Nuclear Information System (INIS)

    Stellner, K.; Glatz, C.; Linke, R.

    1975-01-01

    A solid phase radioimmunoassay with 125 I is described for cardiac patients. The test for the digoxin determination and the poisoning due to cardiac glycosides can be measured very accurately and carried out easily. In addition, the test determination can be automatically performed in connection with other tests. (GSE/LH) [de

  19. Solid state photon upconversion utilizing thermally activated delayed fluorescence molecules as triplet sensitizer

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Tony C.; Congreve, Daniel N.; Baldo, Marc A., E-mail: baldo@mit.edu [Department of Electrical Engineering and Computer Science, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States)

    2015-07-20

    The ability to upconvert light is useful for a range of applications, from biological imaging to solar cells. But modern technologies have struggled to upconvert incoherent incident light at low intensities. Here, we report solid state photon upconversion employing triplet-triplet exciton annihilation in an organic semiconductor, sensitized by a thermally activated-delayed fluorescence (TADF) dye. Compared to conventional phosphorescent sensitizers, the TADF dye maximizes the wavelength shift in upconversion due to its small singlet-triplet splitting. The efficiency of energy transfer from the TADF dye is 9.1%, and the conversion yield of sensitizer exciton pairs to singlet excitons in the annihilator is 1.1%. Our results demonstrate upconversion in solid state geometries and with non-heavy metal-based sensitizer materials.

  20. Experimental (solid + liquid) or (liquid + liquid) phase equilibria of (amine + nitrile) binary mixtures

    International Nuclear Information System (INIS)

    Domanska, Urszula; Marciniak, Malgorzata

    2007-01-01

    (Solid + liquid) phase diagrams have been determined for (hexylamine, or octylamine, or 1,3-diaminopropane + acetonitrile) mixtures. Simple eutectic systems have been observed in these mixtures. (Liquid + liquid) phase diagrams have been determined for (octylamine, or decylamine + propanenitrile, or + butanenitrile) mixtures. Mixtures with propanenitrile and butanenitrile show immiscibility in the liquid phase with an upper critical solution temperature, UCST. (Solid + liquid) phase diagrams have been correlated using NRTL, NRTL 1, Wilson and UNIQUAC equations. (Liquid + liquid) phase diagrams have been correlated using NRTL equation

  1. Sequential, solid-phase assay for biotin in physiologic fluids that correlates with expected biotin status

    International Nuclear Information System (INIS)

    Mock, D.M.; DuBois, D.B.

    1986-01-01

    Interest in accurate measurement of biotin concentrations in plasma and urine has been stimulated by recent advances in the understanding of biotin-responsive inborn errors of metabolism and by several reports describing acquired biotin deficiency during parenteral alimentation. This paper presents a biotin assay utilizing radiolabeled avidin in a sequential, solid-phase method; the assay has increased sensitivity compared to previous methods (greater than or equal to 10 fmol/tube), correlates with expected trends in biotin concentrations in blood and urine in a rat model of biotin deficiency, and can utilize commercially available radiolabeled avidin

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

    Science.gov (United States)

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

    2016-04-01

    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.

  3. Improved detection limits for phthalates by selective solid-phase micro-extraction

    KAUST Repository

    Zia, Asif I.; Afsarimanesh, Nasrin; Xie, Li; Nag, Anindya; Al-Bahadly, I. H.; Yu, P. L.; Kosel, Jü rgen

    2016-01-01

    Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid

  4. Elementary excitations and phase transformations in solids

    International Nuclear Information System (INIS)

    Cowley, R.A.

    1985-01-01

    Neutron scattering is and will continue to be a uniquely powerful tool for the study of elementary excitations and phase transformations in solids. The paper examines a few recent experiments on molecular crystals, superionic materials, paramagnetic scattering and phase transitions to see what experimental features made these experiments possible, and hence to make suggestions about future needs. It is concluded that new instruments will extend the scope of neutron scattering studies to new excitations, that there is a need for higher resolution, particularly for phase transition studies, and that it will be important to use intensity information, discrimination against unwanted inelastic processes and polarization analysis to reliably measure the excitations in new materials. (author)

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

    DEFF Research Database (Denmark)

    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...

  6. Investigation of solid-phase hydrogenation of amino acids and peptides

    International Nuclear Information System (INIS)

    Zolotarev, Yu.A.; Myasoedov, N.F.; Zajtsev, D.A.; Lubnin, M.Yu.; Tatur, V.Yu.; Kozik, V.S.; Dorokhova, E.M.; Rozenberg, S.N.

    1990-01-01

    The possibility of synthesizing amino acids and peptides multiply labelled with tritium or deuterium by the method of solid-phase isotopic exchange with gaseous hydrogen isotopes was verified. Establishment of the isotopic hydrogen equilibrium between the gaseous phase and the solid phase formed by the amino acid molecules was found experimentally. The activation energy of the isotopic exchange is 13 kcal/mol. A mathematical model was set up for the isotopic exchange with a probable substitution of hydrogen atoms. Uniformly labelled amino acids were obtained in a high optical purity and with 80 to 90% hydrogen substitution by deuterium and tritium. Tritiated peptides were prepared in high yields at molar activities of 1.5 to 3.7 TBq/mmol. (author). 4 tabs

  7. Organic dye for highly efficient solid-state dye-sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt-Mende, L.; Bach, U.; Humphry-Baker, R.; Ito, S.; Graetzel, M. [Institut des Sciences et Ingenierie Chimiques (ISIC), Laboratoire de Photonique et Interfaces (LPI), Ecole Polytechnique Federale de Lausanne (EPFL), CH-1015 Lausanne (Switzerland); Horiuchi, T.; Miura, H. [Technology Research Laboratory, Corporate Research Center, Mitsubishi Paper Mills Limited, 46, Wadai, Tsukuba City, Ibaraki 300-4247 (Japan); Uchida, S. [Institute of Multidisciplinary Research for Advanced Materials (IMRAM), Tohoku University, 1-1 Katahira 2-chome, Aoba-ku, Sendai 980-8577 (Japan)

    2005-04-04

    The feasibility of solid-state dye-sensitized solar cells as a low-cost alternative to amorphous silicon cells is demonstrated. Such a cell with a record efficiency of over 4 % under simulated sunlight is reported, made possible by using a new organic metal-free indoline dye as the sensitizer with high absorption coefficient. (Abstract Copyright [2005], Wiley Periodicals, Inc.)

  8. The use of solid sorbents for direct accumulation of organic compounds from water matrices : a review of solid-phase extraction techniques

    NARCIS (Netherlands)

    Liska, I.; Krupcik, J.; Leclercq, P.A.

    1989-01-01

    The main principles of solid-phase extraction techniques are reviewed in this paper. Various solid sorbents can be used as a suitable trap for direct accumulation of organic compounds from aqueous solutions. The trapped analytes can be desorbed by elution with suitably chosen liquid phases. These

  9. The growth and tensile deformation behavior of the silver solid solution phase with zinc

    International Nuclear Information System (INIS)

    Wu, Jiaqi; Lee, Chin C.

    2016-01-01

    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.

  10. Three-phase boundary length in solid-oxide fuel cells: A mathematical model

    Energy Technology Data Exchange (ETDEWEB)

    Janardhanan, Vinod M. [Institutefor Chemical Technology and Polymer Chemistry, University of Karlsruhe (TH), Kaiserstr. 12, D-76128 Karlsruhe (Germany); Heuveline, Vincent; Deutschmann, Olaf [Institute for Applied and Numerical Mathematics, University of Karlsruhe (TH), Kaiserstr. 12, D-76128 Karlsruhe (Germany)

    2008-03-15

    A mathematical model to calculate the volume specific three-phase boundary length in the porous composite electrodes of solid-oxide fuel cell is presented. The model is exclusively based on geometrical considerations accounting for porosity, particle diameter, particle size distribution, and solids phase distribution. Results are presented for uniform particle size distribution as well as for non-uniform particle size distribution. (author)

  11. Three-phase boundary length in solid-oxide fuel cells: A mathematical model

    Science.gov (United States)

    Janardhanan, Vinod M.; Heuveline, Vincent; Deutschmann, Olaf

    A mathematical model to calculate the volume specific three-phase boundary length in the porous composite electrodes of solid-oxide fuel cell is presented. The model is exclusively based on geometrical considerations accounting for porosity, particle diameter, particle size distribution, and solids phase distribution. Results are presented for uniform particle size distribution as well as for non-uniform particle size distribution.

  12. Solid-Phase Contact Assay That Uses a lux-Marked Nitrosomonas europaea Reporter Strain To Estimate Toxicity of Bioavailable Linear Alkylbenzene Sulfonate in Soil

    OpenAIRE

    Brandt, Kristian K.; Pedersen, Anders; Sørensen, Jan

    2002-01-01

    Information about in situ toxicity of the bioavailable pools of adsorptive soil pollutants is a prerequisite for proper ecological risk assessment in contaminated soils. Such toxicity data may be obtained by assays allowing for direct exposure of introduced test microorganisms to the toxicants, as they appear in solid solution equilibria in the natural soil. We describe a novel sensitive solid-phase contact assay for in situ toxicity testing of soil pollutants based on a recombinant biolumine...

  13. A simple and sensitive approach to quantify methyl farnesoate in whole arthropods by matrix-solid phase dispersion and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Montes, Rosa; Rodil, Rosario; Neuparth, Teresa; Santos, Miguel M; Cela, Rafael; Quintana, José Benito

    2017-07-28

    Methyl farnesoate (MF) is an arthropod hormone that plays a key role in the physiology of several arthropods' classes being implicated in biological processes such as molting and reproduction. The development of an analytical technique to quantify the levels of this compound in biological tissues can be of major importance for the field of aquaculture/apiculture conservation and in endocrine disruption studies. Therefore, the aim of this study was to develop a simple and sensitive method to measure native levels of MF in the tissue of three representative species from different arthropods classes with environmental and/or economic importance. Thus, a new approach using whole organisms and the combination of matrix solid-phase dispersion with gas chromatography coupled to mass spectrometry was developed. This method allows quantifying endogenous MF at low levels (LOQs in the 1.2-3.1ng/g range) in three arthropod species, and could be expanded to additional arthropod classes. The found levels ranged between 2 and 12ng/g depending on the studied species and gender. The overall recovery of the method was evaluated and ranged between 69 and 96%. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. A reactor/separator device for use in automated solid phase immunoassay

    International Nuclear Information System (INIS)

    Farina, P.R.; Ordonez, K.P.; Siewers, I.J.

    1979-01-01

    A reactor/separator device is described for use in automated solid phase immunoassay, including radioimmunoassays. The device is a column fitted at the bottom portion with a water impermeable disc which can hold, for example, immunoabsorbents, immobilized antisera or ion exchange resins. When the contents of the column supported by the disc are brought into contact with an aqueous phase containing reagents or reactants, a chemical reaction is initiated. After the reaction, centrifugally applied pressure forces the aqueous phase through the filter disc making it water permeable and separating a desired component for subsequent analysis. The reactor/separator device of the present invention permits kinetic solid phase assays (non-equilibrium conditions) to be carried out which would be difficult to perform by other conventional methods. (author)

  15. Faults of solid-phase welding in titanium joints and their effect on strength

    International Nuclear Information System (INIS)

    Matyushkin, B.A.; Redchits, V.V.

    1982-01-01

    A possibility of the usage of thermal arc energy for the determination of the kinetics of solid-phase joint formation of the VT20 titanium alloy is found out experimentally. Positive action of diffusion annealing upon mechanical properties. of solid-phase joints is explained by the defect elimination

  16. Method for calculating solid-solid phase transitions at high temperature: An application to N2O

    International Nuclear Information System (INIS)

    Kuchta, B.; Etters, R.D.

    1992-01-01

    Two similar techniques for calculating solid-solid phase transitions at high temperatures are developed, where the contribution of the entropy may be a decisive factor. They utilize an artificial reversible path from one phase to another by application of a control parameter. Thermodynamic averages are calculated using constant-volume and constant-pressure Monte Carlo techniques. An application to N 2 O at room temperature shows that the cubic Pa3 to orthorhombic Cmca transition occurs near 4.9-GPa pressure, very close to the value calculated at very low temperatures. These results support experimental evidence that the transition pressure is virtually independent of temperature

  17. A review of solid-fluid selection options for optical-based measurements in single-phase liquid, two-phase liquid-liquid and multiphase solid-liquid flows

    Science.gov (United States)

    Wright, Stuart F.; Zadrazil, Ivan; Markides, Christos N.

    2017-09-01

    Experimental techniques based on optical measurement principles have experienced significant growth in recent decades. They are able to provide detailed information with high-spatiotemporal resolution on important scalar (e.g., temperature, concentration, and phase) and vector (e.g., velocity) fields in single-phase or multiphase flows, as well as interfacial characteristics in the latter, which has been instrumental to step-changes in our fundamental understanding of these flows, and the development and validation of advanced models with ever-improving predictive accuracy and reliability. Relevant techniques rely upon well-established optical methods such as direct photography, laser-induced fluorescence, laser Doppler velocimetry/phase Doppler anemometry, particle image/tracking velocimetry, and variants thereof. The accuracy of the resulting data depends on numerous factors including, importantly, the refractive indices of the solids and liquids used. The best results are obtained when the observational materials have closely matched refractive indices, including test-section walls, liquid phases, and any suspended particles. This paper reviews solid-liquid and solid-liquid-liquid refractive-index-matched systems employed in different fields, e.g., multiphase flows, turbomachinery, bio-fluid flows, with an emphasis on liquid-liquid systems. The refractive indices of various aqueous and organic phases found in the literature span the range 1.330-1.620 and 1.251-1.637, respectively, allowing the identification of appropriate combinations to match selected transparent or translucent plastics/polymers, glasses, or custom materials in single-phase liquid or multiphase liquid-liquid flow systems. In addition, the refractive indices of fluids can be further tuned with the use of additives, which also allows for the matching of important flow similarity parameters such as density and viscosity.

  18. Deterministic phase measurements exhibiting super-sensitivity and super-resolution

    DEFF Research Database (Denmark)

    Schäfermeier, Clemens; Ježek, Miroslav; Madsen, Lars S.

    2018-01-01

    Phase super-sensitivity is obtained when the sensitivity in a phase measurement goes beyond the quantum shot noise limit, whereas super-resolution is obtained when the interference fringes in an interferometer are narrower than half the input wavelength. Here we show experimentally that these two...

  19. Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

    Science.gov (United States)

    Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

    2014-11-26

    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.

  20. Solid-phase micro-extraction in bioanalysis, exemplified by lidocaine determination

    NARCIS (Netherlands)

    de Jong, GJ; Koster, EHM

    2000-01-01

    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

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

    African Journals Online (AJOL)

    A headspace solid-phase microextraction (HS-SPME) method was developed as a preliminary investigation using univariate approach for the analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow ...

  2. Solid phase separation technique for use in radioimmunoassays

    International Nuclear Information System (INIS)

    Tu, J.I.

    1979-01-01

    A radioimmunoassay procedure, and article of manufacture for carrying out that procedure, are disclosed herein. The solid phase separation technique utilized in the radioimmunoassay of this invention utilizes a test tube, the internal surface of which has been coated with two antibody layers

  3. The study of long-term stability in liquid-solid phases for HLW disposal

    International Nuclear Information System (INIS)

    Wei, Y.Y.; Tseng, C.L.; Yang, J.Y.; Ke, C.H.; Wang, T.H.; Jan, Y.L.; Lee, C.B.; Lan, P.L.; Hsu, C.N.; Tsai, S.C.; Li, M.H.; Teng, S.P.

    2005-01-01

    Full text of publication follows: This study is conducted to observe changes in both chemical properties of buffer materials and liquid phases over an experimental period of 2 years. In our experiments, bentonite powder and crushed granite are separately mixed with synthetic groundwater, synthetic seawater and de-ionised water at a fixed liquid-solid ratio of 30. A mixed set with both bentonite and granite together as solid phase is also investigated. During this study, aliquots of the liquid phases are sampled every two months and pH and Eh values are measured immediately. Concentrations of Na, Mg, K, Al, Ca, Ti, Mn, Ba, Fe, Sr, Li and Th are analyzed in the liquid phase directly by ICP-AES. After separation by centrifugation followed by freeze drying and digestion, the solid phases are analyzed as well for elemental composition. Alteration of solid phases during the experimental period is discussed. The preliminary results show that the pH values of the three solutions vary considerably in the individual experimental systems containing bentonite, granite or the mixed system. In general, higher pH values are found in DI-water for all solid phases. Eh values fluctuate a lot in the range 100 to 300 mV in all experiment sets. Different to the experiments with granite for which similar Eh values are found in all solutions, a significantly different Eh-value is found in the experiment with bentonite in DI-water as compared to the other solutions. The results from element analysis indicate that equilibrium is achieved after only two months and element concentrations change only slightly thereafter. We conclude from our experiments that both bentonite and granite keep their characteristics as radionuclide sorbents in the vicinity of a nuclear waste repository. Reaction equilibria appear to be attained rapidly. Because there are just a few alterations in this study, it would be a huge error source in analyzing from the inhomogeneous solid phase such as granite and losses

  4. Solid phase stability of molybdenum under compression: Sound velocity measurements and first-principles calculations

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xiulu [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China); Laboratory for Extreme Conditions Matter Properties, Southwest University of Science and Technology, 621010 Mianyang, Sichuan (China); Liu, Zhongli [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China); College of Physics and Electric Information, Luoyang Normal University, 471022 Luoyang, Henan (China); Jin, Ke; Xi, Feng; Yu, Yuying; Tan, Ye; Dai, Chengda; Cai, Lingcang [Laboratory for Shock Wave and Detonation Physics Research, Institute of Fluid Physics, P.O. Box 919-102, 621900 Mianyang, Sichuan (China)

    2015-02-07

    The high-pressure solid phase stability of molybdenum (Mo) has been the center of a long-standing controversy on its high-pressure melting. In this work, experimental and theoretical researches have been conducted to check its solid phase stability under compression. First, we performed sound velocity measurements from 38 to 160 GPa using the two-stage light gas gun and explosive loading in backward- and forward-impact geometries, along with the high-precision velocity interferometry. From the sound velocities, we found no solid-solid phase transition in Mo before shock melting, which does not support the previous solid-solid phase transition conclusion inferred from the sharp drops of the longitudinal sound velocity [Hixson et al., Phys. Rev. Lett. 62, 637 (1989)]. Then, we searched its structures globally using the multi-algorithm collaborative crystal structure prediction technique combined with the density functional theory. By comparing the enthalpies of body centered cubic structure with those of the metastable structures, we found that bcc is the most stable structure in the range of 0–300 GPa. The present theoretical results together with previous ones greatly support our experimental conclusions.

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

    NARCIS (Netherlands)

    Matovic, M.

    2007-01-01

    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

  6. Development and Application of Solid Phase Extraction Method for ...

    African Journals Online (AJOL)

    NICO

    for the addition of organic modifier, sample load volume, conditioning solvent, washing solvent and ... Solid phase extraction, polycyclic aromatic hydrocarbons, water samples, ... such as polymeric, activated carbon or silica modified with.

  7. Kinetic modeling of solid-state partitioning phase transformation with simultaneous misfit accommodation

    International Nuclear Information System (INIS)

    Song, Shaojie; Liu, Feng

    2016-01-01

    Considering a spherical misfitting precipitate growing into a finite elastic-perfectly plastic supersaturated matrix, a kinetic modeling for such solid-state partitioning phase transformation is presented, where the interactions of interface migration, solute diffusion and misfit accommodation are analyzed. The linkage between interface migration and solute diffusion proceeds through interfacial composition and interface velocity; their effects on misfit accommodation are mainly manifested in an effective transformation strain, which depends on instantaneous composition field and precipitate size. Taking γ to α transformation of a binary Fe-0.5 at.% C alloy under both isothermal and continuous cooling conditions as examples, the effects of misfit accommodation on the coupling interface migration and solute diffusion are well evaluated and discussed. For the isothermal transformation, a counterbalancing influence between mechanical and chemical driving forces is found so that the mixed-mode transformation kinetics is not sensitive with respect to the elastic–plastic accommodation of the effective misfit strain. Different from the isothermal process, during the continuous cooling condition, the effects of misfit accommodation on the kinetics of solid-state partitioning phase transformation are mainly manifested in the great decrease of the transformation starting temperature and the thermodynamic equilibrium composition. The present kinetic modeling was applied to predict the experimentally measured γ/α transformation of Fe-0.47 at.% C alloy conducted with a cooling rate of 10 K min −1 and a good agreement was achieved.

  8. UV sensitivity of various solid state detectors

    International Nuclear Information System (INIS)

    Knezevic, Zeljka; Ranogajec-Komor, Maria; Miljanic, Saveta

    2008-01-01

    Full text: The light sensitivity is an important characteristic of solid state passive dosimeters used in individual, clinical and environmental dosimetry. Light sensitivity stands for the response directly induced by visible or UV light in a fully annealed material. For the above mentioned applications a negligible light sensitivity is an advantage. However, high light sensitivity and linear response allows the use of detectors as UV dosimeters. For this purpose various TL detectors and the glass element of the RPL dosemeter type SC-1 were systematically investigated after exposure to UV light (254 and 366 nm) as a function of time. The following solid state detectors were investigated relative to TLD-100: Li 2 B 4 O 7 :Cu,Ag,P LiF:Mg,Cu,P, LiF:Mg,Cu,Si, Al 2 O 3 :C and the glass element of RPL dosimeter. UV irradiations were performed with Camag UV lamp at 254 nm and at 366 nm. The illumination times were 5, 10 and 20 minutes. Day light illumination was also carried out at room temperature over time period of several hours up to 2 weeks. The UV light response of each detector was compared to the response obtained after irradiation with 137 Cs. Al 2 O 3 :C, showed high light sensitivity; after 10 minutes illumination with 254 nm UV light the response was equivalent to 130 mGy 137 Cs gamma irradiation. The 254 nm UV response of LiF:Mg,Cu,P (GR-200 A), as well as TLD-700H and Li 2 B 4 O 7 :Cu,Ag,P were proportional to the time of illumination. The responses after 10 min UV illumination were equivalent to 0.001 mGy, 0.01 mGy and 0.1 mGy 137 Cs gamma irradiation, respectively. The complete SC-1 RPL dosimeter is insensitive to light because the glass element is encapsulated in light protected holder throughout the automatic evaluation process following the annealing (irradiation, preheat, readout). The responses of the previously annealed glass element after 20 min illumination with 254 nm and 366 nm UV light were equivalent to 45μSv and 3 μSv of 137 Cs gamma

  9. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    Directory of Open Access Journals (Sweden)

    H. Heidari

    2009-08-01

    Full Text Available AbstractBackground and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated. Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  10. Rapid and sensitive analysis of phthalate metabolites, bisphenol A, and endogenous steroid hormones in human urine by mixed-mode solid-phase extraction, dansylation, and ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Wang, He-xing; Wang, Bin; Zhou, Ying; Jiang, Qing-wu

    2013-05-01

    Steroid hormone levels in human urine are convenient and sensitive indicators for the impact of phthalates and/or bisphenol A (BPA) exposure on the human steroid hormone endocrine system. In this study, a rapid and sensitive method for determination of 14 phthalate metabolites, BPA, and ten endogenous steroid hormones in urine was developed and validated on the basis of ultra-performance liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry. The optimized mixed-mode solid phase-extraction separated the weakly acidic or neutral BPA and steroid hormones from acidic phthalate metabolites in urine: the former were determined in positive ion mode with a methanol/water mobile phase containing 10 mM ammonium formate; the latter were determined in negative ion mode with a acetonitrile/water mobile phase containing 0.1 % acetic acid, which significantly alleviated matrix effects for the analysis of BPA and steroid hormones. Dansylation of estrogens and BPA realized simultaneous and sensitive analysis of the endogenous steroid hormones and BPA in a single chromatographic run. The limits of detection were less than 0.84 ng/mL for phthalate metabolites and less than 0.22 ng/mL for endogenous steroid hormones and BPA. This proposed method had satisfactory precision and accuracy, and was successfully applied to the analyses of human urine samples. This method could be valuable when investigating the associations among endocrine-disrupting chemicals, endogenous steroid hormones, and relevant adverse outcomes in epidemiological studies.

  11. High sensitivity phase retrieval method in grating-based x-ray phase contrast imaging

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Zhao; Gao, Kun; Chen, Jian; Wang, Dajiang; Wang, Shenghao; Chen, Heng; Bao, Yuan; Shao, Qigang; Wang, Zhili, E-mail: wangnsrl@ustc.edu.cn [National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230029 (China); Zhang, Kai [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Zhu, Peiping; Wu, Ziyu, E-mail: wuzy@ustc.edu.cn [National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230029, China and Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)

    2015-02-15

    Purpose: Grating-based x-ray phase contrast imaging is considered as one of the most promising techniques for future medical imaging. Many different methods have been developed to retrieve phase signal, among which the phase stepping (PS) method is widely used. However, further practical implementations are hindered, due to its complex scanning mode and high radiation dose. In contrast, the reverse projection (RP) method is a novel fast and low dose extraction approach. In this contribution, the authors present a quantitative analysis of the noise properties of the refraction signals retrieved by the two methods and compare their sensitivities. Methods: Using the error propagation formula, the authors analyze theoretically the signal-to-noise ratios (SNRs) of the refraction images retrieved by the two methods. Then, the sensitivities of the two extraction methods are compared under an identical exposure dose. Numerical experiments are performed to validate the theoretical results and provide some quantitative insight. Results: The SNRs of the two methods are both dependent on the system parameters, but in different ways. Comparison between their sensitivities reveals that for the refraction signal, the RP method possesses a higher sensitivity, especially in the case of high visibility and/or at the edge of the object. Conclusions: Compared with the PS method, the RP method has a superior sensitivity and provides refraction images with a higher SNR. Therefore, one can obtain highly sensitive refraction images in grating-based phase contrast imaging. This is very important for future preclinical and clinical implementations.

  12. High sensitivity phase retrieval method in grating-based x-ray phase contrast imaging

    International Nuclear Information System (INIS)

    Wu, Zhao; Gao, Kun; Chen, Jian; Wang, Dajiang; Wang, Shenghao; Chen, Heng; Bao, Yuan; Shao, Qigang; Wang, Zhili; Zhang, Kai; Zhu, Peiping; Wu, Ziyu

    2015-01-01

    Purpose: Grating-based x-ray phase contrast imaging is considered as one of the most promising techniques for future medical imaging. Many different methods have been developed to retrieve phase signal, among which the phase stepping (PS) method is widely used. However, further practical implementations are hindered, due to its complex scanning mode and high radiation dose. In contrast, the reverse projection (RP) method is a novel fast and low dose extraction approach. In this contribution, the authors present a quantitative analysis of the noise properties of the refraction signals retrieved by the two methods and compare their sensitivities. Methods: Using the error propagation formula, the authors analyze theoretically the signal-to-noise ratios (SNRs) of the refraction images retrieved by the two methods. Then, the sensitivities of the two extraction methods are compared under an identical exposure dose. Numerical experiments are performed to validate the theoretical results and provide some quantitative insight. Results: The SNRs of the two methods are both dependent on the system parameters, but in different ways. Comparison between their sensitivities reveals that for the refraction signal, the RP method possesses a higher sensitivity, especially in the case of high visibility and/or at the edge of the object. Conclusions: Compared with the PS method, the RP method has a superior sensitivity and provides refraction images with a higher SNR. Therefore, one can obtain highly sensitive refraction images in grating-based phase contrast imaging. This is very important for future preclinical and clinical implementations

  13. Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

    Science.gov (United States)

    Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

    2014-10-01

    Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    DEFF Research Database (Denmark)

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

    2004-01-01

    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 formatio...

  15. Tetraphenylimidodiphosphinate as solid phase extractant for preconcentrative separation of thorium from aqueous solution

    International Nuclear Information System (INIS)

    Na Liu; Yanfei Wang; Chuhua He

    2016-01-01

    A simple and reliable method for solid phase extraction of thorium using tetraphenylimidodiphosphinate is presented. The solid phase extraction process was optimized at equilibrium time 3 h, pH = 4.5, initial concentration 30 mg L -1 and extractant dosage 0.01 g with 98.95 % of removal efficiency and 29.68 mg g -1 of adsorption capacity. The interfering ions experiments indicated that it had almost no effect on thorium adsorption. Kinetics data follow the pseudo-first-order model and equilibrium data agreed with the Langmuir isotherm model very well. FT-IR analysis indicated that imino group and phosphoryl acted as the significant roles in the solid phase extraction process. (author)

  16. Zirconium determination in rocks by solid-phase spectrophotometry

    International Nuclear Information System (INIS)

    Brykina, G.D.; Lebedeva, G.G.; Agapova, G.F.; AN SSSR, Moscow

    1990-01-01

    A method was developed for determination of zirconium in rocks by solid-phase spectrophotometry using AV-17x8-Cl anion exchanger modified with xylenol orange. Relative standard deviation at the level of (2-4.9)x10 -3 % ZrO 2 was about 0.245

  17. Anti-double strand (ds) DNA antibody formation by NZB/W (F1) spleen cells in a microculture system detected by solid phase radioimmunoassay.

    Science.gov (United States)

    Okudaira, H; Terada, E; Ogita, T; Aotsuka, S; Yokohari, R

    1981-01-01

    A solid-phase radioimmunoassay method was devised to detect mouse anti-double strand (ds) DNA antibody. This method could easily detect the anti-dsDNA antibody in 1 : 10,000 dilutions (1 unit) of pooled 9-10-month-old female NZB/W F1 sera. The sensitivity was about 10(3)- and 10(2)-fold higher than that of the modified Farr method and of the double antibody technique respectively. NZB/W mice developed high titer anti-dsDNA antibody as they grew older. Spleen cells brought to a microculture system using flat-bottomed polystyrene plates produced anti-dsDNA antibody clearly detectable by solid-phase radioimmunoassay. Anti-dsDNA antibody produced in vitro (y units) was in close correlation with the anti-dsDNA antibody titer of the spleen donor (x units) (y = 4.8 X 10(-2) x -65, gamma = 0.94, P less than 0.001). A combination of the microculture system and solid-phase radioimmunoassay was recommended for the characterization of anti-dsDNA antibody-forming cells.

  18. Anti-double strand (ds) DNA antibody formation by NZB/W (F1) spleen cells in a microculture system detected by solid-phase radioimmunoassay

    International Nuclear Information System (INIS)

    Okudaira, H.; Terada, E.; Ogita, T.; Aotsuka, S.; Yokohari, R.

    1981-01-01

    A solid-phase radioimmunoassay method was devised to detect mouse anti-double strand (ds) DNA antibody. This method could easily detect the anti-ds DNA antibody in 1 : 10,000 dilutions (1 unit) of pooled 9-10 month-old female NZB/W F1 sera. The sensitivity was about 10 3 and 10 2 -fold higher than that of the modified Farr method and of the double antibody technique respectively. NZB/W mice developed high titer anti-dsDNA antibody as they grew older. Spleen cells brought to a microculture system using flat-bottomed polystyrene plates produced anti-dsDNA antibody clearly detectable by solid-phase radioimmunoassay. Anti-dsDNA antibody produced in vitro (y units) was in close correlation with the anti-dsDNA antibody titer of the spleen donor (x units) (y = 4.8 X 10 -2 x-65, γ = 0.94, P < 0.001). A combination of the microculture system and solid-phase radioimmunoassay was recommended for the characterization of anti-dsDNA antibody-forming cells. (Auth.)

  19. Microwave assisted solid phase extraction for separation preconcentration sulfamethoxazole in wastewater using tyre based activated carbon as solid phase material prior to spectrophotometric determination

    Science.gov (United States)

    Mogolodi Dimpe, K.; Mpupa, Anele; Nomngongo, Philiswa N.

    2018-01-01

    This work was chiefly encouraged by the continuous consumption of antibiotics which eventually pose harmful effects on animals and human beings when present in water systems. In this study, the activated carbon (AC) was used as a solid phase material for the removal of sulfamethoxazole (SMX) in wastewater samples. The microwave assisted solid phase extraction (MASPE) as a sample extraction method was employed to better extract SMX in water samples and finally the analysis of SMX was done by the UV-Vis spectrophotometer. The microwave assisted solid phase extraction method was optimized using a two-level fractional factorial design by evaluating parameters such as pH, mass of adsorbent (MA), extraction time (ET), eluent ratio (ER) and microwave power (MP). Under optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) were 0.5 μg L- 1 and 1.7 μg L- 1, respectively, and intraday and interday precision expressed in terms of relative standard deviation were > 6%.The maximum adsorption capacity was 138 mg g- 1 for SMX and the adsorbent could be reused eight times. Lastly, the MASPE method was applied for the removal of SMX in wastewater samples collected from a domestic wastewater treatment plant (WWTP) and river water.

  20. Solid Phase Characterization Of Heel Samples From Tank 241-C-110

    International Nuclear Information System (INIS)

    Page, J.S.; Cooke, G.A.; Pestovich, J.A.; Huber, H.J.

    2011-01-01

    During sluicing operations of tank 241-C-110, a significant amount of solids were unable to be retrieved. These solids (often referred to as the tank 'heel') were sampled in 2010 and chemically and mineralogically analyzed in the 222-S Laboratory. Additionally, dissolution tests were performed to identify the amount of undissolvable material after using multiple water contacts. This report covers the solid phase characterization of six samples from these tests using scanning electron microscopy, polarized light microscopy, and X-ray diffraction. The chemical analyses, particle size distribution analysis, and dissolution test results are reported separately. Two of the samples were from composites created from as-received material - Composite A and Composite B. The main phase in these samples was sodium-fluoride-phosphate hydrate (natrophosphate) - in the X-ray diffraction spectra, this phase was the only phase identifiable. Polarized light microscopy showed the presence of minor amounts of gibbsite and other phases. These phases were identified by scanning electron microscopy - energy dispersive X-ray spectroscopy as sodium aluminosilicates, sodium diuranate, and sodium strontium phosphate hydrate (nastrophite) crystals. The natrophosphate crystals in the scanning electron microscopy analysis showed a variety of erosive and dissolution features from perfectly shaped octahedral to well-rounded appearance. Two samples were from water-washed Composites A and B, with no change in mineralogy compared to the as-received samples. This is not surprising, since the water wash had only a short period of water contact with the material as opposed to the water dissolution tests. The last two samples were residual solids from the water dissolution tests. These tests included multiple additions of water at 15 C and 45 C. The samples were sieved to separate a coarser fraction of > 710 μm and a finer fraction of < 710 μm. These two fractions were analyzed separately. The coarser

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

    Institute of Scientific and Technical Information of China (English)

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

    2003-01-01

    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.

  2. Solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K

    International Nuclear Information System (INIS)

    Ren Jing; Gu Zhengfei; Cheng Gang; Zhou Huaiying

    2005-01-01

    The solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K (Pr ≤ 70%) were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectroscopy (EDS) techniques. The 1173 K isothermal section consists of 13 single-phase regions, 22 two-phase regions and 10 three-phase regions. At 1173 K, we have observed that the maximum solid solubility of Pt in α-Fe is below 1.5 at.% and the solid solution region of Pt in γ-Fe is from 2 to 35 at.%; the maximum solid solubility of Fe in Pt is 18 at.%. The maximum solubility of Fe in PrPt 5 , PrPt 3 , PrPt 2 , Pr 3 Pt 4 , PrPt, Pr 3 Pt 2 and Pr 7 Pt 3 is below 1 at.%. The maximum solubility of Pr in α-(Fe, Pt), γ-(Fe, Pt), FePt, FePt 3 and (Pt, Fe) (the solid solution of Fe in Pt) is 6, 2, 4, 4.5 and 1.5 at.%, respectively. In this work, it is found that the phase Pr 3 Pt 4 does not exist in the ternary system. The binary compounds Fe 7 Pr and Fe 2 Pr and any new ternary compounds were not observed

  3. Practical solid and liquid phase markers for studying gastric emptying in man

    International Nuclear Information System (INIS)

    Thomforde, G.M.; Brown, M.L.; Malagelada, J.R.

    1985-01-01

    This paper presents a method used to evaluate solid and liquid phase markers for radionuclide gastric emptying studies. The authors conducted in vitro and in vivo comparative experiments employing several radiolabeled markers. Among the solid phase markers tested, Tc-99m-sulfur colloid in vivo-labeled liver and I-131-fiber performed optimally. However, Tc-99M sulfur colloid in scrambled egg showed very acceptable performance and it is significantly easier to prepare. Among liquid phase markers, they found In-111-DTPA stabilized with 1% albumin to be a good agent and appropriate for dual isotope emptying studies

  4. Simple fabrication of solid phase microextraction fiber employing nitrogen-doped ordered mesoporous polymer by in situ polymerization.

    Science.gov (United States)

    Zheng, Juan; Liang, Yeru; Liu, Shuqin; Jiang, Ruifen; Zhu, Fang; Wu, Dingcai; Ouyang, Gangfeng

    2016-01-04

    A combination of nitrogen-doped ordered mesoporous polymer (NOMP) and stainless steel wires led to highly sensitive, selective, and stable solid phase microextraction (SPME) fibers by in situ polymerization for the first time. The ordered structure of synthesized NOMP coating was illustrated by transmission electron microscopy (TEM) and X-ray diffraction (XRD), and microscopy analysis by scanning electron microscopy (SEM) confirmed a homogenous morphology of the NOMP-coated fiber. The NOMP-coated fiber was further applied for the extraction of organochlorine pesticides (OCPs) with direct-immersion solid-phase microextraction (DI-SPME) method followed by gas chromatography-mass spectrometry (GC-MS) quantification. Under the optimized conditions, low detection limits (0.023-0.77 ng L(-1)), a wide linear range (9-1500 ng L(-1)), good repeatability (3.5-8.1%, n=6) and excellent reproducibility (1.5-8.3%, n=3) were achieved. Moreover, the practical feasibility of the proposed method was evaluated by determining OCPs in environmental water samples with satisfactory recoveries. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    DEFF Research Database (Denmark)

    Nielsen, John

    1998-01-01

    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...

  6. Solid-Phase Extraction Combined with High Performance Liquid ...

    African Journals Online (AJOL)

    Methods: Solid-phase extraction method was employed for the extraction of the estrogen from milk and high performance liquid chromatography-diode array detector (HPLC-DAD) was used for the determination of estrogen. Results: Optimal chromatographic conditions were achieved on an Eclipse XDB-C18 column at a ...

  7. Lessons learned: from dye-sensitized solar cells to all-solid-state hybrid devices.

    Science.gov (United States)

    Docampo, Pablo; Guldin, Stefan; Leijtens, Tomas; Noel, Nakita K; Steiner, Ullrich; Snaith, Henry J

    2014-06-25

    The field of solution-processed photovoltaic cells is currently in its second spring. The dye-sensitized solar cell is a widely studied and longstanding candidate for future energy generation. Recently, inorganic absorber-based devices have reached new record efficiencies, with the benefits of all-solid-state devices. In this rapidly changing environment, this review sheds light on recent developments in all-solid-state solar cells in terms of electrode architecture, alternative sensitizers, and hole-transporting materials. These concepts are of general applicability to many next-generation device platforms. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

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

    2018-01-01

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

  9. Microwave-assisted solid-phase Ugi four-component condensations

    DEFF Research Database (Denmark)

    Nielsen, John

    1999-01-01

    An 18-member library was constructed from 2 isocyanides, 3 aldehydes and 3 carboxylic acids via microwave-assisted solid-phase Ugi reactions on TentaGel S RAM. Products of high purity were obtained in moderate to excellent yields after reaction times of 5 minutes or less (irradiation at 60W). (C...

  10. Detection of HLA Antibodies in Organ Transplant Recipients – Triumphs and Challenges of the Solid Phase Bead Assay

    Science.gov (United States)

    Tait, Brian D.

    2016-01-01

    This review outlines the development of human leukocyte antigen (HLA) antibody detection assays and their use in organ transplantation in both antibody screening and crossmatching. The development of sensitive solid phase assays such as the enzyme-linked immunosorbent assay technique, and in particular the bead-based technology has revolutionized this field over the last 10–15 years. This revolution however has created a new paradigm in clinical decision making with respect to the detection of low level pretransplant HLA sensitization and its clinical relevance. The relative sensitivities of the assays used are discussed and the relevance of conflicting inter-assay results. Each assay has its advantages and disadvantages and these are discussed. Over the last decade, the bead-based assay utilizing the Luminex® fluorocytometer instrument has become established as the “gold standard” for HLA antibody testing. However, there are still unresolved issues surrounding this technique, such as the presence of denatured HLA molecules on the beads which reveal cryptic epitopes and the issue of appropriate fluorescence cut off values for positivity. The assay has been modified to detect complement binding (CB) in addition to non-complement binding (NCB) HLA antibodies although the clinical relevance of the CB and NCB IgG isotypes is not fully resolved. The increase sensitivity of the Luminex® bead assay over the complement-dependent cytotoxicity crossmatch has permitted the concept of the “virtual crossmatch” whereby the crossmatch is predicted to a high degree of accuracy based on the HLA antibody specificities detected by the solid phase assay. Dialog between clinicians and laboratory staff on an individual patient basis is essential for correct clinical decision making based on HLA antibody results obtained by the various techniques. PMID:28018342

  11. Investigation into process of solid-phase synthesis of calcium vanadates

    International Nuclear Information System (INIS)

    Fotiev, A.A.; Krasnenko, T.I.; Slobodin, B.V.

    1983-01-01

    Processes of solid-phase synthesis of calcium vanadates by Toubandt method, measuring electric conductivity and Ca 45 and V 48 radioactive indicators are investigated. It is shown that reaction diffusion during calcium vanadates production from oxides is ensured by calcium and oxygen ions or calcium ions and electrons through the product layer, as to oxygen - through the gas phase

  12. The mechanism of reequilibration of solids in the presence of a fluid phase

    International Nuclear Information System (INIS)

    Putnis, Andrew; Putnis, Christine V.

    2007-01-01

    The preservation of morphology (pseudomorphism) and crystal structure during the transformation of one solid phase to another is regularly used as a criterion for a solid-state mechanism, even when there is a fluid phase present. However, a coupled dissolution-reprecipitation mechanism also preserves the morphology and transfers crystallographic information from parent to product by epitaxial nucleation. The generation of porosity in the product phase is a necessary condition for such a mechanism as it allows fluid to maintain contact with a reaction interface which moves through the parent phase from the original surface. We propose that interface-coupled dissolution-reprecipitation is a general mechanism for reequilibration of solids in the presence of a fluid phase. - Graphical abstract: A single crystal of KBr is transformed to a porous single crystal of KCl by immersion in saturated KCl solution. The image shows partial transformation of a crystal of KBr (core) to KCl (porous, milky rim) by an interface coupled dissolution-reprecipitation mechanism. The external dimensions and crystallographic orientation of the original crystal are preserved, while a reaction interface moves through the crystal

  13. Aqueous Microwave-Assisted Solid-Phase Synthesis Using Boc-Amino Acid Nanoparticles

    Directory of Open Access Journals (Sweden)

    Yoshinobu Fukumori

    2013-07-01

    Full Text Available We have previously developed water-based microwave (MW-assisted peptide synthesis using Fmoc-amino acid nanopaticles. It is an organic solvent-free, environmentally friendly method for peptide synthesis. Here we describe water-based MW-assisted solid-phase synthesis using Boc-amino acid nanoparticles. The microwave irradiation allowed rapid solid-phase reaction of nanoparticle reactants on the resin in water. We also demonstrated the syntheses of Leu-enkephalin, Tyr-Gly-Gly-Phe-Leu-OH, and difficult sequence model peptide, Val-Ala-Val-Ala-Gly-OH, using our water-based MW-assisted protocol with Boc-amino acid nanoparticles.

  14. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    Directory of Open Access Journals (Sweden)

    H Heidari

    2012-05-01

    Full Text Available

    Background and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.

    Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated.

    Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.

    Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  15. Development Of Radioimmunoassay For Prolactin HORMONE Using Solid Phase Magnetic Particles

    International Nuclear Information System (INIS)

    SHAFIK, H.M.; MEHANY, N.L.

    2009-01-01

    The preparation and development of primary reagents of prolactin (PRL) radioimmunoassay (RIA) technique using solid phase magnetic particles with low cost is considered to be the main objective of the present study. The production of polyclonal antibodies was undertaken by immunizing four female New-Zealand rabbits through primary injection and four booster doses subcutaneously. The preparation of 125 I-prolactin radiotracer was carried out using chloramine-T. The preparation of standard prolactin was undertaken by preparing stock standard solution of prolactin and diluted with assay buffer. Activation and coupling of low magnetizable particles with the purified anti-PRL was carried out. Optimization and validation of the assay were carried out. The results obtained provide a highly sensitive, specific and accurate RIA system of PRL. In conclusion, this assay could be used in diagnosis of galactorrhea, prolactinoma, visual impairment and diagnosis of infertility in males and females.

  16. Solid phase extraction-electrospray ionization mass spectrometric method for the determination of palladium

    International Nuclear Information System (INIS)

    Pranaw Kumar; Telmore, Vijay M.; Jaison, P.G.; Sarkar, Arnab; Alamelu, D.; Aggarwal, S.K.

    2015-01-01

    Platinum group of element (PGEs) are extensively used as a catalyst and anticancer reagent. Due to the soft nature of PGEs, sulphur based donar ligands are used for the separation of these elements. Studies on the formation of different species are helpful for obtaining the ideas about separation of these elements from the complex matrices. Palladium (Pd) is studied as a representative element which is also formed by nuclear fission of fissile nuclides. In view of the relatively small amount of solvent required for separation, solid phase extraction is preferred over most of the separation methods. Solid phase extraction method using DPX as a stationary phase was previously reported for the separation of Pd in SHLLW using benzoylthiourea as a ligand. However, in case of large volume samples manual extraction by DPX is tedious task. In the present studies, the feasibility of extraction using benzoylthiourea on automated solid phase extraction system was carried out for the extraction of Pd

  17. Interfacial chemistry and the design of solid-phase nucleic acid hybridization assays using immobilized quantum dots as donors in fluorescence resonance energy transfer.

    Science.gov (United States)

    Algar, W Russ; Krull, Ulrich J

    2011-01-01

    The use of quantum dots (QDs) as donors in fluorescence resonance energy transfer (FRET) offer several advantages for the development of multiplexed solid-phase QD-FRET nucleic acid hybridization assays. Designs for multiplexing have been demonstrated, but important challenges remain in the optimization of these systems. In this work, we identify several strategies based on the design of interfacial chemistry for improving sensitivity, obtaining lower limits of detection (LOD) and enabling the regeneration and reuse of solid-phase QD-FRET hybridization assays. FRET-sensitized emission from acceptor dyes associated with hybridization events at immobilized QD donors provides the analytical signal in these assays. The minimization of active sensing area reduces background from QD donor PL and allows the resolution of smaller amounts of acceptor emission, thus lowering the LOD. The association of multiple acceptor dyes with each hybridization event can enhance FRET efficiency, thereby improving sensitivity. Many previous studies have used interfacial protein layers to generate selectivity; however, transient destabilization of these layers is shown to prevent efficient regeneration. To this end, we report a protein-free interfacial chemistry and demonstrate the specific detection of as little as 2 pmol of target, as well as an improved capacity for regeneration.

  18. Phase relations and Gibbs energies of spinel phases and solid solutions in the system Mg-Rh-O

    Energy Technology Data Exchange (ETDEWEB)

    Jacob, K.T., E-mail: katob@materials.iisc.ernet.in [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Prusty, Debadutta [Department of Materials Engineering, Indian Institute of Science, Bangalore 560 012 (India); Kale, G.M. [Institute for Materials Research, University of Leeds, Leeds, LS2 9JT (United Kingdom)

    2012-02-05

    Highlights: Black-Right-Pointing-Pointer Refinement of phase diagram for the system Mg-Rh-O and thermodynamic data for spinel compounds MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} is presented. Black-Right-Pointing-Pointer A solid-state electrochemical cell is used for thermodynamic measurement. Black-Right-Pointing-Pointer An advanced design of the solid-state electrochemical cell incorporating buffer electrodes is deployed to minimize polarization of working electrode. Black-Right-Pointing-Pointer Regular solution model for the spinel solid solution MgRh{sub 2}O{sub 4} - Mg{sub 2}RhO{sub 4} based on ideal mixing of cations on the octahedral site is proposed. Black-Right-Pointing-Pointer Factors responsible for stabilization of tetravalent rhodium in spinel compounds are identified. - Abstract: Pure stoichiometric MgRh{sub 2}O{sub 4} could not be prepared by solid state reaction from an equimolar mixture of MgO and Rh{sub 2}O{sub 3} in air. The spinel phase formed always contained excess of Mg and traces of Rh or Rh{sub 2}O{sub 3}. The spinel phase can be considered as a solid solution of Mg{sub 2}RhO{sub 4} in MgRh{sub 2}O{sub 4}. The compositions of the spinel solid solution in equilibrium with different phases in the ternary system Mg-Rh-O were determined by electron probe microanalysis. The oxygen potential established by the equilibrium between Rh + MgO + Mg{sub 1+x}Rh{sub 2-x}O{sub 4} was measured as a function of temperature using a solid-state cell incorporating yttria-stabilized zirconia as an electrolyte and pure oxygen at 0.1 MPa as the reference electrode. To avoid polarization of the working electrode during the measurements, an improved design of the cell with a buffer electrode was used. The standard Gibbs energies of formation of MgRh{sub 2}O{sub 4} and Mg{sub 2}RhO{sub 4} were deduced from the measured electromotive force (e.m.f.) by invoking a model for the spinel solid solution. The parameters of the model were optimized using the measured

  19. Solid-solid phase transformation via internal stress-induced virtual melting, significantly below the melting temperature. Application to HMX energetic crystal.

    Science.gov (United States)

    Levitas, Valery I; Henson, Bryan F; Smilowitz, Laura B; Asay, Blaine W

    2006-05-25

    We theoretically predict a new phenomenon, namely, that a solid-solid phase transformation (PT) with a large transformation strain can occur via internal stress-induced virtual melting along the interface at temperatures significantly (more than 100 K) below the melting temperature. We show that the energy of elastic stresses, induced by transformation strain, increases the driving force for melting and reduces the melting temperature. Immediately after melting, stresses relax and the unstable melt solidifies. Fast solidification in a thin layer leads to nanoscale cracking which does not affect the thermodynamics or kinetics of the solid-solid transformation. Thus, virtual melting represents a new mechanism of solid-solid PT, stress relaxation, and loss of coherence at a moving solid-solid interface. It also removes the athermal interface friction and deletes the thermomechanical memory of preceding cycles of the direct-reverse transformation. It is also found that nonhydrostatic compressive internal stresses promote melting in contrast to hydrostatic pressure. Sixteen theoretical predictions are in qualitative and quantitative agreement with experiments conducted on the PTs in the energetic crystal HMX. In particular, (a) the energy of internal stresses is sufficient to reduce the melting temperature from 551 to 430 K for the delta phase during the beta --> delta PT and from 520 to 400 K for the beta phase during the delta --> beta PT; (b) predicted activation energies for direct and reverse PTs coincide with corresponding melting energies of the beta and delta phases and with the experimental values; (c) the temperature dependence of the rate constant is determined by the heat of fusion, for both direct and reverse PTs; results b and c are obtained both for overall kinetics and for interface propagation; (d) considerable nanocracking, homogeneously distributed in the transformed material, accompanies the PT, as predicted by theory; (e) the nanocracking does not

  20. Solid-phase oligosaccharide and glycopeptide synthesis using glycosynthases

    DEFF Research Database (Denmark)

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

    2002-01-01

    and the prospect of automatability. Here, we report the first application of glycosynthases to solid-phase oligosaccharide synthesis by use of the 51 kDa serine and glycine mutants of Agrobacterium sp. beta-glucosidase, Abg E358S and E358G. Acceptors were linked to PEGA resin through a backbone amide linker (BAL...

  1. Solid-Phase Synthesis of Smac Peptidomimetics Incorporating Triazoloprolines and Biarylalanines

    DEFF Research Database (Denmark)

    Le Quement, Sebastian T.; Ishoey, Mette; Petersen, Mette T.

    2011-01-01

    by deactivating proteolytic caspases. The Smac protein has an antagonistic effect on IAPs, thus providing structural clues for the synthesis of new pro-apoptotic compounds. Herein, we report a solid-phase approach for the synthesis of Smac-derived tetrapeptide libraries. On the basis of a common (N......-Me)AVPF sequence, peptides incorporating triazoloprolines and biarylalanines were synthesized by means of Cu(I)-catalyzed azide–alkyne cycloaddition and Pd-catalyzed Suzuki cross-coupling reactions. Solid-phase procedures were optimized to high efficiency, thus accessing all products in excellent crude purities...... and yields (both typically above 90%). The peptides were subjected to biological evaluation in a live/dead cellular assay which revealed that structural decorations on the AVPF sequence indeed are highly important for cytotoxicity toward HeLa cells....

  2. Determination of clenbuterol in bovine liver by combining matrix solid phase dispersion and molecularly imprinted solid phase extraction followed by liquid chromatography/electrospray ion trap multiple stage mass spectrometry

    NARCIS (Netherlands)

    Crescenzi, C; Bayoudh, S; Cormack, P.A G; Klein, T; Ensing, K

    2001-01-01

    Matrix solid-phase dispersion(MSPD) is a new sample pretreatment for solid samples. This technique greatly simplifies sample pretreatment but, nonetheless, the extracts often still require an extra cleanup step that is both laborious and time-consuming. The potential;of combining MSPD with

  3. A Variational Model for Two-Phase Immiscible Electroosmotic Flow at Solid Surfaces

    KAUST Repository

    Shao, Sihong

    2012-01-01

    We develop a continuum hydrodynamic model for two-phase immiscible flows that involve electroosmotic effect in an electrolyte and moving contact line at solid surfaces. The model is derived through a variational approach based on the Onsager principle of minimum energy dissipation. This approach was first presented in the derivation of a continuum hydrodynamic model for moving contact line in neutral two-phase immiscible flows (Qian, Wang, and Sheng, J. Fluid Mech. 564, 333-360 (2006)). Physically, the electroosmotic effect can be formulated by the Onsager principle as well in the linear response regime. Therefore, the same variational approach is applied here to the derivation of the continuum hydrodynamic model for charged two-phase immiscible flows where one fluid component is an electrolyte exhibiting electroosmotic effect on a charged surface. A phase field is employed to model the diffuse interface between two immiscible fluid components, one being the electrolyte and the other a nonconductive fluid, both allowed to slip at solid surfaces. Our model consists of the incompressible Navier-Stokes equation for momentum transport, the Nernst-Planck equation for ion transport, the Cahn-Hilliard phase-field equation for interface motion, and the Poisson equation for electric potential, along with all the necessary boundary conditions. In particular, all the dynamic boundary conditions at solid surfaces, including the generalized Navier boundary condition for slip, are derived together with the equations of motion in the bulk region. Numerical examples in two-dimensional space, which involve overlapped electric double layer fields, have been presented to demonstrate the validity and applicability of the model, and a few salient features of the two-phase immiscible electroosmotic flows at solid surface. The wall slip in the vicinity of moving contact line and the Smoluchowski slip in the electric double layer are both investigated. © 2012 Global-Science Press.

  4. Finite element modeling for integrated solid-solid PCM-building material with varying phase change temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, D.; Fung, A.S.; Siddiqui, O. [Ryerson Polytechnic Univ., Toronto, ON (Canada). Dept. of Mechanical and Industrial Engineering

    2008-08-15

    Solid-solid phase change materials (SSPCMs) are used to enhance thermal storage performance and reduce indoor temperature fluctuations in buildings. In this study, a finite element model (FEM) was used to investigate the thermal properties of different types of SSPCMs. An effective heat capacity method was used to develop the model. An integrated PCM-building material was analyzed in relation to temperature and heat flux profiles. Governing equations for the heat transfer process were composed of Navier-Stokes momentum equations; a mass conservation equation; and an energy conservation equation. Effective heat capacity was described as a linear function of the latent heat of fusion on both the heating and cooling processes. Data from the simulation were then compared with an experiment suing drywall, concrete and gypcrete samples. Heat flux across the surfaces and temperatures on the surfaces of the materials were measured. Data were used to validate the finite element model (FEM). Results of the study suggested that heat flux profiles are an effective means of understanding phase change processes. It was concluded that PCMs with lower phase change temperatures lengthened energy releases and improved thermal comfort in the building. 12 refs., 2 tabs., 14 figs.

  5. Study on the technical parameters of two different systems of RIA performed with solid-phase antibody test tubes prepared with magnetic microparticle covalence conjagation or conventional physical absorption

    International Nuclear Information System (INIS)

    Chen Zhiqiang; Wang Chengmin; Tang Baojun

    2007-01-01

    Objective: To investigate a new method of preparation of solid-phase antibody with flurorescein isothioeynate (FITC)-anti FITC magnetic nanoparticles system (for FT 3 and TSH). Methods: FT 3 and TSH monoclonal antibody IgC was la- belied with FITC. Anti-FITC magnetic mieroparticles was prepared and conjugated with the FITC labelled antibody to form the solid - phase coated test tube for RIA. Solid-phase test tube prepared with the conventional physical absorption method was also used for RIA and the technical parameters of the two systems were compared. Results: For FT 3 , the sensitivity was 0.18pmol/L with the new method and 0.43pmol/L with the conventional method. Other parameters were; intra-CV, 8.96% vs 16.26%; inter-CV, 15.25% vs 18.83%, correlation with PR method r=0.9825 vs r=0.9102. For TSH, sensitivity was 0.061 μIU/ml vs 0.04 μ IU/ml, intra- CV, 7.6% vs 6.92%, inter-CV, 8.55% vs 14.23%, correlation between the new and conventional method, r=0. 9987. TSH RIA was especially rapid with the new technic: 79 min vs 190 min. Conclusion: For FT 3 and TSH RIA, the new method takes much less time with increased homogeniety. (authors)

  6. A solid-phase-radioimmunoassay for total serum thyroxine

    International Nuclear Information System (INIS)

    Moedder, G.; Sokolowski, G.

    1978-01-01

    A new solid phase radioimmunoassay for total serum thyroxine was evaluated over a longer time under clinical routine conditions and compared with an established test system. The results show up that the T 4 values are precise, reliable and reproducible, the is incomplicate to handle and well suitable for semiautomatic pipetting systems. (orig.) 891 MG [de

  7. Analysis of a solid-phase radioimmunoassay for antibodies to cytoplasmic antigen fractions of Candida albicans

    International Nuclear Information System (INIS)

    Mauch, H.; Bromback, J.

    1981-01-01

    An indirect solid-phase radioimmunoassay (SPRIA) in individual polystyrene microtiter cups has been adapted for measurement of antibody to various cytoplasmic and carbohydrate antigen fractions of Candida albicans. The assay was optimized for sensitivity, precision and linearization of serum dilution curves. The optimized procedure allows computerized measurement of anti-Candida antibodies and can be used for measurement of antibody over a wide concentration range. The procedure obviates variation due to changes in day-to-day counts as a result of isotope decay and end-point antibody dilutions. The assay has been used to demonstrate a Poisson-like distribution of antibody levels in the sera of persons showing no symptoms of candidiasis. The minimum antibody level detectable by the assay is about two orders of magnitude lower than the lowest level found in human serum and 4 orders of magnitude lower than the most sensitive test used hitherto, the hemagglutination test. (Auth.)

  8. Melting along the Hugoniot and solid phase transition for Sn via sound velocity measurements

    Science.gov (United States)

    Song, Ping; Cai, Ling-cang; Tao, Tian-jiong; Yuan, Shuai; Chen, Hong; Huang, Jin; Zhao, Xin-wen; Wang, Xue-jun

    2016-11-01

    It is very important to determine the phase boundaries for materials with complex crystalline phase structures to construct their corresponding multi-phase equation of state. By measuring the sound velocity of Sn with different porosities, different shock-induced melting pressures along the solid-liquid phase boundary could be obtained. The incipient shock-induced melting of porous Sn samples with two different porosities occurred at a pressure of about 49.1 GPa for a porosity of 1.01 and 45.6 GPa for a porosity of 1.02, based on measurements of the sound velocity. The incipient shock-induced melting pressure of solid Sn was revised to 58.1 GPa using supplemental measurements of the sound velocity. Trivially, pores in Sn decreased the shock-induced melting pressure. Based on the measured longitudinal sound velocity data, a refined solid phase transition and the Hugoniot temperature-pressure curve's trend are discussed. No bcc phase transition occurs along the Hugoniot for porous Sn; further investigation is required to understand the implications of this finding.

  9. Determination of organophosphorus pesticides using molecularly imprinted polymer solid phase extraction

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Syairah Salleh; Wan Aini Wan Ibrahim

    2011-01-01

    Molecularly imprinted polymer solid phase extraction (MIP-SPE) method has been developed for the determination of organophosphorus pesticides (OPPs) in water samples. The MIP was prepared by thermo-polymerization method using methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as crosslinker, acetonitrile as porogenic solvent and quinalphos as the template molecule. The three OPPs (diazinon, quinalphos and chloropyrifos) were selected as target analytes as they are widely used in agriculture sector. Various parameters affecting the extraction efficiency of the imprinted polymers have been evaluated to optimize the selective preconcentration of OPPs from aqueous samples. The characteristics of the MIP-SPE method were validated by high performance liquid chromatography (HPLC). The accuracy and selectivity of the MIP-SPE process developed were verified using non-imprinted polymer solid phase extraction (NIP-SPE) and a commercial C 18 -SPE was used for comparison. The recoveries of the target analytes obtained using the MIPs as the solid phase sorbent ranged from 83% to 98% (RSDs 1.05 - 1.98 %; n=3) for water sample. The developed MIP-SPE method demonstrates that it could be applied for the determination of OPPs in water samples. (author)

  10. Effects of deep cryogenic treatment on the solid-state phase transformation of Cu-Al alloy in cooling process

    Science.gov (United States)

    Wang, Yuhui; Liao, Bo; Liu, Jianhua; Chen, Shuqing; Feng, Yu; Zhang, Yanyan; Zhang, Ruijun

    2012-07-01

    The solid-state phase transformation temperature and duration of deep cryogenic treated and untreated Cu-Al alloys in cooling process were measured by differential scanning calorimetry measurement. The solid-state phase transformation activation energy and Avrami exponent were calculated according to these measurements. The effects of deep cryogenic treatment on the solid-state phase transformation were investigated based on the measurement and calculation as well as the observation of alloy's microstructure. The results show that deep cryogenic treatment can increase the solid-phase transformation activation energy and shorten the phase transformation duration, which is helpful to the formation of fine grains in Cu-Al alloy.

  11. Solid phase microextraction speciation analysis of triclosan in aqueous mediacontaining sorbing nanoparticles

    NARCIS (Netherlands)

    Zielinska, K.

    2014-01-01

    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

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

    NARCIS (Netherlands)

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

    2000-01-01

    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

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

    Directory of Open Access Journals (Sweden)

    Ireneusz Sowa

    2018-03-01

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

  14. Estrogenic and AhR activities in dissolved phase and suspended solids from wastewater treatment plants.

    Science.gov (United States)

    Dagnino, Sonia; Gomez, Elena; Picot, Bernadette; Cavaillès, Vincent; Casellas, Claude; Balaguer, Patrick; Fenet, Hélène

    2010-05-15

    The distribution of estrogen receptor (ERalpha) and Aryl Hydrocarbon Receptor (AhR) activities between the dissolved phase and suspended solids were investigated during wastewater treatment. Three wastewater treatment plants with different treatment technologies (waste stabilization ponds (WSPs), trickling filters (TFs) and activated sludge supplemented with a biofilter system (ASB)) were sampled. Estrogenic and AhR activities were detected in both phases in influents and effluents. Estrogenic and AhR activities in wastewater influents ranged from 41.8 to 79 ng/L E(2) Eq. and from 37.9 to 115.5 ng/L TCDD Eq. in the dissolved phase and from 5.5 to 88.6 ng/g E(2) Eq. and from 15 to 700 ng/g TCDD Eq. in the suspended solids. For both activities, WSP showed greater or similar removal efficiency than ASB and both were much more efficient than TF which had the lowest removal efficiency. Moreover, our data indicate that the efficiency of removal of ER and AhR activities from the suspended solid phase was mainly due to removal of suspended solids. Indeed, ER and AhR activities were detected in the effluent suspended solid phase indicating that suspended solids, which are usually not considered in these types of studies, contribute to environmental contamination by endocrine disrupting compounds and should therefore be routinely assessed for a better estimation of the ER and AhR activities released in the environment. Copyright 2010 Elsevier B.V. All rights reserved.

  15. Determination of 8 Synthetic Food Dyes by Solid Phase Extraction ...

    African Journals Online (AJOL)

    Keywords: Synthetic colors, Food, Fruit flavored drinks, Solid phase extraction, RP-HPLC. Tropical Journal of ..... food dyes by thin-layer chromatography-fast atom bombardment ... food dyes in soft drinks containing natural pigments by.

  16. Immobilization and functional reconstitution of antibody Fab fragment by solid-phase refolding.

    Science.gov (United States)

    Kumada, Yoichi; Hamasaki, Kyoto; Nakagawa, Aya; Sasaki, Eiju; Shirai, Tatsunori; Okumura, Masahiro; Inoue, Manami; Kishimoto, Michimasa

    2013-12-31

    In this study, we demonstrated the successful preparation of a Fab antibody-immobilized hydrophilic polystyrene (phi-PS) plate via one- and two-step solid-phase refolding methods. Both polystyrene-binding peptide (PS-tag)-fused Fd fragment of heavy chain (Fab H-PS) and full-length of light-chain (Fab L-PS) were individually produced in insoluble fractions of Escherichia coli cells, and they were highly purified in the presence of 8M of urea. Antigen-binding activities of Fab antibody immobilized were correctly recovered by the one-step solid-phase refolding method that a mixture of Fab H-PS and Fab L-PS was immobilized in the presence of 0.5-2M urea, followed by surface washing of the phi-PS plate with PBST. These results indicate that by genetic fusion of a PS-tag, a complex between Fab H and Fab L was efficiently immobilized on the surface of a phi-PS plate even in the presence of a low concentration of urea, and was then correctly refolded to retain its high antigen-binding activity via removal of the urea. A two-step solid-phase refolding method whereby Fab H-PS and Fab L-PS were successively refolded on the surface of a phi-PS plate also resulted in Fab antibody formation on the plate. Furthermore, both the binding affinity and the specificity of the Fab antibody produced by the two-step method were highly maintained, according to the results of sandwich ELISA and competitive ELISA using Fab antibody-immobilized plate via two-step solid-phase refolding. Thus, the solid-phase refolding method demonstrated in this study should be quite useful for the preparation of a Fab antibody-immobilized PS surface with high efficiency from individually produced Fab H-PS and Fab L-PS. This method will be applicable to the preparation of a large Fab antibody library on the surface of a PS plate for use in antibody screening. © 2013. Published by Elsevier B.V. All rights reserved.

  17. New Approaches in Soil Organic Matter Fluorescence; A Solid Phase Fluorescence Approach

    Science.gov (United States)

    Bowman, M. M.; Sanclements, M.; McKnight, D. M.

    2017-12-01

    Fluorescence spectroscopy is a well-established technique to investigate the composition of organic matter in aquatic systems and is increasingly applied to soil organic matter (SOM). Current methods require that SOM be extracted into a liquid prior to analysis by fluorescence spectroscopy. Soil extractions introduce an additional layer of complexity as the composition of the organic matter dissolved into solution varies based upon the selected extractant. Water is one of the most commonly used extractant, but only extracts the water-soluble fraction of the SOM with the insoluble soil organic matter fluorescence remaining in the soil matrix. We propose the use of solid phase fluorescence on whole soils as a potential tool to look at the composition of organic matter without the extraction bias and gain a more complete understand of the potential for fluorescence as a tool in terrestrial studies. To date, the limited applications of solid phase fluorescence have ranged from food and agriculture to pharmaceutical with no clearly defined methods and limitations available. We are aware of no other studies that use solid phase fluorescence and thus no clear methods to look at SOM across a diverse set of soil types and ecosystems. With this new approach to fluorescence spectroscopy there are new challenges, such as blank correction, inner filter effect corrections, and sample preparation. This work outlines a novel method for analyzing soil organic matter using solid phase fluorescence across a wide range of soils collected from the National Ecological Observatory Network (NEON) eco-domains. This method has shown that organic matter content in soils must be diluted to 2% to reduce backscattering and oversaturation of the detector in forested soils. In mineral horizons (A) there is observed quenching of the humic-like organic matter, which is likely a result of organo-mineral complexation. Finally, we present preliminary comparisons between solid and liquid phase

  18. Solid phase extraction of magnetic carbon doped Fe3O4 nanoparticles.

    Science.gov (United States)

    Yang, Jing; Li, Jia-yuan; Qiao, Jun-qin; Lian, Hong-zhen; Chen, Hong-yuan

    2014-01-17

    Carbon decorated Fe3O4 nanoparticles (Fe3O4/C) are promising magnetic solid-phase extraction (MSPE) sorbents in environmental and biological analysis. Fe3O4/C based MSPE method shows advantages of easy operation, rapidness, high sensitivity, and environmental friendliness. In this paper, the MSPE mechanism of Fe3O4/C nanoparticles has been comprehensively investigated, for the first time, through the following three efforts: (1) the comparison of extraction efficiency for polycyclic aromatic hydrocarbons (PAHs) between the Fe3O4/C sorbents and activated carbon; (2) the chromatographic retention behaviors of hydrophobic and hydrophilic compounds on Fe3O4/C nanoparticles as stationary phase; (3) related MSPE experiments for several typical compounds such as pyrene, naphthalene, benzene, phenol, resorcinol, anisole and thioanisole. It can be concluded that there are hybrid hydrophobic interaction and hydrogen bonding interaction or dipole-dipole attraction between Fe3O4/C sorbents and analytes. It is the existence of carbon and oxygen-containing functional groups coated on the surface of Fe3O4/C nanoparticles that is responsible for the effective extraction process. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Experimental Demonstration of Phase Sensitive Parametric Processes in a Nano-Engineered Silicon Waveguide

    DEFF Research Database (Denmark)

    Kang, Ning; Fadil, Ahmed; Pu, Minhao

    2013-01-01

    We demonstrate experimentally phase-sensitive processes in nano-engineered silicon waveguides for the first time. Furthermore, we highlight paths towards the optimization of the phase-sensitive extinction ratio under the impact of two-photon and free-carrier absorption.......We demonstrate experimentally phase-sensitive processes in nano-engineered silicon waveguides for the first time. Furthermore, we highlight paths towards the optimization of the phase-sensitive extinction ratio under the impact of two-photon and free-carrier absorption....

  20. Double-antibody solid-phase radioimmunoassay: a simplified phase-separation procedure applied to various ligands

    International Nuclear Information System (INIS)

    Tevaarwerk, G.J.M.; Boyle, D.A.; Hurst, C.J.; Anguish, I.; Uksik, P.

    1980-01-01

    The purpose was to develop a simplified and reliable method of separating free from antibody-bound ligand using a precipitating antibody linked to a cellulose derivative. Dose-response curves and control sera were set up in parallel for various pituitary and placental polypeptides, steroid hormones, insulin, glucagon, triiodothyronine, thyroxine, angiotensin I, calcitonin, gastrin, cyclic AMP, and digoxin. After first-antibody reactions had reached equilibrium, free and bound ligand were separated using a double-antibody solid-phase system in parallel with conventional methods, including dextran-coated charcoal, double-antibody precipitation, single-antibody solid phase, organic solvents, salt precipitation, and anion-exchange resins. The effect of variations in temperature, incubation time, protein content, pH, and amount of separating material added were studied. The results showed that separation was complete within 1 hr for small ligand molecules and within 2 hr for larger ones. Dose-response curves and control-sera results closely paralleled those obtained with conventional methods. The method was not affected by moderate variations in incubation variables. Nonspecific binding was less than 3% in all assays, while intra-assay and interassay coefficients of variation were similar to those obtained with conventional phase-separation methods. It is concluded that the method is a simple and rapid alternative phase-separation system. It has the advantage of being free from common nonspecific intersample variations, and can be applied to any assay system based on rabbit or guinea pig antibodies without preliminay time- or reagent-consuming titration or adjustments to establish optimum phase-separating conditions

  1. Modeling and Analysis of a Three-Phase Solid-State Var ...

    African Journals Online (AJOL)

    Modeling and Analysis of a Three-Phase Solid-State Var Compensator (SSVC) ... Nigerian Journal of Technology. Journal Home ... The problems associated with the flow of reactive power in transmission and distribution lines are well known.

  2. Formation of organic solid phases in hydrocarbon reservoir fluids. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Andersen, S.I.; Lindeloff, N.; Stenby, E.H.

    1998-12-31

    The occurrence of solid phases during oil recovery is a potential problem. The present work has mainly been concerned with wax formation due to cooling of oils with a large paraffin content. 8 oils have been included in this project, although only a few of these have till now been subject to all the experimental techniques applied. The oils and wax fractions from these have been characterized using techniques such as GC-MS and Ftir. The goal has in part been to get a detailed description of the oil composition for use in model evaluation and development and in part to get a fundamental understanding of waxy oil properties and behaviour. A high pressure (200 bar) equipment has been developed for automatic detection of wax appearance using a filtration technique and laser light turbidimetry. The latter was found to be far superior to the filtration. The filtration was used to sample the incipient solid phase for characterization. However entrapment of liquid in the filters currently used have hampered this part. A number of model systems and one gas condensate have been investigated. The GC-MS procedure was found only to been able to detect molecules up to n-C45 and the group type analysis was not accurate enough for modelling purposes. Using Ftir it was obvious that incipient phases may contain very complex molecules (asphaltenes) which are not captured by GC-MS especially when fractionation is done using the acetone precipitation at elevated temperature. The latter fractionation procedure has been investigated thoroughly as a tool for understanding wax distribution etc. Within thermodynamic modelling a delta lattice parameter model has been developed which incorporates the non-ideality of the solid phases into the calculation of SLE. The non-ideality is estimated from pure component properties. A new algorithm for phase equilibria involving gas-liquid-solid has been developed. Currently both the model work and the experimental works are continued. (au)

  3. Parameters influencing charge separation in solid-state dye-sensitized solar cells using novel hole conductors

    NARCIS (Netherlands)

    Kroeze, J.E.; Hirata, N.; Schmidt-Mende, L.; Orizu, C.; Ogier, S.D.; Carr, K.; Grätzel, M.; Durrant, J.R.

    2006-01-01

    Solid-state dye-sensitized solar cells employing a solid organic hole-transport material (HTM) are currently under intensive investigation, since they offer a number of practical advantages over liquid-electrolyte junction devices. Of particular importance to the design of such devices is the

  4. Phase-sensitive atomic dynamics in quantum light

    Science.gov (United States)

    Balybin, S. N.; Zakharov, R. V.; Tikhonova, O. V.

    2018-05-01

    Interaction between a quantum electromagnetic field and a model Ry atom with possible transitions to the continuum and to the low-lying resonant state is investigated. Strong sensitivity of atomic dynamics to the phase of applied coherent and squeezed vacuum light is found. Methods to extract the quantum field phase performing the measurements on the atomic system are proposed. In the case of the few-photon coherent state high accuracy of the phase determination is demonstrated, which appears to be much higher in comparison to the usually used quantum-optical methods such as homodyne detection.

  5. Solidification of liquid electrolyte with imidazole polymers for quasi-solid-state dye-sensitized solar cells

    International Nuclear Information System (INIS)

    Wang Miao; Lin Yuan; Zhou Xiaowen; Xiao Xurui; Yang Lei; Feng Shujing; Li Xueping

    2008-01-01

    Quasi-solid-state electrolytes were prepared by employing the imidazole polymers to solidify the liquid electrolyte containing lithium iodide, iodine and ethylene carbonate (EC)/propylene carbonate (PC) mixed solvent. The ionic conductivity and diffusion behavior of triiodide in the quasi-solid-state electrolytes were examined in terms of the polymer content. Application of the quasi-solid-state electrolytes to the dye-sensitized solar cells, the maximum energy conversion efficiency of 7.6% (AM 1.5, 100 mW cm -2 ) was achieved. The dependence of the photovoltaic performance on the polymer content and on the different anions of the imidazole polymers was studied by electrochemical impedance spectroscopy and cyclic voltammetry. The results indicate the charge transfer behaviors occurred at nanocrystalline TiO 2 /electrolyte and Pt/electrolyte interface play an important role in influencing the photovoltaic performance of quasi-solid-state dye-sensitized solar cells

  6. Probing the liquid and solid phases in closely spaced two-dimensional systems

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Ding

    2014-03-06

    partially filled Landau levels - can crystallize into a Wigner crystal. The Wigner crystal is bound to get pinned and hence localizes electrons in the bulk. This may cause an increase of the quantum Hall plateau width. To unveil the existence of such a solid, one has to go beyond standard transport investigations. Both microwave and NMR experiments have shown strong evidences for Wigner crystal formation. In Part I of the thesis, we present measurements of a thermodynamic quantity - the chemical potential. We provide further insight into this solid phase by studying the B-field as well as temperature dependence of the electron crystallization. The sensitive technique that we employ to measure the chemical potential is developed on a GaAs heterostructure with two quantum wells. In fact, in the presence of a perpendicular magnetic field this bilayer system hosts a unique quantum Hall state when each layer has a half filled Landau level. An electron residing in one layer can pair up with an empty state in the opposite layer and excitons may form. These excitons are believed to form an exciton condensate under appropriate conditions. Part II of this thesis is devoted to the understanding of this correlated state. We employ a single electron transistor to probe the chemical potential - more directly its derivative with respect to density, the compressibility - around the ν{sub tot} = 1 quantum Hall state. We then compare excitation gap obtained from this approach with the gap determined from thermally activated transport studies. Our results help to clarify the nature of the excitations at ν{sub tot} = 1. Apart from the thermodynamic measurement, we also perform tunneling experiments on the bilayer. A systematic study of the interlayer tunneling on the distance between the two layers is carried out. Also, we investigate the tunneling on a bilayer with a constriction in the center. Interesting phenomena are observed such as an oscillating pattern in the tunneling current as we

  7. Probing the liquid and solid phases in closely spaced two-dimensional systems

    International Nuclear Information System (INIS)

    Zhang, Ding

    2014-01-01

    filled Landau levels - can crystallize into a Wigner crystal. The Wigner crystal is bound to get pinned and hence localizes electrons in the bulk. This may cause an increase of the quantum Hall plateau width. To unveil the existence of such a solid, one has to go beyond standard transport investigations. Both microwave and NMR experiments have shown strong evidences for Wigner crystal formation. In Part I of the thesis, we present measurements of a thermodynamic quantity - the chemical potential. We provide further insight into this solid phase by studying the B-field as well as temperature dependence of the electron crystallization. The sensitive technique that we employ to measure the chemical potential is developed on a GaAs heterostructure with two quantum wells. In fact, in the presence of a perpendicular magnetic field this bilayer system hosts a unique quantum Hall state when each layer has a half filled Landau level. An electron residing in one layer can pair up with an empty state in the opposite layer and excitons may form. These excitons are believed to form an exciton condensate under appropriate conditions. Part II of this thesis is devoted to the understanding of this correlated state. We employ a single electron transistor to probe the chemical potential - more directly its derivative with respect to density, the compressibility - around the ν tot = 1 quantum Hall state. We then compare excitation gap obtained from this approach with the gap determined from thermally activated transport studies. Our results help to clarify the nature of the excitations at ν tot = 1. Apart from the thermodynamic measurement, we also perform tunneling experiments on the bilayer. A systematic study of the interlayer tunneling on the distance between the two layers is carried out. Also, we investigate the tunneling on a bilayer with a constriction in the center. Interesting phenomena are observed such as an oscillating pattern in the tunneling current as we gradually open

  8. Development of simple immunoradiometric assays using avidin coupled to polystyrene beads as a common solid phase

    International Nuclear Information System (INIS)

    Jyotsna, N.; Singh, Y.; Chouthkanthiwar, V.; Paradkar, S.; Sivaprasad, N.

    1998-01-01

    In this paper, we describe the preparation and application of avidin coupled polystyrene beads as a common solid phase for use in immunoradiometric assays (IRMAs). The assay system is based on two matched commercial monoclonal antibodies, of which, the capture antibody is biotinylated using biotinamidocaproate N-hydroxysuccinimide ester and the detection antibody is radiolabeled with 125 I by conventional Chloramine-T method. Avidin was immobilized on the polystyrene beads through a primary coat of bovine serum albumin using glutaraldhyde activation method. Various factors, such as concentration of reagents, incubation time, etc. were optimised to obtain a simple assay protocol consisting of only two pipetting steps, namely, that of a mixture of the two labelled antibodies (radiolabelled and biotinylated) and of the standard or sample. The advantage of the Avidin-Biotin system is the improved sensitivity, economy of antibody and the possibility to use a common solid phase in assays for different analytes. Using the polystyrene beads along with the novel decanting device, it has been possible to achieve the convenience of the 'coated-tube' technology without the expensive automation necessary for large scale preparation of antibody coated tubes. This protocol has been successfully applied to Prolactin, LH and FSH assays. The sensitivity of the Prolactin assay is 8μIU/mL (0.3 ng/mL), that of the FSH assay is 1mIU/mL and that of the LH assay is 0.9 mIU/mL. The intra-assay and inter-assay variations were <10%. Shelf life of the avidin coupled beads was found to be about 8 months and that of the biotin labelled antibodies up to 18 months. (author)

  9. Phase characteristics of solid-state amplifiers in sub-harmonic bunchers

    International Nuclear Information System (INIS)

    Liu Rong; Ma Xinpeng; Zhao Fengli; Wang Xiangjian; Wang Guangwei; Huang Yongqing; Zhang Donghui

    2009-01-01

    To study the phase characteristics of solid-state amplifiers(20 kW/142.8 MHz,10 kW/571.2 MHz) in sub-harmonic bunchers(SHBs) of the BEPC II linear accelerator, phase shift in pulse and phase stability are measured using a digital measurement method based on field programmable gate array(FPGA). The hardware of the measurement system includes the frequency synthesizer, digital signal processing board(FPGA) and PC, and the software includes an internal algorithm on FPGA, communication procedures and PC client interface procedures. The measurement results of phase characteristics are consistent with the actual situation, which is the basis for the further implement of phase compensation in SHBs. (authors)

  10. Liquid chromatography tandem mass spectrometry method using solid-phase extraction and bead-beating-assisted matrix solid-phase dispersion to quantify the fungicide tebuconazole in controlled frog exposure study: analysis of water and animal tissue

    DEFF Research Database (Denmark)

    Hansen, Martin; Poulsen, Rikke; Luong, Xuan

    2014-01-01

    and on tissue from exposed and non-exposed adult X. laevis. Using solid-phase extraction (SPE), the analytical method allows for quantification of tebuconazole at concentrations as low as 3.89 pg mL(-1) in 10 mL water samples. Using bead-beating-assisted matrix solid-phase dispersion (MSPD), it was possible...

  11. Solid phase extraction and metabolic profiling of exudates from living copepods

    DEFF Research Database (Denmark)

    Selander, Erik; Heuschele, Jan; Nylund, Göran M.

    2016-01-01

    describe the development of a closed loop solid phase extraction setup that allows for extraction of exuded metabolites from live copepods. We captured exudates from male and female Temora longicornis and analyzed the content with high resolution LC-MS. Chemometric methods revealed 87 compounds...... that solid phase extraction in combination with metabolic profiling of exudates is a useful tool to develop our understanding of the chemical interplay between pelagic organisms....... Copepodamide G, known to induce defensive responses in phytoplankton, was among the ten compounds of highest relative abundance in both male and female extracts. The presence of copepodamide G shows that the method can be used to capture and analyze chemical signals from living source organisms. We conclude...

  12. A Photolabile Linker for the Solid-Phase Synthesis of Peptide Hydrazides and Heterocycles

    DEFF Research Database (Denmark)

    Qvortrup, Katrine; Komnatnyy, Vitaly V.; Nielsen, Thomas Eiland

    2014-01-01

    A photolabile hydrazine linker for the solid-phase synthesis of peptide hydrazides and hydrazine-derived heterocycles is presented. The developed protocols enable the efficient synthesis of structurally diverse peptide hydrazides derived from the standard amino adds, including those with side......-chain protected residues at the C-terminal of the resulting peptide hydrazide, and are useful for the synthesis of dihydropyrano[2,3-c]pyrazoles. The linker is compatible with most commonly used coupling reagents and protecting groups for solid-phase peptide synthesis....

  13. ON-SITE SOLID-PHASE EXTRACTION AND LABORATORY ...

    Science.gov (United States)

    Fragrance materials such as synthetic musks in aqueous samples, are normally determined by gas chromatography/mass spectrometry in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of I -L samples. Full-scan mass spectra are required to verify that a target analyte has been found by comparison with the mass spectra of fragrance compounds in the NIST mass spectral library. A I -L sample usually provides insufficient analyte for full scan data acquisition. This paper describes an on-site extraction method developed at the U.S. Environmental Protection Agency (USEPA)- Las Vegas Nevada - for synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for a wide array of synthetic musks. Quantification of these compounds was achieved from the full-scan data directly, without the need to acquire SIM data. The detection limits obtained with this method are an order of magnitude lower than those obtained from liquid-liquid and other solid phase extraction methods. This method is highly reproducible, and recoveries ranged from 80 to 97% in spiked sewage treatment plant effluent. The high rate of sorbent-sample mass transfer eliminated the need for a methanolic activation step, which reduced extraction time, labor, and solvent use, More samples could be extracted in the field at lower cost. After swnple extraction, the light- weight cartridges ar

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

    Science.gov (United States)

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

    2013-12-20

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

  15. Solid phase crystallisation of HfO2 thin films

    International Nuclear Information System (INIS)

    Modreanu, M.; Sancho-Parramon, J.; O'Connell, D.; Justice, J.; Durand, O.; Servet, B.

    2005-01-01

    In this paper, we report on the solid phase crystallisation of carbon-free HfO 2 thin films deposited by plasma ion assisted deposition (PIAD). After deposition, the HfO 2 films were annealed in N 2 ambient for 3 h at 350, 550 and 750 deg. C. Several characterisation techniques including X-ray reflectometry (XRR), X-ray diffraction (XRD), spectroscopic ellipsometry (SE) and atomic force microscopy (AFM) were used for the physical characterisation of as-deposited and annealed HfO 2 . XRD has revealed that the as-deposited HfO 2 film is in an amorphous-like state with only traces of crystalline phase and that the annealed films are in a highly crystalline state. These results are in good agreement with the SE results showing an increase of refractive index by increasing the annealing temperature. XRR results show a significant density gradient over the as-deposited film thickness, which is characteristic of the PIAD method. The AFM measurements show that the HfO 2 layers have a smooth surface even after annealing at 750 deg. C. The present study demonstrates that the solid phase crystallisation of HfO 2 PIAD thin films starts at a temperature as low as 550 deg. C

  16. Colloidal Sb2S3 Nanocrystals: Synthesis, Characterization and Fabrication of Solid-State Semiconductor Sensitized Solar Cell

    KAUST Repository

    Abulikemu, Mutalifu

    2015-12-26

    Inorganic nanocrystals composed of earth-abundant and non-toxic elements are crucial to fabricated sustainable photovoltaic devices in large scale. In this study, various-shaped and different phases of antimony sulfide nanocrystals, which is composed of non-scarce and non-toxic elements, are synthesized using hot-injection colloidal method. The effect of various synthetic parameters on the final morphology is explored. Also, foreign ion (Chlorine) effects on the morphology of Sb2S3 nanocrystals have been observed. Structural, optical and morphological properties of the nanocrystals were investigated, and Sb2S3 nanocrystal-based solid-state semiconductor-sensitized solar cells were fabricated using as-prepared nanocrystals. We achieved promising power conversion efficiencies of 1.48%.

  17. Colloidal Sb2S3 Nanocrystals: Synthesis, Characterization and Fabrication of Solid-State Semiconductor Sensitized Solar Cell

    KAUST Repository

    Abulikemu, Mutalifu; Del Gobbo, Silvano; Anjum, Dalaver H.; Malik, Mohammad A; Bakr, Osman

    2015-01-01

    Inorganic nanocrystals composed of earth-abundant and non-toxic elements are crucial to fabricated sustainable photovoltaic devices in large scale. In this study, various-shaped and different phases of antimony sulfide nanocrystals, which is composed of non-scarce and non-toxic elements, are synthesized using hot-injection colloidal method. The effect of various synthetic parameters on the final morphology is explored. Also, foreign ion (Chlorine) effects on the morphology of Sb2S3 nanocrystals have been observed. Structural, optical and morphological properties of the nanocrystals were investigated, and Sb2S3 nanocrystal-based solid-state semiconductor-sensitized solar cells were fabricated using as-prepared nanocrystals. We achieved promising power conversion efficiencies of 1.48%.

  18. Molecularly imprinted solid-phase extraction in the analysis of agrochemicals.

    Science.gov (United States)

    Yi, Ling-Xiao; Fang, Rou; Chen, Guan-Hua

    2013-08-01

    The molecular imprinting technique is a highly predeterminative recognition technology. Molecularly imprinted polymers (MIPs) can be applied to the cleanup and preconcentration of analytes as the selective adsorbent of solid-phase extraction (SPE). In recent years, a new type of SPE has formed, molecularly imprinted polymer solid-phase extraction (MISPE), and has been widely applied to the extraction of agrochemicals. In this review, the mechanism of the molecular imprinting technique and the methodology of MIP preparations are explained. The extraction modes of MISPE, including offline and online, are discussed, and the applications of MISPE in the analysis of agrochemicals such as herbicides, fungicides and insecticides are summarized. It is concluded that MISPE is a powerful tool to selectively isolate agrochemicals from real samples with higher extraction and cleanup efficiency than commercial SPE and that it has great potential for broad applications.

  19. The constitutive distributed parameter model of multicomponent chemical processes in gas, fluid and solid phase

    International Nuclear Information System (INIS)

    Niemiec, W.

    1985-01-01

    In the literature of distributed parameter modelling of real processes is not considered the class of multicomponent chemical processes in gas, fluid and solid phase. The aim of paper is constitutive distributed parameter physicochemical model, constructed on kinetics and phenomenal analysis of multicomponent chemical processes in gas, fluid and solid phase. The mass, energy and momentum aspects of these multicomponent chemical reactions and adequate phenomena are utilized in balance operations, by conditions of: constitutive invariance for continuous media with space and time memories, reciprocity principle for isotropic and anisotropic nonhomogeneous media with space and time memories, application of definitions of following derivative and equation of continuity, to the construction of systems of partial differential constitutive state equations, in the following derivative forms for gas, fluid and solid phase. Couched in this way all physicochemical conditions of multicomponent chemical processes in gas, fluid and solid phase are new form of constitutive distributed parameter model for automatics and its systems of equations are new form of systems of partial differential constitutive state equations in sense of phenomenal distributed parameter control

  20. Prediction of transport phenomena in near and far field: interaction solid phase/fluid phase

    International Nuclear Information System (INIS)

    Mingarro, E.

    1995-01-01

    The prediction of transport phenomena in near and far field is presented in the present report. The study begins with the analysis of solid phases stability: solubility of storage waste: UO 2 and solubility of radionuclides the redox and sorption-desorption conditions are the last aspects studied to predict the transport phenomena

  1. The diagnosis of malaria infection using a solid-phase radioimmunoassay for the detection of malaria antigens

    International Nuclear Information System (INIS)

    Mackey, L.; Perrin, L.; Leemans, E.; Lambert, P.H.

    1980-01-01

    A method was devised to show that malaria parasites can be detected serologically in infected blood with a high degree of sensitivity. Using a murine malaria model, parasites were demonstrated in a solid-phase radio-immunoassay which measured antibody-binding inhibition. Lysed red blood cells (r.b.c.) were incubated with labelled specific antibody and were then reacted in antigen-coated tubes. The degree of inhibition of antibody binding in the tubes correlated with the level of parasitaemia in the test blood. Using homologous antisera the test detected infection at a level of 1 parasite/million r.b.c.. The specificity of the method was shown by comparison of antibody-binding inhibition in normal and infected r.b.c. and in r.b.c. from non-infected mice with induced reticulocytosis. The sensitivity was shown in vitro in tests of serially diluted blood of high parasitaemia and in vivo for the detection of early infection. The presence of antibody in the test blood did not significantly affect the sensitivity of parasite detection. (author)

  2. Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

    Science.gov (United States)

    Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

    2015-12-01

    A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. A photolabile linker for the solid-phase synthesis of 4-substituted NH-1,2,3-triazoles

    DEFF Research Database (Denmark)

    Qvortrup, Katrine; Nielsen, Thomas Eiland

    2011-01-01

    A novel photolabile linker for solid-phase synthesis is presented. The linker displays an azido handle for copper-catalyzed azide–alkyne cycloaddition reactions with a variety of alkynes, remains intact under typical solid-phase reaction conditions, and enables a mild photolytic release of 4...

  4. The use of solid phase microextraction as sample preparation technique for determination of n-nitrosodimethylamine in water polluted by hydrazine-based rocket fuel

    Directory of Open Access Journals (Sweden)

    Bulat Kenessov

    2009-05-01

    Full Text Available A paper describes a method for determination of N-nitrosodimethylamine in water, polluted by spills of 1,1-dimethylhydrazine, based on solid phase microextraction coupled to gas chromatography/mass spectrometry. A method detection limit was determined to be 1 ug/kg, relative error was below 20%. A method is very sensitive and selective as well as quite simple, relatively cheap and fully automated.

  5. Copper welding in solid phase; Svarka medi v tverdoj faze

    Energy Technology Data Exchange (ETDEWEB)

    Avagyan, V Sh

    1993-12-31

    An analysis of the publications on the technology of diffusion welding of copper in solid phase is carried out. The aspects of diffusion welding of copper with silver, aluminium, nickels, chromium, titanium, stainless steel and refractory metals are considered 35 refs.

  6. A novel phase-sensitive scanning near-field optical microscope

    International Nuclear Information System (INIS)

    Wu Xiao-Yu; Lin Sun; Tan Qiao-Feng; Wang Jia

    2015-01-01

    Phase is one of the most important parameters of electromagnetic waves. It is the phase distribution that determines the propagation, reflection, refraction, focusing, divergence, and coupling features of light, and further affects the intensity distribution. In recent years, the designs of surface plasmon polariton (SPP) devices have mostly been based on the phase modulation and manipulation. Here we demonstrate a phase sensitive multi-parameter heterodyne scanning near-field optical microscope (SNOM) with an aperture probe in the visible range, with which the near field optical phase and amplitude distributions can be simultaneously obtained. A novel architecture combining a spatial optical path and a fiber optical path is employed for stability and flexibility. Two kinds of typical nano-photonic devices are tested with the system. With the phase-sensitive SNOM, the phase and amplitude distributions of any nano-optical field and localized field generated with any SPP nano-structures and irregular phase modulation surfaces can be investigated. The phase distribution and the interference pattern will help us to gain a better understanding of how light interacts with SPP structures and how SPP waves generate, localize, convert, and propagate on an SPP surface. This will be a significant guidance on SPP nano-structure design and optimization. (paper)

  7. Comparison of solid-phase and eluate assays to gauge the ecotoxicological risk of organic wastes on soil organisms

    International Nuclear Information System (INIS)

    Domene, Xavier; Alcaniz, Josep M.; Andres, Pilar

    2008-01-01

    Development of methodologies to assess the safety of reusing polluted organic wastes in soil is a priority in Europe. In this study, and coupled with chemical analysis, seven organic wastes were subjected to different aquatic and soil bioassays. Tests were carried out with solid-phase waste and three different waste eluates (water, methanol, and dichloromethane). Solid-phase assays were indicated as the most suitable for waste testing not only in terms of relevance for real situations, but also because toxicity in eluates was generally not representative of the chronic effects in solid-phase. No general correlations were found between toxicity and waste pollutant burden, neither in solid-phase nor in eluate assays, showing the inability of chemical methods to predict the ecotoxicological risks of wastes. On the contrary, several physicochemical parameters reflecting the degree of low organic matter stability in wastes were the main contributors to the acute toxicity seen in collembolans and daphnids. - Comparison of solid-phase and eluate bioassays for organic waste testing

  8. Solid solution and amorphous phase in Ti–Nb–Ta–Mn systems synthesized by mechanical alloying

    Energy Technology Data Exchange (ETDEWEB)

    Aguilar, C., E-mail: claudio.aguilar@usm.cl [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Guzman, P. [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Lascano, S. [Departamento de Ingeniería Mecánica, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Parra, C. [Departamento de Física, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Bejar, L. [Instituto de Investigaciones Metalúrgicas, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, Morelia C.P. 58000, Michoacán (Mexico); Medina, A. [Facultad de Ingeniería Mecánica, Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, C.P. 58000, Michoacán (Mexico); Guzman, D. [Departamento de Metalurgia, Universidad de Atacama, Av. España 485, Copiapó (Chile)

    2016-06-15

    This work discusses the formation of Ti–30Nb–13Ta–xMn (x: 2, 4 and 6 wt%) solid solution by mechanical alloying using a shaker mill. A solid solution was formed after 15 h of milling and an amorphous phase was formed after 30 h of milling, according to X-ray diffraction results. Disappearance of strongest X-ray diffraction peaks of Nb, Ta and Mn indicated the formation of solid solution, while, X-ray diffraction patterns of powders milled for 30 h showed an amorphous hump with crystalline peaks in the angular range of 35–45° in 2θ. TEM image analysis showed the presence of nanocrystalline intermetallic compounds embedded in an amorphous matrix. Mn{sub 2}Ti, MnTi and NbTi{sub 4} intermetallic compounds were detected and revealed crystallites with size ranging from 3 to 20 nm. The Gibbs free energy for the formation of solid solution and amorphous phase of three ternary systems (Ti–Nb–Ta, Ti–Nb–Mn and Ti–Ta–Mn) was calculated using extended Miedema's model. Experimental and thermodynamic data confirmed that solid solution was first formed in the alloy with 6wt% Mn followed by the formation of an amorphous phase as milling time increases. The presence of Mn promoted the formation of amorphous phase because the atomic radius difference between Mn with Ti, Nb and Ta. - Highlights: • Thermodynamics analysis of extension of solid solution of the Ti–Nb–Ta–Mn system. • Formation of amorphous phase and intermetallic compounds were observed. • Nanocrystalline intermetallic compounds were formed with the sizes between 3 and 20 nm.

  9. Solid phase extraction and spectrophotometric determination of mercury in tobacco and tobacco additives with 5-(p-aminobenzylidene)-thiothiorhodanine

    International Nuclear Information System (INIS)

    Yang, Weizhu; Yang, Guangyu

    2006-01-01

    A highly sensitive, selective and rapid method for the determination of mercury based on the rapid reaction of mercury(II) with 5-(p-aminobenzylidene)-thiorhodanine (ABTR) and the solid phase extraction of the colored chelate with C 18 disks has been developed. At pH 3.5 and in the presence of emulsifier-OP medium, ABTR reacts with mercury(II) to form a red chelate of a 1:2 (mercury to ABTR) molar ratio. This chelate was enriched by solid phase extraction with C 18 disks and the retained chelate eluted form the disks with dimethyl formamide (DMF). An enrichment factor of 50 was achieved. In the DMF medium, the molar absorptivity of the chelate is 1.21 X 10 5 L mol -1 cm -1 at 545 nm, and Beer's law is obeyed in the 0.01∼3 μg mL -1 range in the measured solution. The relative standard deviation for eleven sample replicate measurements at the 0.01 μg mL -1 level is 1.7%. This method was applied to the determination of mercury in tobacco and tobacco additives and good preconcentration was found between proposed and comparative methods results. (author)

  10. Ultrasonic detection of solid phase mass flow ratio of pneumatic conveying fly ash

    Science.gov (United States)

    Duan, Guang Bin; Pan, Hong Li; Wang, Yong; Liu, Zong Ming

    2014-04-01

    In this paper, ultrasonic attenuation detection and weight balance are adopted to evaluate the solid mass ratio in this paper. Fly ash is transported on the up extraction fluidization pneumatic conveying workbench. In the ultrasonic test. McClements model and Bouguer-Lambert-Beer law model were applied to formulate the ultrasonic attenuation properties of gas-solid flow, which can give the solid mass ratio. While in the method of weigh balance, the averaged mass addition per second can reveal the solids mass flow ratio. By contrast these two solid phase mass ratio detection methods, we can know, the relative error is less.

  11. Isostructural solid-solid phase transition in monolayers of soft core-shell particles at fluid interfaces: structure and mechanics.

    Science.gov (United States)

    Rey, Marcel; Fernández-Rodríguez, Miguel Ángel; Steinacher, Mathias; Scheidegger, Laura; Geisel, Karen; Richtering, Walter; Squires, Todd M; Isa, Lucio

    2016-04-21

    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.

  12. Solid-phase synthesis of polyfunctional polylysine dendrons using aldehyde linkers

    DEFF Research Database (Denmark)

    Svenssen, Daniel K.; Mirsharghi, Sahar; Boas, Ulrik

    2014-01-01

    A straightforward method for the solid-phase synthesis of C-terminally modified polylysine dendrons has been developed by applying bisalkoxybenzaldehyde and trisalkoxybenzaldehyde linkers. The method has been used for the synthesis of polylysine dendrons with a variety of C-terminal ‘tail groups’...

  13. Graft-copolymerization of styrene on polypropylene in the solid phase

    NARCIS (Netherlands)

    Beenen, W.; VanderWal, D.; Janssen, L.P.B.M.; Buijtenhuijs, A.; Hogt, A.H.; Wal, Douwe J. v.d.

    The graft-copolymerization of styrene on PP in the solid phase has been studied under various reaction conditions using a radical initiator. Polymerization kinetics were investigated by DSC experiments and reactions in glass ampoules. The conversion rate and grafting efficiency of styrene appeared

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

    DEFF Research Database (Denmark)

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

    1990-01-01

    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...

  15. Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean

    International Nuclear Information System (INIS)

    Zhai, Haiyun; Su, Zihao; Chen, Zuanguang; Liu, Zhenping; Yuan, Kaisong; Huang, Lu

    2015-01-01

    Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g −1 . - Abstract: A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC–LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001–2.0 μg mL −1 (r = 0.9995) with the detection limit (S/N = 3) of 0.075 ng mL −1 . Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC–LIF method can be applied to sensitively determine phloxine B in coffee bean

  16. Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean

    Energy Technology Data Exchange (ETDEWEB)

    Zhai, Haiyun, E-mail: zhaihaiyun@126.com [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Su, Zihao [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Chen, Zuanguang, E-mail: chenzg@mail.sysu.edu.cn [School of Pharmaceutical Science, Sun Yat-sen University, Guangzhou 510006 (China); Liu, Zhenping; Yuan, Kaisong; Huang, Lu [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China)

    2015-03-20

    Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g{sup −1}. - Abstract: A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC–LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001–2.0 μg mL{sup −1} (r = 0.9995) with the detection limit (S/N = 3) of 0.075 ng mL{sup −1}. Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC–LIF method can be applied to sensitively determine phloxine B in coffee bean.

  17. Numerical simulation analysis of four-stage mutation of solid-liquid two-phase grinding

    Science.gov (United States)

    Li, Junye; Liu, Yang; Hou, Jikun; Hu, Jinglei; Zhang, Hengfu; Wu, Guiling

    2018-03-01

    In order to explore the numerical simulation of solid-liquid two-phase abrasive grain polishing and abrupt change tube, in this paper, the fourth order abrupt change tube was selected as the research object, using the fluid mechanics software to simulate,based on the theory of solid-liquid two-phase flow dynamics, study on the mechanism of AFM micromachining a workpiece during polishing.Analysis at different inlet pressures, the dynamic pressure distribution pipe mutant fourth order abrasive flow field, turbulence intensity, discuss the influence of the inlet pressure of different abrasive flow polishing effect.

  18. Solid gas reaction phase diagram under high gas pressure

    International Nuclear Information System (INIS)

    Ishizaki, K.

    1992-01-01

    This paper reports that to evaluate which are the stable phases under high gas pressure conditions, a solid-gas reaction phase diagram under high gas pressure (HIP phase diagram) has been proposed by the author. The variables of the diagram are temperature, reactant gas partial pressure and total gas pressure. Up to the present time the diagrams have been constructed using isobaric conditions. In this work, the stable phases for a real HIP process were evaluated assuming an isochoric condition. To understand the effect of the total gas pressure on stability is of primary importance. Two possibilities were considered and evaluated, those are: the total gas pressure acts as an independent variable, or it only affects the fugacity values. The results of this work indicate that the total gas pressure acts as an independent variable, and in turn also affects the fugacity values

  19. Potassium permanganate and tetraethylammonium chloride are a safe and effective substitute for osmium tetroxide in solid-phase fluorescent chemical cleavage of mismatch.

    OpenAIRE

    Roberts, E; Deeble, V J; Woods, C G; Taylor, G R

    1997-01-01

    Whilst chemical cleavage of mismatch (CCM) detects all point mutations in DNA, its widespread use has been hampered by the complex multistage methodology and the need for toxic chemicals, in particular osmium tetroxide. Here we show that osmium tetroxide can be replaced by potassium permanganate, giving the same spectrum of mutation detection, but with greater sensitivity. The use of potassium permanganate is compatible with solid phase capture and fluorescent detection, giving a safer method...

  20. Determination of Iron Species by Combination of Solvent Assisted-Dispersive Solid Phase Extraction and Spectrophotometry

    Directory of Open Access Journals (Sweden)

    Zahra Dehghani

    2015-06-01

    Full Text Available A simple, rapid and sensitive solvent assisted-dispersive solid phase extraction method was developed for the extraction of iron(II prior to its spectrophotometric determination. The Fe(II reacted with 2,4,6-tris(2-pyridyl-1,3,5-triazine, neutralized with sodium dodecyl sulfate and extracted onto the fine particles of benzophenone which were formed upon rapid injection of a mixture of benzophenone as the sorbent and ethanol as the disperser solvent into the aqueous solution. After phase separation, the sedimented phase containing the complex was dissolved in ethanol and the analyte concentration was determined by measuring its absorption at 594 nm. Total iron was determined after the reduction of Fe(III to Fe(II with hydroxylamine hydrochloride. Under the optimized conditions, an enhancement factor of 32, the detection limit of 0.16 µg l-1, and the relative standard deviation of 1.9% (n = 6 at 20 µg l-1 concentration level of Fe(II were achieved. The method was successfully applied to the determination of iron species in water samples and total iron in infant dry formula milk, apple, rice, spinach and parsley samples.

  1. Improved phase sensitivity in spectral domain phase microscopy using line-field illumination and self phase-referencing

    Science.gov (United States)

    Yaqoob, Zahid; Choi, Wonshik; Oh, Seungeun; Lue, Niyom; Park, Yongkeun; Fang-Yen, Christopher; Dasari, Ramachandra R.; Badizadegan, Kamran; Feld, Michael S.

    2010-01-01

    We report a quantitative phase microscope based on spectral domain optical coherence tomography and line-field illumination. The line illumination allows self phase-referencing method to reject common-mode phase noise. The quantitative phase microscope also features a separate reference arm, permitting the use of high numerical aperture (NA > 1) microscope objectives for high resolution phase measurement at multiple points along the line of illumination. We demonstrate that the path-length sensitivity of the instrument can be as good as 41 pm/Hz, which makes it suitable for nanometer scale study of cell motility. We present the detection of natural motions of cell surface and two-dimensional surface profiling of a HeLa cell. PMID:19550464

  2. Optimizations of large area quasi-solid-state dye-sensitized solar cells

    DEFF Research Database (Denmark)

    Biancardo, M.; West, K.; Krebs, Frederik C

    2006-01-01

    In this paper, we address optimizations of dye sensitized solar cells (DSSCs) through the combination of important issues like semi-transparency, quasi-solid-state constructions and low-cost realization of serially connected modules. DSSCs with a transparency of 50% in the visible region, moderate...... encouraging results. A short circuit current (I-sc) of 4.45 mA cm(-2) with an open circuit voltage (V-oc) of 0.5 V were recorded in standard solar cells sensitized by cis-bis(thiocyano) ruthenium(II)-bis-2, 2'-bipyridine-4, 4'-dicarboxylate. Up-scaling tests demonstrate the easy realization of a 625 cm(2...

  3. Solid phase micro-extraction in environmental atmosphere

    International Nuclear Information System (INIS)

    Tao Ping; Wei Lifan; Tan Yun

    2002-01-01

    Solid phase micro-extraction (SPME) is an advanced technique of sample pretreatment in environmental atmosphere analysis, i.e., a sampling method of extracting volatile organic compounds from environmental gas. According to the primary survey on the theory and application of SPME, a suitable extraction tip, i.e., a coated fused silica fiber, is selected to construct a SPME apparatus. This SPME apparatus is used to extract volatile organic compounds from environmental atmosphere and a qualitative detection is conducted in gas chromatography-mass spectrometer system. Good experimental results are obtained

  4. Application of Solid Phase Extraction on Multiwalled Carbon Nanotubes of Some Heavy Metal Ions to Analysis of Skin Whitening Cosmetics Using ICP-AES

    OpenAIRE

    ALqadami, Ayoub; Abdalla, Mohammad; ALOthman, Zeid; Omer, Kamal

    2013-01-01

    A novel and highly sensitive method for the determination of some heavy metals in skin whitening cosmetics creams using multiwalled carbon nanotubes MWCNTs as solid phase extraction sorbent for the preconcentration of these heavy metals prior to their determination by inductively coupled plasma atomic emission spectrometry is described. Different practical parameters have been thoroughly investigated and the optimum experimental conditions were employed. The developed method was then applied ...

  5. Constant sensitivity circuit for solid state nuclear radiation counters

    International Nuclear Information System (INIS)

    Kronenberg, S.; Erkkila, B.

    1985-01-01

    The utilization of solid state counters in tactical radiological instruments for measuring intensities and doses of fallout gamma rays offers advantages over Geiger-Mueller (GM) counters such as a much wider dynamic range and low operating voltages. Their very small size is suitable for use in miniaturized equipment. However, these devices have a serious problem if used in a mixed, fast neutron/gamma environment such as is encountered e.g. in a battlefield where tactical nuclear weapons are used and neutrons, prompt, initial gammas and fallout gammas are killing factors of comparable importance. Exposure to fast neutrons reduces seriously their sensitivity. This makes the solid state counters at this time unacceptable for use in Army tactical surveillance equipment and in other applications where according to requirements the performance must not be impaired by exposure to fast neutrons. It seems to be possible to reduce to some extent this neutron generated damage by improving the crystal counters

  6. High efficiency solid-state sensitized heterojunction photovoltaic device

    KAUST Repository

    Wang, Mingkui

    2010-06-01

    The high molar extinction coefficient heteroleptic ruthenium dye, NaRu(4,4′-bis(5-(hexylthio)thiophen-2-yl)-2,2′-bipyridine) (4-carboxylic acid-4′-carboxylate-2,2′-bipyridine) (NCS) 2, exhibits certified 5% electric power conversion efficiency at AM 1.5 solar irradiation (100 mW cm-2) in a solid-state dye-sensitized solar cell using 2,2′,7,7′-tetrakis-(N,N-di-pmethoxyphenylamine)-9, 9′-spirobifluorene (spiro-MeOTAD) as the organic hole-transporting material. This demonstration elucidates a class of photovoltaic devices with potential for low-cost power generation. © 2010 Elsevier Ltd. All rights reserved.

  7. High efficiency solid-state sensitized heterojunction photovoltaic device

    KAUST Repository

    Wang, Mingkui; Liu, Jingyuan; Cevey-Ha, Ngoc-Le; Moon, Soo-Jin; Liska, Paul; Humphry-Baker, Robin; Moser, Jacques-E.; Grä tzel, Carole; Wang, Peng; Zakeeruddin, Shaik M.

    2010-01-01

    The high molar extinction coefficient heteroleptic ruthenium dye, NaRu(4,4′-bis(5-(hexylthio)thiophen-2-yl)-2,2′-bipyridine) (4-carboxylic acid-4′-carboxylate-2,2′-bipyridine) (NCS) 2, exhibits certified 5% electric power conversion efficiency at AM 1.5 solar irradiation (100 mW cm-2) in a solid-state dye-sensitized solar cell using 2,2′,7,7′-tetrakis-(N,N-di-pmethoxyphenylamine)-9, 9′-spirobifluorene (spiro-MeOTAD) as the organic hole-transporting material. This demonstration elucidates a class of photovoltaic devices with potential for low-cost power generation. © 2010 Elsevier Ltd. All rights reserved.

  8. Deterministic sensitivity analysis of two-phase flow systems: forward and adjoint methods. Final report

    International Nuclear Information System (INIS)

    Cacuci, D.G.

    1984-07-01

    This report presents a self-contained mathematical formalism for deterministic sensitivity analysis of two-phase flow systems, a detailed application to sensitivity analysis of the homogeneous equilibrium model of two-phase flow, and a representative application to sensitivity analysis of a model (simulating pump-trip-type accidents in BWRs) where a transition between single phase and two phase occurs. The rigor and generality of this sensitivity analysis formalism stem from the use of Gateaux (G-) differentials. This report highlights the major aspects of deterministic (forward and adjoint) sensitivity analysis, including derivation of the forward sensitivity equations, derivation of sensitivity expressions in terms of adjoint functions, explicit construction of the adjoint system satisfied by these adjoint functions, determination of the characteristics of this adjoint system, and demonstration that these characteristics are the same as those of the original quasilinear two-phase flow equations. This proves that whenever the original two-phase flow problem is solvable, the adjoint system is also solvable and, in principle, the same numerical methods can be used to solve both the original and adjoint equations

  9. Gold catalyzed nickel disilicide formation: a new solid-liquid-solid phase growth mechanism.

    Science.gov (United States)

    Tang, Wei; Picraux, S Tom; Huang, Jian Yu; Liu, Xiaohua; Tu, K N; Dayeh, Shadi A

    2013-01-01

    The vapor-liquid-solid (VLS) mechanism is the predominate growth mechanism for semiconductor nanowires (NWs). We report here a new solid-liquid-solid (SLS) growth mechanism of a silicide phase in Si NWs using in situ transmission electron microcopy (TEM). The new SLS mechanism is analogous to the VLS one in relying on a liquid-mediating growth seed, but it is fundamentally different in terms of nucleation and mass transport. In SLS growth of Ni disilicide, the Ni atoms are supplied from remote Ni particles by interstitial diffusion through a Si NW to the pre-existing Au-Si liquid alloy drop at the tip of the NW. Upon supersaturation of both Ni and Si in Au, an octahedral nucleus of Ni disilicide (NiSi2) forms at the center of the Au liquid alloy, which thereafter sweeps through the Si NW and transforms Si into NiSi2. The dissolution of Si by the Au alloy liquid mediating layer proceeds with contact angle oscillation at the triple point where Si, oxide of Si, and the Au alloy meet, whereas NiSi2 is grown from the liquid mediating layer in an atomic stepwise manner. By using in situ quenching experiments, we are able to measure the solubility of Ni and Si in the Au-Ni-Si ternary alloy. The Au-catalyzed mechanism can lower the formation temperature of NiSi2 by 100 °C compared with an all solid state reaction.

  10. In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

    Science.gov (United States)

    Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

    2015-12-18

    A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Ely, T. M.; LaMothe, M. E.; Lachut, J. S.

    2016-01-01

    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.

  12. [Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

    Science.gov (United States)

    Lü, Weichao; Shen, Shuchang; Wang, Chao

    2017-11-08

    With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

  13. Gibbs Energy Modeling of Digenite and Adjacent Solid-State Phases

    Science.gov (United States)

    Waldner, Peter

    2017-08-01

    All sulfur potential and phase diagram data available in the literature for solid-state equilibria related to digenite have been assessed. Thorough thermodynamic analysis at 1 bar total pressure has been performed. A three-sublattice approach has been developed to model the Gibbs energy of digenite as a function of composition and temperature using the compound energy formalism. The Gibbs energies of the adjacent solid-state phases covelitte and high-temperature chalcocite are also modeled treating both sulfides as stoichiometric compounds. The novel model for digenite offers new interpretation of experimental data, may contribute from a thermodynamic point of view to the elucidation of the role of copper species within the crystal structure and allows extrapolation to composition regimes richer in copper than stoichiometric digenite Cu2S. Preliminary predictions into the ternary Cu-Fe-S system at 1273 K (1000 °C) using the Gibbs energy model of digenite for calculating its iron solubility are promising.

  14. Analysis of urinary neurotransmitters by capillary electrophoresis: Sensitivity enhancement using field-amplified sample injection and molecular imprinted polymer solid phase extraction

    International Nuclear Information System (INIS)

    Claude, Berengere; Nehme, Reine; Morin, Philippe

    2011-01-01

    of the FASI/CE-UV method.Therefore, a solid phase extraction (SPE) on a dedicated imprinted polymer (MIP) was developed to extract specific neurotransmitters, catecholamines, metanephrines and indolamines, from urine. Matrix salts were thus discarded after sample extraction on AFFINIMIP TM Catecholamine and Metanephrine (100 mg) cartridge. Therefore, lower limits of quantification were determined in artificial urine (46 nmol L -1 for DA, 11 nmol L -1 for 3-MT and 6 nmol L -1 for 5-HT).The application of this protocol MIP-SPE/FASI-CE-UV analysis of neurotransmitters in human urine gave rise to electropherograms with a very good base line and signal to noise ratios above 15.

  15. Analysis of urinary neurotransmitters by capillary electrophoresis: Sensitivity enhancement using field-amplified sample injection and molecular imprinted polymer solid phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Claude, Berengere, E-mail: berengere.claude@univ-orleans.fr [Institut de Chimie Organique et Analytique, CNRS FR 2708 UMR 6005, Universite d' Orleans, 45067 Orleans (France); Nehme, Reine; Morin, Philippe [Institut de Chimie Organique et Analytique, CNRS FR 2708 UMR 6005, Universite d' Orleans, 45067 Orleans (France)

    2011-08-12

    neurotransmitters in urine, the presence of salts in the matrix greatly reduces the sensitivity of the FASI/CE-UV method.Therefore, a solid phase extraction (SPE) on a dedicated imprinted polymer (MIP) was developed to extract specific neurotransmitters, catecholamines, metanephrines and indolamines, from urine. Matrix salts were thus discarded after sample extraction on AFFINIMIP{sup TM} Catecholamine and Metanephrine (100 mg) cartridge. Therefore, lower limits of quantification were determined in artificial urine (46 nmol L{sup -1} for DA, 11 nmol L{sup -1} for 3-MT and 6 nmol L{sup -1} for 5-HT).The application of this protocol MIP-SPE/FASI-CE-UV analysis of neurotransmitters in human urine gave rise to electropherograms with a very good base line and signal to noise ratios above 15.

  16. Controlled phase gate for solid-state charge-qubit architectures

    International Nuclear Information System (INIS)

    Schirmer, S.G.; Oi, D.K.L.; Greentree, Andrew D.

    2005-01-01

    We describe a mechanism for realizing a controlled phase gate for solid-state charge qubits. By augmenting the positionally defined qubit with an auxiliary state, and changing the charge distribution in the three-dot system, we are able to effectively switch the Coulombic interaction, effecting an entangling gate. We consider two architectures, and numerically investigate their robustness to gate noise

  17. Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

    Energy Technology Data Exchange (ETDEWEB)

    Moon, Sung Won [KIST Gangneung Institute, Gangneung (Korea, Republic of); Ham, Jungyeob [Gangneung-Wonju National University, Gangneung (Korea, Republic of); Chang, Young-Tae [National University of Singapore, Singapore (Singapore); Lee, Jae Wook [University of Science and Technology, Daejon (Korea, Republic of)

    2015-01-15

    In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds.

  18. Solid-phase Synthesis of Combinatorial 2,4-Disubstituted-1,3,5-Triazine via Amine Nucleophilic Reaction

    International Nuclear Information System (INIS)

    Moon, Sung Won; Ham, Jungyeob; Chang, Young-Tae; Lee, Jae Wook

    2015-01-01

    In combinatorial chemistry, solid-phase synthesis is a popular approach formass production of small molecules. Compared to solution-phase synthesis, it is easy to prepare and purify a large number of heterocyclic small molecules via solid-phase chemistry; the overall reaction time is decreased as well. 1,3,5-Triazine is a nitrogen-containing heterocyclic aromatic scaffold that was shown to be a druggable scaffold in recent studies. These structures have been reported as anticancer, antimicrobial, and antiretroviral compounds, as CDKs and p38 MAP kinase inhibitors, as estrogen receptor modulators, and as inosine monophosphate dehydrogenase inhibitors. we designed and synthesized disubstituted triazine compounds as an analog of disubstituted pyrimidine compounds. These disubstituted triazine compounds possess a linear structure which may have biological activity similar to that of disubstituted pyrimidine. Here we report the solid-phase synthesis of disubstituted triazine compounds

  19. Linkers, resins, and general procedures for solid-phase peptide synthesis

    DEFF Research Database (Denmark)

    Shelton, Anne Pernille Tofteng; Jensen, Knud Jørgen

    2013-01-01

    and linkers for solid-phase synthesis is a key parameter for successful peptide synthesis. This chapter provides an overview of the most common and useful resins and linkers for the synthesis of peptides with C-terminal amides, carboxylic acids, and more. The chapter finishes with robust protocols for general...

  20. Solid-Phase Microextraction Coupled to Capillary Atmospheric Pressure Photoionization-Mass Spectrometry for Direct Analysis of Polar and Nonpolar Compounds.

    Science.gov (United States)

    Mirabelli, Mario F; Zenobi, Renato

    2018-04-17

    A novel capillary ionization source based on atmospheric pressure photoionization (cAPPI) was developed and used for the direct interfacing between solid-phase microextraction (SPME) and mass spectrometry (MS). The efficiency of the source was evaluated for direct and dopant-assisted photoionization, analyzing both polar (e.g., triazines and organophosphorus pesticides) and nonpolar (polycyclic aromatic hydrocarbons, PAHs) compounds. The results show that the range of compound polarity, which can be addressed by direct SPME-MS can be substantially extended by using cAPPI, compared to other sensitive techniques like direct analysis in real time (DART) and dielectric barrier discharge ionization (DBDI). The new source delivers a very high sensitivity, down to sub parts-per-trillion (ppt), making it a viable alternative when compared to previously reported and less comprehensive direct approaches.

  1. Binding of properdin to solid-phase immune complexes

    DEFF Research Database (Denmark)

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

    1998-01-01

    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...... fixed to IC was the principal ligand for properdin in the assay. The findings could have biological implications relating to complement-mediated modification of immune complexes in disease....

  2. Influence of pressure on the solid state phase transformation of Cu–Al–Bi alloy

    International Nuclear Information System (INIS)

    Gong, Li; Jian-Hua, Liu; Wen-Kui, Wang; Ri-Ping, Liu

    2010-01-01

    The solid state phase transformation of Cu-Al-Bi alloy under high pressure was investigated by x-ray diffraction, energy dispersive spectroscopy and transmission electron microscopy. Experimental results show that the initial crystalline phase in the Cu-Al-Bi alloy annealed at 750 °C under the pressures in the range of 0–6 GPa is α-Cu solid solution (named as α-Cu phase below), and high pressure has a great influence on the crystallisation process of the Cu-Al-Bi alloy. The grain size of the α-Cu phase decreases with increasing pressure as the pressure is below about 3 GPa, and then increases (P > 3 GPa). The mechanism for the effects of high pressure on the crystallisation process of the alloy has been discussed. (condensed matter: structure, thermal and mechanical properties)

  3. Solid-phase PCR for rapid multiplex detection of Salmonella spp. at the subspecies level, with amplification efficiency comparable to conventional PCR

    DEFF Research Database (Denmark)

    Chin, Wai Hoe; Sun, Yi; Høgberg, Jonas

    2017-01-01

    Solid-phase PCR (SP-PCR) has attracted considerable interest in different research fields since it allows parallel DNA amplification on the surface of a solid substrate. However, the applications of SP-PCR have been hampered by the low efficiency of the solid-phase amplification. In order to incr...... diagnosis, high-throughput DNA sequencing, and single-nucleotide polymorphism analysis. Graphical abstract Schematic representation of solid-phase PCR....

  4. General approach to standardization of the solid-phase radioimmunoassay for quantitation of class-specific antibodies

    Energy Technology Data Exchange (ETDEWEB)

    Zollinger, W D; Boslego, J W [Walter Reed Army Inst. of Research, Washington, DC (USA)

    1981-10-30

    The feasibility of using an anti-human immunoglobulin/human immunoglobulin/(/sup 125/I)anti-human immunoglobulin 'sandwich' in a solid-phase radioimmunoassay to produce a standard curve which could be used to quantitate antigen-specific antibody of a particular immunoglobulin class was investigated. The amount of secondary antibody (SAb) bound was determined as a function of whether the primary antibody (PAb) was bound to its specific solid-phase antigen or by a solid-phase anti-human immunoglobulin. No significant difference between the two values was observed. Quantitation of anti-tetanus toxoid antibody by this method was in a good agreement with quantitative precipitin tests. Comparison of SAb binding as a function of the way the PAb is bound was extended to class-specific PAb by use of murine monoclonal antibodies to meningococcal antigens. In most cases somewhat greater binding of SAb occurred when PAb was bound to antigen, but in several cases where low avidity antibody and/or poor quality antigens were used, greater SAb binding occurred when PAb was bound by anti-mouse immunoglobulin. The results indicate that this approach may be useful as a general method for standardizing the SPRIA and other solid-phase immunoassays such as the ELISA to measure class-specific antibody.

  5. Micro versus macro solid phase extraction for monitoring water contaminants: a preliminary study using trihalomethanes.

    Science.gov (United States)

    Alexandrou, Lydon D; Spencer, Michelle J S; Morrison, Paul D; Meehan, Barry J; Jones, Oliver A H

    2015-04-15

    Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental science. However, traditional methods need electrically powered pumps, can use large volumes of solvent (if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and provides comparable concentration factors to established methods. It is also an enclosed system so volatile components are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required. However, the technology is new and has not been much used for environmental analysis. In this study we compare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile trihalomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane). The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with similar recovery rates for the target compounds. This method shows potential for further development in a range of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

    International Nuclear Information System (INIS)

    Pourreza, N.

    2004-01-01

    Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

  7. Quantum computational capability of a 2D valence bond solid phase

    International Nuclear Information System (INIS)

    Miyake, Akimasa

    2011-01-01

    Highlights: → Our model is the 2D valence bond solid phase of a quantum antiferromagnet. → Universal quantum computation is processed by measurements of quantum correlations. → An intrinsic complexity of strongly-correlated quantum systems could be a resource. - Abstract: Quantum phases of naturally-occurring systems exhibit distinctive collective phenomena as manifestation of their many-body correlations, in contrast to our persistent technological challenge to engineer at will such strong correlations artificially. Here we show theoretically that quantum correlations exhibited in the 2D valence bond solid phase of a quantum antiferromagnet, modeled by Affleck, Kennedy, Lieb, and Tasaki (AKLT) as a precursor of spin liquids and topological orders, are sufficiently complex yet structured enough to simulate universal quantum computation when every single spin can be measured individually. This unveils that an intrinsic complexity of naturally-occurring 2D quantum systems-which has been a long-standing challenge for traditional computers-could be tamed as a computationally valuable resource, even if we are limited not to create newly entanglement during computation. Our constructive protocol leverages a novel way to herald the correlations suitable for deterministic quantum computation through a random sampling, and may be extensible to other ground states of various 2D valence bond phases beyond the AKLT state.

  8. Structural study of chlorine tri-fluoride and bromine penta-fluoride in liquid and solid phase

    International Nuclear Information System (INIS)

    Rousson, R.

    1973-01-01

    This research thesis reports the structural study of chlorine tri-fluoride and bromine penta-fluoride between 20 C and about -265 C. After some generalities on these compounds and a presentation of the experimental technique, the author reports and discusses results obtained with these both compounds: Raman spectrum for the liquid and for the solid phase, infrared spectrum for the solid phase, calorimetric measurements. In the case of chlorine tri-fluoride, the author studies the evolution of the liquid spectrum with temperature, shows the existence of an intermediate solid phase, and compares results obtained by Raman spectroscopy and nuclear magnetic resonance. He also applies to bromine penta-fluoride an analysis of normal coordinates of a XF 5 molecule: relationship between force constants and vibration frequencies, application of Wilson method, resolution of the molecular equation, determination of normal vibration modes [fr

  9. Microencapsulated Comb-Like Polymeric Solid-Solid Phase Change Materials via In-Situ Polymerization

    Directory of Open Access Journals (Sweden)

    Wei Li

    2018-02-01

    Full Text Available To enhance the thermal stability and permeability resistance, a comb-like polymer with crystallizable side chains was fabricated as solid-solid phase change materials (PCMs inside the cores of microcapsules and nanocapsules prepared via in-situ polymerization. In this study, the effects on the surface morphology and microstructure of micro/nanocapsules caused by microencapsulating different types of core materials (i.e., n-hexadecane, ethyl hexadecanoate, hexadecyl acrylate and poly(hexadecyl acrylate were systematically studied via field emission scanning electron microscope (FE-SEM and transmission electron microscope (TEM. The confined crystallization behavior of comb-like polymer PCMs cores was investigated via differential scanning calorimeter (DSC. Comparing with low molecular organic PCMs cores, the thermal stability of PCMs microencapsulated comb-like polymer enhanced significantly, and the permeability resistance improved obviously as well. Based on these resultant analysis, the microencapsulated comb-like polymeric PCMs with excellent thermal stability and permeability resistance showed promising foreground in the field of organic solution spun, melt processing and organic coating.

  10. Thermal conductivity of solid cyclohexane in orientationally ordered and disordered phases

    International Nuclear Information System (INIS)

    Konstantinov, V. A.; Revyakin, V. P.; Sagan, V. V.; Pursky, O. I.; Sysoev, V. M.

    2011-01-01

    Thermal conductivity Λ P of solid cyclohexane is measured at a pressure P = 0.1 MPa in the temperature range from 80 K to the melting point, which covers the ranges of low-temperature orientationally ordered phase II and high-temperature orientationally disordered phase I. Thermal conductivity Λ V is measured at a constant volume in orientationally disordered phase I. The thermal conductivity measured at atmospheric pressure decreases with increasing temperature as Λ P ∝ T −1.15 in phase II, whereas Λ P ∝ T −0.3 in phase I. As temperature increases, isochoric thermal conductivity Λ V in phase I increases gradually. The experimental data are described in terms of a modified Debye model of thermal conductivity with allowance for heat transfer by both phonons and “diffuse” modes.

  11. Auditory cortical neurons are sensitive to static and continuously changing interaural phase cues.

    Science.gov (United States)

    Reale, R A; Brugge, J F

    1990-10-01

    1. The interaural-phase-difference (IPD) sensitivity of single neurons in the primary auditory (AI) cortex of the anesthetized cat was studied at stimulus frequencies ranging from 120 to 2,500 Hz. Best frequencies of the 43 AI cells sensitive to IPD ranged from 190 to 2,400 Hz. 2. A static IPD was produced when a pair of low-frequency tone bursts, differing from one another only in starting phase, were presented dichotically. The resulting IPD-sensitivity curves, which plot the number of discharges evoked by the binaural signal as a function of IPD, were deeply modulated circular functions. IPD functions were analyzed for their mean vector length (r) and mean interaural phase (phi). Phase sensitivity was relatively independent of best frequency (BF) but highly dependent on stimulus frequency. Regardless of BF or stimulus frequency within the excitatory response area the majority of cells fired maximally when the ipsilateral tone lagged the contralateral signal and fired least when this interaural-phase relationship was reversed. 3. Sensitivity to continuously changing IPD was studied by delivering to the two ears 3-s tones that differed slightly in frequency, resulting in a binaural beat. Approximately 26% of the cells that showed a sensitivity to static changes in IPD also showed a sensitivity to dynamically changing IPD created by this binaural tonal combination. The discharges were highly periodic and tightly synchronized to a particular phase of the binaural beat cycle. High synchrony can be attributed to the fact that cortical neurons typically respond to an excitatory stimulus with but a single spike that is often precisely timed to stimulus onset. A period histogram, binned on the binaural beat frequency (fb), produced an equivalent IPD-sensitivity function for dynamically changing interaural phase. For neurons sensitive to both static and continuously changing interaural phase there was good correspondence between their static (phi s) and dynamic (phi d

  12. IN SITU SOLID-PHASE EXTRACTION AND ANALYSIS OF ...

    Science.gov (United States)

    Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of 1-L samples. A 1-L sample, however, usually provides too little analyte for full-scan data acquisition.We have developed an on-site extraction method for extracting synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for various synthetic musk compounds. Quantification of these compounds was conveniently achieved from the full-scan data directly, without preparing SIM descriptors for each compound to acquire SIM data. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-s

  13. Solid thermoluminescent dosemeter of sodium tetraborate and brazilian fluoride sensitive to thermal neutrons

    International Nuclear Information System (INIS)

    Fratin, L.

    1988-01-01

    The techniques of compacting sodium tetraborate and natural fluoride mixtures were studied in this work, with the aim of producing a solid dosimeter sensitive to thermal neutrons. The production procedure involves the vitrification of the sodium tetraborate, the grinding, mixture, cold pressing and the sinterization of the pellets. A special arrangement was built for irradiation where paraffin was used as moderator for neutrons from a 241 Am-Be source. Two different mass ratios of sodium tetraborate and flourite showed a linear thermoluminescent response to the neutron fluence in the range of 1.0 to 7.0 x 10 8 n (sub)tcm -2 . Solid dosimeters, manufactured from natural fluorite and sodium chloride, showed a response to gamma radiation similar to the response of the dosimeters sensitive to neutrons. These dosimeters are need to identify the proportion of thermoluminescent response due to gamma radiation present in a neutron field. (author) [pt

  14. Modeling of Thermal Phase Noise in a Solid Core Photonic Crystal Fiber-Optic Gyroscope.

    Science.gov (United States)

    Song, Ningfang; Ma, Kun; Jin, Jing; Teng, Fei; Cai, Wei

    2017-10-26

    A theoretical model of the thermal phase noise in a square-wave modulated solid core photonic crystal fiber-optic gyroscope has been established, and then verified by measurements. The results demonstrate a good agreement between theory and experiment. The contribution of the thermal phase noise to the random walk coefficient of the gyroscope is derived. A fiber coil with 2.8 km length is used in the experimental solid core photonic crystal fiber-optic gyroscope, showing a random walk coefficient of 9.25 × 10 -5 deg/√h.

  15. Solid-phase synthesis of head and tail bis-acridinylated peptides

    Czech Academy of Sciences Publication Activity Database

    Šebestík, Jaroslav; Matějka, P.; Hlaváček, Jan; Stibor, I.

    2004-01-01

    Roč. 45, č. 6 (2004), s. 1203-1205 ISSN 0040-4039 R&D Projects: GA ČR GA203/02/1379 Institutional research plan: CEZ:AV0Z4055905 Keywords : 9-amino acridine * solid phase synthesis * head and tail peptide conjugates Subject RIV: CC - Organic Chemistry Impact factor: 2.484, year: 2004

  16. Phase Evolution and Mechanical Behavior of the Semi-Solid SIMA Processed 7075 Aluminum Alloy

    Directory of Open Access Journals (Sweden)

    Behzad Binesh

    2016-02-01

    Full Text Available Microstructural and mechanical behaviors of semi-solid 7075 aluminum alloy were investigated during semi-solid processing. The strain induced melt activation (SIMA process consisted of applying uniaxial compression strain at ambient temperature and subsequent semi-solid treatment at 600–620 °C for 5–35 min. Microstructures were characterized by scanning electron microscope (SEM, energy dispersive spectroscopy (EDS, and X-ray diffraction (XRD. During the isothermal heating, intermetallic precipitates were gradually dissolved through the phase transformations of α-Al + η (MgZn2 → liquid phase (L and then α-Al + Al2CuMg (S + Mg2Si → liquid phase (L. However, Fe-rich precipitates appeared mainly as square particles at the grain boundaries at low heating temperatures. Cu and Si were enriched at the grain boundaries during the isothermal treatment while a significant depletion of Mg was also observed at the grain boundaries. The mechanical behavior of different SIMA processed samples in the semi-solid state were investigated by means of hot compression tests. The results indicated that the SIMA processed sample with near equiaxed microstructure exhibits the highest flow resistance during thixoforming which significantly decreases in the case of samples with globular microstructures. This was justified based on the governing deformation mechanisms for different thixoformed microstructures.

  17. Traveltime sensitivity kernels for wave equation tomography using the unwrapped phase

    KAUST Repository

    Djebbi, Ramzi

    2014-02-18

    Wave equation tomography attempts to improve on traveltime tomography, by better adhering to the requirements of our finite-frequency data. Conventional wave equation tomography, based on the first-order Born approximation followed by cross-correlation traveltime lag measurement, or on the Rytov approximation for the phase, yields the popular hollow banana sensitivity kernel indicating that the measured traveltime at a point is insensitive to perturbations along the ray theoretical path at certain finite frequencies. Using the instantaneous traveltime, which is able to unwrap the phase of the signal, instead of the cross-correlation lag, we derive new finite-frequency traveltime sensitivity kernels. The kernel reflects more the model-data dependency, we typically encounter in full waveform inversion. This result confirms that the hollow banana shape is borne of the cross-correlation lag measurement, which exposes the Born approximations weakness in representing transmitted waves. The instantaneous traveltime can thus mitigate the additional component of nonlinearity introduced by the hollow banana sensitivity kernels in finite-frequency traveltime tomography. The instantaneous traveltime simply represents the unwrapped phase of Rytov approximation, and thus is a good alternative to Born and Rytov to compute the misfit function for wave equation tomography. We show the limitations of the cross-correlation associated with Born approximation for traveltime lag measurement when the source signatures of the measured and modelled data are different. The instantaneous traveltime is proven to be less sensitive to the distortions in the data signature. The unwrapped phase full banana shape of the sensitivity kernels shows smoother update compared to the banana–doughnut kernels. The measurement of the traveltime delay caused by a small spherical anomaly, embedded into a 3-D homogeneous model, supports the full banana sensitivity assertion for the unwrapped phase.

  18. Traveltime sensitivity kernels for wave equation tomography using the unwrapped phase

    KAUST Repository

    Djebbi, Ramzi; Alkhalifah, Tariq Ali

    2014-01-01

    Wave equation tomography attempts to improve on traveltime tomography, by better adhering to the requirements of our finite-frequency data. Conventional wave equation tomography, based on the first-order Born approximation followed by cross-correlation traveltime lag measurement, or on the Rytov approximation for the phase, yields the popular hollow banana sensitivity kernel indicating that the measured traveltime at a point is insensitive to perturbations along the ray theoretical path at certain finite frequencies. Using the instantaneous traveltime, which is able to unwrap the phase of the signal, instead of the cross-correlation lag, we derive new finite-frequency traveltime sensitivity kernels. The kernel reflects more the model-data dependency, we typically encounter in full waveform inversion. This result confirms that the hollow banana shape is borne of the cross-correlation lag measurement, which exposes the Born approximations weakness in representing transmitted waves. The instantaneous traveltime can thus mitigate the additional component of nonlinearity introduced by the hollow banana sensitivity kernels in finite-frequency traveltime tomography. The instantaneous traveltime simply represents the unwrapped phase of Rytov approximation, and thus is a good alternative to Born and Rytov to compute the misfit function for wave equation tomography. We show the limitations of the cross-correlation associated with Born approximation for traveltime lag measurement when the source signatures of the measured and modelled data are different. The instantaneous traveltime is proven to be less sensitive to the distortions in the data signature. The unwrapped phase full banana shape of the sensitivity kernels shows smoother update compared to the banana–doughnut kernels. The measurement of the traveltime delay caused by a small spherical anomaly, embedded into a 3-D homogeneous model, supports the full banana sensitivity assertion for the unwrapped phase.

  19. Recent Developments in Solid-Phase Extraction for Near and Attenuated Total Reflection Infrared Spectroscopic Analysis

    Directory of Open Access Journals (Sweden)

    Christian W. Huck

    2016-05-01

    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.

  20. Transport mechanisms and wetting dynamics in molecularly thin films of long-chain alkanes at solid/vapour interface : relation to the solid-liquid phase transition

    OpenAIRE

    Lazar, Paul

    2005-01-01

    Wetting and phase transitions play a very important role our daily life. Molecularly thin films of long-chain alkanes at solid/vapour interfaces (e.g. C30H62 on silicon wafers) are very good model systems for studying the relation between wetting behaviour and (bulk) phase transitions. Immediately above the bulk melting temperature the alkanes wet partially the surface (drops). In this temperature range the substrate surface is covered with a molecularly thin ordered, solid-like alkane film (...

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

    Science.gov (United States)

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

    2018-03-01

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

  2. Computer-aided design model for anaerobic-phased-solids digester system

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Z.; Zhang, R. [University of California, Davis, CA (United States); Tiangco, V. [California Energy Commission, Sacramento, CA (United States)

    1999-07-01

    The anaerobic-phased-solids (APS) digester system is a newly developed anaerobic digestion system for converting solid wastes, such as crop residues and food wastes, into biogas for power and heat generation. A computer-aided engineering design model has been developed to design the APS-digester system and study the heat transfer from the reactors and energy production of the system. Simulation results of a case study are presented by using the model to predict the heating energy requirement and biogas energy production for anaerobic digestion of garlic waste. The important factors, such as environmental conditions, insulation properties, and characteristics of the wastes, on net energy production are also investigated. (author)

  3. Evaluation of a Solid Phase DNA Binding Matrix for Downstream PCR Analysis

    National Research Council Canada - National Science Library

    Bader, Douglas E; Fisher, Glen R; Stratilo, Chad W

    2005-01-01

    A commercially available solid-phase DNA binding matrix (FTA cards) was evaluated for its ability to capture and release DNA for downstream gene amplification and detection assays using polymerase chain reaction (PCR...

  4. Technical note: New applications for on-line automated solid phase extraction

    OpenAIRE

    MacFarlane, John D.

    1997-01-01

    This technical note explains the disadvantages of manual solid phase extraction (SPE) techniques and the benefits to be gained with automatic systems. The note reports on a number of general and highly specific applications using the Sample Preparation Unit OSP-2A.

  5. Sol-gel titania-coated needles for solid phase dynamic extraction-GC/MS analysis of desomorphine and desocodeine.

    Science.gov (United States)

    Su, Chi-Ju; Srimurugan, Sankarewaran; Chen, Chinpiao; Shu, Hun-Chi

    2011-01-01

    Novel sol-gel titania film coated needles for solid-phase dynamic extraction (SPDE)-GC/MS analysis of desomorphine and desocodeine are described. The high thermal stability of titania film permits efficient extraction and analysis of poorly volatile opiate drugs. The influences of sol-gel reaction time, coating layer, extraction and desorption time and temperature on the SPDE needle performance were investigated. The deuterium labeled internal standard was introduced either during the extraction of analyte or directly injected to GC after the extraction process. The latter method was shown to be more sensitive for the analysis of water and urine samples containing opiate drugs. The proposed conditions provided a wide linear range (from 5-5000 ppb), and satisfactory linearity, with R(2) values from 0.9958 to 0.9999, and prominent sensitivity, LOQs (1.0-5.0 ng/g). The sol-gel titania film coated needle with SPDE-GC/MS will be a promising technique for desomorphine and desocodeine analysis in urine.

  6. Measurement of IgG antibodies to house dust mite and grass pollen by a solid-phase radioimmunoassay

    Energy Technology Data Exchange (ETDEWEB)

    Delespesse, G; Debisschop, M J; Flament, J [Hopital Saint Pierre, Louvain (Belgium). Lab. de Recherches de la Clinique Medicale

    1979-09-01

    A solid-phase radioimmunoassay was used to measure specific IgG antibodies to either Dermatophagoides pteronyssinus (DPT) or grass pollens. Radiolabelled protein A from Staphylococcus aureus (SpA) was used to determine the IgG antibodies attached to the microtubes. The binding of IgG from either normal or allergic sera to DPT-coated tubes was antigen specific and mediated by the Fab fragment of the immunoglobulin. IgG antibodies from non-allergic serum competed with IgE antibodies to DPT. IgE antibodies did not significantly interfere with the assay. Indeed heating a reaginic serum resulted in a striking reduction of the (/sup 125/I) anti- IgE binding to allergen-coated tubes without modifying the (/sup 125/I)-SpA binding. Furthermore, filtration of a reaginic serum through Sephacryl S-200 separated a peak of IgE antibodies. The solid phase method was more sensitive than a double-antibody technique employing the same DPT extract as labelled antigen. Non-allergic subjects had less IgG antibodies to DPT or grass pollens than allergic patients. In untreated patients, there was a good correlation between levels of IgG and IgE antibodies to grass pollens but not to DPT. Patients hyposensitized to house dust mite had on the average three times more specific IgG antibodies than untreated cases. (author).

  7. Measurement of IgG antibodies to house dust mite and grass pollen by a solid-phase radioimmunoassay

    International Nuclear Information System (INIS)

    Delespesse, G.; Debisschop, M.J.; Flament, J.

    1979-01-01

    A solid-phase radioimmunoassay was used to measure specific IgG antibodies to either Dermatophagoides pteronyssinus (DPT) or grass pollens. Radiolabelled protein A from Staphylococcus aureus (SpA) was used to determine the IgG antibodies attached to the microtubes. The binding of IgG from either normal or allergic sera to DPT-coated tubes was antigen specific and mediated by the Fab fragment of the immunoglobulin. IgG antibodies from non-allergic serum competed with IgE antibodies to DPT. IgE antibodies did not significantly interfere with the assay. Indeed heating a reaginic serum resulted in a striking reduction of the ( 125 I) anti- IgE binding to allergen-coated tubes without modifying the ( 125 I)-SpA binding. Furthermore, filtration of a reaginic serum through Sephacryl S-200 separated a peak of IgE antibodies. The solid phase method was more sensitive than a double-antibody technique employing the same DPT extract as labelled antigen. Non-allergic subjects had less IgG antibodies to DPT or grass pollens than allergic patients. In untreated patients, there was a good correlation between levels of IgG and IgE antibodies to grass pollens but not to DPT. Patients hyposensitized to house dust mite had on the average three times more specific IgG antibodies than untreated cases. (author)

  8. Determination of quaternary ammonium compounds in seawater samples by solid-phase extraction and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Bassarab, P; Williams, D; Dean, J R; Ludkin, E; Perry, J J

    2011-02-04

    A method for the simultaneous determination of two biocidal quaternary ammonium compounds; didecyldimethylammonium chloride (didecyldimethyl quat) and dodecylbenzyldimethylammonium chloride (benzyl quat), in seawater by solid phase extraction (SPE) followed by liquid chromatography-mass spectrometry (LC-MS) was developed. The optimised procedure utilised off-line extraction of the analytes from seawater using polymeric (Strata-X) SPE cartridges. Recoveries ranged from 80 to 105%, with detection limits at the low parts-per-trillion (ng/l) level for both analytes. To demonstrate sensitivity, environmental concentrations were measured at three different locations along the North East coast of England with measured values in the range 120-270ng/l. Copyright © 2010 Elsevier B.V. All rights reserved.

  9. Simulating mixed-phase Arctic stratus clouds: sensitivity to ice initiation mechanisms

    Directory of Open Access Journals (Sweden)

    G. McFarquhar

    2009-07-01

    Full Text Available The importance of Arctic mixed-phase clouds on radiation and the Arctic climate is well known. However, the development of mixed-phase cloud parameterization for use in large scale models is limited by lack of both related observations and numerical studies using multidimensional models with advanced microphysics that provide the basis for understanding the relative importance of different microphysical processes that take place in mixed-phase clouds. To improve the representation of mixed-phase cloud processes in the GISS GCM we use the GISS single-column model coupled to a bin resolved microphysics (BRM scheme that was specially designed to simulate mixed-phase clouds and aerosol-cloud interactions. Using this model with the microphysical measurements obtained from the DOE ARM Mixed-Phase Arctic Cloud Experiment (MPACE campaign in October 2004 at the North Slope of Alaska, we investigate the effect of ice initiation processes and Bergeron-Findeisen process (BFP on glaciation time and longevity of single-layer stratiform mixed-phase clouds. We focus on observations taken during 9–10 October, which indicated the presence of a single-layer mixed-phase clouds. We performed several sets of 12-h simulations to examine model sensitivity to different ice initiation mechanisms and evaluate model output (hydrometeors' concentrations, contents, effective radii, precipitation fluxes, and radar reflectivity against measurements from the MPACE Intensive Observing Period. Overall, the model qualitatively simulates ice crystal concentration and hydrometeors content, but it fails to predict quantitatively the effective radii of ice particles and their vertical profiles. In particular, the ice effective radii are overestimated by at least 50%. However, using the same definition as used for observations, the effective radii simulated and that observed were more comparable. We find that for the single-layer stratiform mixed-phase clouds simulated, process

  10. Simulating mixed-phase Arctic stratus clouds: sensitivity to ice initiation mechanisms

    Science.gov (United States)

    Sednev, I.; Menon, S.; McFarquhar, G.

    2009-07-01

    The importance of Arctic mixed-phase clouds on radiation and the Arctic climate is well known. However, the development of mixed-phase cloud parameterization for use in large scale models is limited by lack of both related observations and numerical studies using multidimensional models with advanced microphysics that provide the basis for understanding the relative importance of different microphysical processes that take place in mixed-phase clouds. To improve the representation of mixed-phase cloud processes in the GISS GCM we use the GISS single-column model coupled to a bin resolved microphysics (BRM) scheme that was specially designed to simulate mixed-phase clouds and aerosol-cloud interactions. Using this model with the microphysical measurements obtained from the DOE ARM Mixed-Phase Arctic Cloud Experiment (MPACE) campaign in October 2004 at the North Slope of Alaska, we investigate the effect of ice initiation processes and Bergeron-Findeisen process (BFP) on glaciation time and longevity of single-layer stratiform mixed-phase clouds. We focus on observations taken during 9-10 October, which indicated the presence of a single-layer mixed-phase clouds. We performed several sets of 12-h simulations to examine model sensitivity to different ice initiation mechanisms and evaluate model output (hydrometeors' concentrations, contents, effective radii, precipitation fluxes, and radar reflectivity) against measurements from the MPACE Intensive Observing Period. Overall, the model qualitatively simulates ice crystal concentration and hydrometeors content, but it fails to predict quantitatively the effective radii of ice particles and their vertical profiles. In particular, the ice effective radii are overestimated by at least 50%. However, using the same definition as used for observations, the effective radii simulated and that observed were more comparable. We find that for the single-layer stratiform mixed-phase clouds simulated, process of ice phase initiation

  11. ''reverse'' solid-phase radioimmunoasssay for IgM-antibodies to hepatitis A virus

    Energy Technology Data Exchange (ETDEWEB)

    Meurman, O H; Matter, L; Krishna, R V; Krech, U H [Institute of Medical Microbiology, St. Gallen, Switzerland

    1981-01-01

    A ''reverse'' solid-phase radio-immuno-assay for IgM antibodies to hepatitis A virus (HAV) was developed. Anti-human IgM immunoglobulins were bound on the wells of polyvinylchloride microtiter plates. Serum specimens were incubated in the anti-human IgM coated wells and bound IgM antibodies were then assayed for antigen specificity by subsequent incubations with HAV antigen and /sup 125/I-labelled human anti-HAV IgG. The test showed a high sensitivity and specificity for anti-HAV IgM antibodies. No false-positive reactions were observed either in the sera from patients with hepatobiliary disorders other than HAV infection or in the sera containing both rheumatoid factor and anti-HAV IgG antibodies. In acute HAV infections specific IgM antibodies were present already in the first specimens taken within a few days after the onset of jaundice. The persistence of the IgM antibodies was from 4 to 6 months. IgM antibody titers up to 1,000,000 were observed in the acute phase of HAV infection. In routine diagnostic work the titration of the sera was not necessary, since a reliable qualitative result was obtained by testing the sera in a single dilution of 1:100. A similar reverse immuno-assay principle may be adaptable for the diagnostic determination of IgM antibodies to different viral and microbial antigens.

  12. Observation of a New High-Pressure Solid Phase in Dynamically Compressed Aluminum

    Science.gov (United States)

    Polsin, D. N.

    2017-10-01

    Aluminum is ideal for testing theoretical first-principles calculations because of the relative simplicity of its atomic structure. Density functional theory (DFT) calculations predict that Al transforms from an ambient-pressure, face-centered-cubic (fcc) crystal to the hexagonal close-packed (hcp) and body-centered-cubic (bcc) structures as it is compressed. Laser-driven experiments performed at the University of Rochester's Laboratory for Laser Energetics and the National Ignition Facility (NIF) ramp compressed Al samples to pressures up to 540 GPa without melting. Nanosecond in-situ x-ray diffraction was used to directly measure the crystal structure at pressures where the solid-solid phase transformations of Al are predicted to occur. Laser velocimetry provided the pressure in the Al. Our results show clear evidence of the fcc-hcp and hpc-bcc transformations at 216 +/- 9 GPa and 321 +/- 12 GPa, respectively. This is the first experimental in-situ observation of the bcc phase in compressed Al and a confirmation of the fcc-hcp transition previously observed under static compression at 217 GPa. The observations indicate these solid-solid phase transitions occur on the order of tens of nanoseconds time scales. In the fcc-hcp transition we find the original texture of the sample is preserved; however, the hcp-bcc transition diminishes that texture producing a structure that is more polycrystalline. The importance of this dynamic is discussed. The NIF results are the first demonstration of x-ray diffraction measurements at two different pressures in a single laser shot. This material is based upon work supported by the Department of Energy National Nuclear Security Administration under Award Number DE-NA0001944.

  13. Solid-phase enzyme immunoassay or radioimmunoassay for the detection of immune complexes based on their recognition by conglutinin: conglutinin-binding test

    International Nuclear Information System (INIS)

    Casali, P.; Bossus, A.; Carpentier, N.A.; Lambert, P.H.

    1977-01-01

    Bovine conglutinin was used in a solid-phase assay for the detection of immune complexes. In a first step, the tested serum sample was incubated in polypropylene tubes coated with conglutinin to allow C3-coated immune complexes to bind to solid-phase conglutinin. In a second step, the conglutinin-bound complexes were detected using an enzyme-conjugated or radiolabelled anti-immunoglobulin antibody. The conglutinin-binding (KgB) test did not suffer from the interference of DNA, heparin or endotoxins. Its limit of sensitivity for aggregated IgG was 3 μg/ml undiluted human serum. Immune complexes prepared in vitro using tetanus toxoid, or DNA, and corresponding antibodies in human sera could be detected at various antigen/antibody ratios and at antibody concentrations lower than 8 μg/ml. The KgB test allowed for the detection of immune complexes in sera from patients with systemic lupus erythematosus, rheumatoid arthritis, idiopathic vasculitis, leprosy and leukemia. These sera were also tested using the 125 I-labelled Clq-binding activity (BA) test and the KgB test simultaneously, and a significant rank order correlation was observed. In patients with leukemia, a significant correlation was observed using three tests, KgB, 125 I-labelled Clq BA and Raji-cell radioimmunoassay (RIA). Therefore, the KgB test appears as a simple and reproducible method, utilizing a very stable reagent, with a sensitivity and specificity comparable to the other tests studied and allowing for clinical application. (author)

  14. The effect of high antigen density on solid-phase radioimmunoassays for antibody regardless of immunoglobulin class

    International Nuclear Information System (INIS)

    Rubin, R.L.; Hardtke, M.A.; Carr, R.I.

    1980-01-01

    Human sera containing antibody to casein or to bovine serum albumin were used to assess the validity and utility of a solid-phase assay for quantitating antibody activity. Rabbit anti-human immunoglobulin radiolabeled with 125 I and capable of reacting with all human immunoglobulin classes was used to detect antibody bound to antigen immobilized to polystyrene tubes by a new covalent technique. This method results in very high antigen concentrations in highly stable association with polystyrene tubes. Kinetic and absorption studies demonstrated that low avidity antibodies are better detected when antigen is immobilized by the covalent method than when passively adsorbed. Conditions are described for minimizing artifactual interactions and for obtaining results similar to those obtained with conventional, liquid-phase assays. Failure to reach equilibrium in solid-phase assays and other problems are proposed to explain, in part, the inability to obtain a better correlation between solid- and liquid-phase immunoassays. (Auth.)

  15. A new solid-phase sandwich radioimmunoassay and its application to the detection of snake venom

    International Nuclear Information System (INIS)

    Coulter, A.R.; Cox, J.C.; Sutherland, S.K.; Waddel, C.J.

    1978-01-01

    A solid-phase sandwich radioimmunoassay is described which can be used for the detection and quantitative estimation of crude snake venom and a snake neurotoxin in clinical and experimental situations. Rabbit IgG antivenom or antineurotoxin, covalently coupled to a solid phase (CH-Sepharose 4B) is incubated with sample of unknown venom concentration. Venom bound by the solid-phase antibody is detected by reaction with 125 I-labelled rabbit IgG antivenom or antineurotoxin ([ 125 I]IgG). The resultant count, T, is the total (specific and non-specific) uptake of [ 125 I]IgG. Non-specific binding N, is similarly determined, but with normal rabbit IgG antivenom or antineurotoxin ([ 125 I]IgG). The resultant count, T, is the total (specific and non-specific) uptake of [ 125 I]IgG. Non-specific binding N, is similarly determined, but with normal rabbit IgG bound to the solid phase. A T:N value greater than 1.8 for human serum or urine indicates the presence of venom in a sample (P>0.95). Positive samples are assayed at several dilutions and the venom present estimated from the specific count (T-N). Levels of 0.4 ng/ml of crude tiger snake venom (TSV) and 0.1 ng/ml of neurotoxin can be reliably detected by this procedure. (Auth.)

  16. Recombination barrier layers in solid-state quantum dot-sensitized solar cells

    KAUST Repository

    Roelofs, Katherine E.

    2012-06-01

    By replacing the dye in the dye-sensitized solar cell design with semiconductor quantum dots as the light-absorbing material, solid-state quantum dot-sensitized solar cells (ss-QDSSCs) were fabricated. Cadmium sulfide quantum dots (QDs) were grown in situ by successive ion layer adsorption and reaction (SILAR). Aluminum oxide recombination barrier layers were deposited by atomic layer deposition (ALD) at the TiO2/hole-conductor interface. For low numbers of ALD cycles, the Al2O3 barrier layer increased open circuit voltage, causing an increase in device efficiency. For thicker Al2O3 barrier layers, photocurrent decreased substantially, leading to a decrease in device efficiency. © 2012 IEEE.

  17. Solid-phase vibrational redox reactions in coordinated oxides

    International Nuclear Information System (INIS)

    Kostikova, G.P.; Korol'kov, D.V.; Kostikov, Yu.P.

    1996-01-01

    The properties of multicomponent oxides (YBa 2 Cu 3 O 7-x , etc.), incorporating different valency forms of each of two (or more) different elements have been compared with the properties of the known chemical systems, where vibrational (periodic) redox-reactions are realized a fortiori. The essence of the new theoretical concept suggested consists in the following: high-T c superconductivity of the complex oxides and similar compounds originates from vibrational redox reaction proceeding in solid phase and involving different valency atoms of every element

  18. Solid-phase extraction of carotenoids.

    Science.gov (United States)

    Shen, Yao; Hu, Yumin; Huang, Ke; Yin, Shi'an; Chen, Bo; Yao, Shouzhuo

    2009-07-24

    In this work, solid-phase extraction (SPE) trapping performance of lutein and beta-carotene, which were used as the model molecules of carotenoids, was investigated. The absorption, elution, and enrichment of carotenoids on SPE cartridges with four different sorbents, i.e. C(30), C(18), diol, and silica, were compared respectively with the help of frontal analysis technique. The high retentions of both lutein and beta-carotene were achieved on the C(18) and C(30) cartridges. The diol and silica cartridges only had good retention for lutein. The optimized SPE method for sample pretreatment for the carotenoids analysis was obtained after the investigation of trapping performance. The method was applied successfully to the analysis of biological sample, i.e. serum and human breast milk. The recovery, accuracy, and precision of SPE method comparing with those of traditional liquid-liquid extraction (LLE) method for the sample pretreatment for the analysis of carotenoids owned a number of advantages such as rapid, no chloroform used, and accurate versus LLE.

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

    Science.gov (United States)

    Sheldon, Rex; Weiser, Martin W.

    1993-01-01

    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.

  20. Three magnetic particles solid phase radioimmunoassay for T4: Comparison of their results with established methods

    International Nuclear Information System (INIS)

    Bashir, T.

    1996-01-01

    The introduction of solid phase separation techniques is an important improvement in radioimmunoassays and immunoradiometric assays. Magnetic particle solid phase method has additional advantages over others, as the separation is rapid and centrifugation is not required. Three types of magnetic particles have been studied in T 4 RIA and the results have been compared with commercial kits and other established methods. (author). 4 refs, 9 figs, 2 tabs

  1. Use of the 2-chlorotrityl chloride resin for microwave-assisted solid phase peptide synthesis.

    Science.gov (United States)

    Ieronymaki, Matthaia; Androutsou, Maria Eleni; Pantelia, Anna; Friligou, Irene; Crisp, Molly; High, Kirsty; Penkman, Kirsty; Gatos, Dimitrios; Tselios, Theodore

    2015-09-01

    A fast and efficient microwave (MW)-assisted solid-phase peptide synthesis protocol using the 2-chlorotrityl chloride resin and the Fmoc/tBu methodology, has been developed. The established protocol combines the advantages of MW irradiation and the acid labile 2-chlorotrityl chloride resin. The effect of temperature during the MW irradiation, the degree of resin substitution during the coupling of the first amino acids and the rate of racemization for each amino acid were evaluated. The suggested solid phase methodology is applicable for orthogonal peptide synthesis and for the synthesis of cyclic peptides. © 2015 Wiley Periodicals, Inc.

  2. Determination of trace iron in the boiler water used in power generation plants by solid-phase spectrophotometry.

    Science.gov (United States)

    Sarenqiqige; Maeda, Akihiro; Yoshimura, Kazuhisa

    2014-01-01

    A sensitive, simple and low-cost determination method for the total iron concentration in boiler water systems of power generation plants was developed by solid phase spectrometry (SPS) using 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ) as a coloring agent. The reagents and 0.08 cm(3) of a cation exchanger were added to a 50-cm(3) boiler water sample, then mixed for 30 min to adsorb/concentrate the produced Fe(TPTZ)2(2+) colored complex on the solid beads, resulting in a 625 times concentration of the target analyte without any other procedure. The detection limit of 0.1 μg dm(-3) was obtained, and the optimum conditions for the digestion procedure and color developing reaction was investigated and reported. According to the application of this method to real samples, the present SPS method is the best one because of the shorter analysis time, simpler operation and use of very low-cost equipment compared to the conventional methods, such as TPTZ solution spectrophotometric method after a 16 times concentration, ICP-MS and AAS.

  3. Structures of the particles of the condensed dispersed phase in solid fuel combustion products plasma

    International Nuclear Information System (INIS)

    Samaryan, A.A.; Chernyshev, A.V.; Nefedov, A.P.; Petrov, O.F.; Fortov, V.E.; Mikhailov, Yu.M.; Mintsev, V.B.

    2000-01-01

    The results of experimental investigations of a type of dusty plasma which has been least studied--the plasma of solid fuel combustion products--were presented. Experiments to determine the parameters of the plasma of the combustion products of synthetic solid fuels with various compositions together with simultaneous diagnostics of the degree of ordering of the structures of the particles of the dispersed condensed phase were performed. The measurements showed that the charge composition of the plasma of the solid fuels combustion products depends strongly on the easily ionized alkali-metal impurities which are always present in synthetic fuel in one or another amount. An ordered arrangement of the particles of a condensed dispersed phase in structures that form in a boundary region between the high-temperature and condensation zones was observed for samples of aluminum-coated solid fuels with a low content of alkali-metal impurities

  4. Determination of Scopolamine in Human Saliva Using Solid Phase Extraction and LC/MS/MS

    Science.gov (United States)

    Wang, Zuwei; Vaksman, Zalman; Boyd, Jason; Putcha, Lakshmi

    2007-01-01

    Purpose: Scopolamine is the preferred treatment for motion sickness during space flight because of its quick onset of action, short half-life and favorable side-effect profile. The dose administered depends on the mode of administration and usually ranges between 0.1 and 0.8 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids by using conventional HPLC methods. To measure scopolamine in saliva and thereby to evaluate the pharmacokinetics of scopolamine, we developed an LC/MS/MS method using off-line solid phase extraction. Method: Samples (0.5mL) were loaded onto Waters Oasis HLB co-polymer cartridges (10 mg, 1 mL) and eluted with 0.5 mL methanol without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 4 minutes. The mobile phase for separation was 90:10 (v/v) methanol: ammonium acetate (2 mM) in water, pH 5.0 +/- 0.1. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 yields 138.1 and internal standard (IS) hyoscyamine m/z = 290.2 yields 124.1. Results: The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at 1.7 and 3.2 min respectively. The linear range is 50-5000 pg/mL for scopolamine in saliva with correlation coefficients > 0.99 with a CV < 0.5 %. The intra-day and inter-day CVs are < 15 % for quality control samples with concentrations of 75, 300, 750 and 3000 pg/mL of scopolamine in human saliva. Conclusion: Solid phase extraction allows more rapid sample preparation and greater precision than liquid extraction. Furthermore, we increased the sensitivity and specificity by adjusting the LC mobile phase and using an MS

  5. Speciation analysis of aqueous nanoparticulate diclofenac complexes by solid-phase microextraction

    NARCIS (Netherlands)

    Zielinska, K.; Leeuwen, van H.P.; Thibault, S.; Town, R.M.

    2012-01-01

    The dynamic sorption of an organic compound by nanoparticles (NPs) is analyzed by solid-phase microextraction (SPME) for the example case of the pharmaceutical diclofenac in dispersions of impermeable (silica, SiO(2)) and permeable (bovine serum albumin, BSA) NPs. It is shown that only the

  6. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry.

    Science.gov (United States)

    Amin, Alaa S; El-Sharjawy, Abdel-Azeem M; Kassem, Mohammed A

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L(-1) of Tl(III) with relative standard deviation (RSD) of 1.40% (n=10). The detection and quantification limits are 150 and 495 ng L(-1) using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31×10(7) L mol(-1)cm(-1) and 0.00156 ng cm(-2), respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry

    Science.gov (United States)

    Amin, Alaa S.; El-Sharjawy, Abdel-Azeem M.; Kassem, Mohammed A.

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L-1 of Tl(III) with relative standard deviation (RSD) of 1.40% (n = 10). The detection and quantification limits are 150 and 495 ng L-1 using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31 × 107 L mol-1 cm-1 and 0.00156 ng cm-2, respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples.

  8. Single Photon Sensitive HgCdTe Avalanche Photodiode Detector (APD), Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Leveraging Phase I SBIR successes, in Phase II, a single photon sensitive LIDAR receiver will be fabricated and delivered to NASA. In Phase I, high-gain,...

  9. New practical algorithm for modelling analyte recovery in bioanalytical reversed phase and mixed-mode solid phase extraction

    NARCIS (Netherlands)

    Hendriks, G.; Uges, D. R. A.; Franke, J. P.

    2008-01-01

    Solid phase extraction (SPE) is a widely used method for sample cleanup and sample concentration in bioanalytical sample preparation. A few methods to model the retention behaviour on SPE cartridges have been described previously but they are either not applicable to ionised species or are not

  10. On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue.

    Science.gov (United States)

    Ensafi, Ali A; Ghaderi, Ali R

    2007-09-05

    An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5M HNO(3) and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 microg of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5M HNO(3) solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ngmL(-1) Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ngmL(-1) Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments.

  11. A new polyethylene glycol fiber prepared by coating porous zinc electrodeposited onto silver for solid-phase microextraction of styrene

    International Nuclear Information System (INIS)

    Sungkaew, Sakchaibordee; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

    2010-01-01

    A new polyethylene glycol fiber was developed for solid-phase microextraction (SPME) of styrene by electrodepositing porous Zn film on Ag wire substrate followed by coating with polyethylene glycol sol-gel (Ag/Zn/PEG sol-gel fiber). The scanning electron micrographs of fibers surface revealed a highly porous structure. The extraction property of the developed fiber-to-styrene residue from polystyrene packaged food was investigated by headspace solid-phase microextraction (HS-SPME) and analyzed with a gas chromatograph coupled with flame ionization detection (GC-FID). The new Ag/Zn/PEG sol-gel fiber is simple to prepare, low cost, robust, has high thermal stability and long lifetime, up to 359 extractions. Repeatability of one fiber (n = 6) was in the range of 4.7-7.5% and fiber-to-fiber reproducibility (n = 4) for five concentration values were in the range 3.4-10%. This Ag/Zn/PEG sol-gel fiber was compared to two commercial SPME fibers, 75 μm carboxen/polydimethylsiloxane (CAR/PDMS) and 100 μm polydimethylsiloxane (PDMS). Under their optimum conditions, Ag/Zn/PEG sol-gel fiber showed the highest sensitivity and the lowest detection limit at 0.28 ± 0.01 ng mL -1 .

  12. A Variational Model for Two-Phase Immiscible Electroosmotic Flow at Solid Surfaces

    KAUST Repository

    Shao, Sihong; Qian, Tiezheng

    2012-01-01

    We develop a continuum hydrodynamic model for two-phase immiscible flows that involve electroosmotic effect in an electrolyte and moving contact line at solid surfaces. The model is derived through a variational approach based on the Onsager

  13. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L{sup −1} and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L{sup −1} of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic.

  14. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-01-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L −1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L −1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract. - Highlights: • Efficient retention and preconcentration of As by combining an IL with MWCNTs • Determination of As by ETAAS with direct injection of MWCNTs • Thermal degradation of MWCNTs in the graphite furnace of ETAAS • Highly sensitive speciation and determination of As in garlic

  15. Phase-Sensitive Coherence and the Classical-Quantum Boundary in Ghost Imaging

    Science.gov (United States)

    Erkmen, Baris I.; Hardy, Nicholas D.; Venkatraman, Dheera; Wong, Franco N. C.; Shapiro, Jeffrey H.

    2011-01-01

    The theory of partial coherence has a long and storied history in classical statistical optics. the vast majority of this work addresses fields that are statistically stationary in time, hence their complex envelopes only have phase-insensitive correlations. The quantum optics of squeezed-state generation, however, depends on nonlinear interactions producing baseband field operators with phase-insensitive and phase-sensitive correlations. Utilizing quantum light to enhance imaging has been a topic of considerable current interest, much of it involving biphotons, i.e., streams of entangled-photon pairs. Biphotons have been employed for quantum versions of optical coherence tomography, ghost imaging, holography, and lithography. However, their seemingly quantum features have been mimicked with classical-sate light, questioning wherein lies the classical-quantum boundary. We have shown, for the case of Gaussian-state light, that this boundary is intimately connected to the theory of phase-sensitive partial coherence. Here we present that theory, contrasting it with the familiar case of phase-insensitive partial coherence, and use it to elucidate the classical-quantum boundary of ghost imaging. We show, both theoretically and experimentally, that classical phase-sensitive light produces ghost imaging most closely mimicking those obtained in biphotons, and we derived the spatial resolution, image contrast, and signal-to-noise ratio of a standoff-sensing ghost imager, taking into account target-induced speckle.

  16. Laminating solution-processed silver nanowire mesh electrodes onto solid-state dye-sensitized solar cells

    KAUST Repository

    Hardin, Brian E.; Gaynor, Whitney; Ding, I-Kang; Rim, Seung-Bum; Peumans, Peter; McGehee, Michael D.

    2011-01-01

    Solution processed silver nanowire meshes (Ag NWs) were laminated on top of solid-state dye-sensitized solar cells (ss-DSCs) as a reflective counter electrode. Ag NWs were deposited in <1 min and were less reflective compared to evaporated Ag

  17. Isostructural solid-solid transition of (colloidal) simple fluids

    International Nuclear Information System (INIS)

    Tejero, C.F.; Daanoun, A.; Lakkerkerker, H.N.W.; Baus, M.

    1995-01-01

    A variational approach based on the Gibbs-Bogoliubov inequality is used in order to evaluate the free energy of simple fluids described by a double-Yukawa pair potential. A hard-sphere reference fluid is used to describe the fluid phases, and an Einstein reference crystal to describe the solid phases. Apart from the usual type of phase diagram, typical of atomic simple fluids with long-ranged attractions, we find two types of phase diagrams, specific to colloidal systems with intermediate and short-ranged attractions. One of the latter phase diagrams exhibits an isostructural solid-solid transition, which has not yet been observed experimentally

  18. Synthesis of nanostructured solid-state phases of V{sub 7}O{sub 16} and V{sub 2}O{sub 5} compounds for ppb-level detection of ammonia

    Energy Technology Data Exchange (ETDEWEB)

    Huotari, J., E-mail: joni.huotari@ee.oulu.fi [Faculty of Information Technology and Electrical Engineering, P.O. Box 4500, FIN-90014, University of Oulu (Finland); Lappalainen, J. [Faculty of Information Technology and Electrical Engineering, P.O. Box 4500, FIN-90014, University of Oulu (Finland); Eriksson, J.; Bjorklund, R. [Department of Physics, Chemistry and Biology, Linköping University, SE-581 83, Linköping (Sweden); Heinonen, E. [Center of Microscopy and Nanotechnology, Erkki Koiso-Kanttilankatu 3, Tietotalo 1, Linnanmaa, FIN-90570, Oulu (Finland); Miinalainen, I. [Biocenter Oulu, P.O. Box 5000, FI-90014, University of Oulu (Finland); Puustinen, J. [Faculty of Information Technology and Electrical Engineering, P.O. Box 4500, FIN-90014, University of Oulu (Finland); Lloyd Spetz, A. [Faculty of Information Technology and Electrical Engineering, P.O. Box 4500, FIN-90014, University of Oulu (Finland); Department of Physics, Chemistry and Biology, Linköping University, SE-581 83, Linköping (Sweden)

    2016-08-05

    Solid state phase of V{sub 7}O{sub 16} with separate V{sub 2}O{sub 5} phase were fabricated by pulsed laser deposition. The crystal structure and symmetry of the deposited films were studied with X-ray diffraction and Raman spectroscopy, respectively. Rietveld analysis was performed to the X-ray diffraction measurement results. The surface potentials and morphologies of the films were studied with atomic force microscopy, and microstructure of the thin films was analysed by transmission electron microscopy. Raman spectroscopy and Rietveld refinement results confirmed that the thin-film crystal structures varied between orthorombic V{sub 2}O{sub 5} phase and another phase, triclinic V{sub 7}O{sub 16}, previously found only in the walls of vanadium oxide nanotubes (VO{sub x}-NT), bound together with organic amine. We have earlier presented the first results of stable and pure metal-oxide solid-state phase of V{sub 7}O{sub 16} manufactured from ceramic V{sub 2}O{sub 5} target. Here we show more detailed study of these structures. The microstructure studies showed a variation on the porosity of the films according to crystal structures and also some fibre-like nanostructures were found in the films. The surface morphology depended strongly on the crystal structure and the surface potential studies showed ∼50 meV difference in the work function values between the phases. Compounds were found to be extremely sensitive towards ammonia, NH{sub 3}, down to ∼40 ppb concentrations, and have shown to have the stability and selectivity to control the Selective Catalytic Reduction process, where nitrogen oxides are reduced by ammonia in, e.g. diesel exhausts. - Highlights: • The triclinic V{sub 7}O{sub 16} phase is proven to exist in solid state thin-film form. • The existence of V{sub 7}O{sub 16} in thin-film form is proven by several methods. • The structure of mixed V{sub 7}O{sub 16} and V{sub 2}O{sub 5} is proven to be sensitive to NH{sub 3} at ppb-level.

  19. Entangled-Pair Transmission Improvement Using Distributed Phase-Sensitive Amplification

    Directory of Open Access Journals (Sweden)

    Anjali Agarwal

    2014-12-01

    Full Text Available We demonstrate the transmission of time-bin entangled photon pairs through a distributed optical phase-sensitive amplifier (OPSA. We utilize four-wave mixing at telecom wavelengths in a 5-km dispersion-shifted fiber OPSA operating in the low-gain limit. Measurements of two-photon interference curves show no statistically significant degradation in the fringe visibility at the output of the OPSA. In addition, coincidence counting rates are higher than direct passive transmission because of constructive interference between amplitudes of input photon pairs and those generated in the OPSA. Our results suggest that application of distributed phase-sensitive amplification to transmission of entangled photon pairs could be highly beneficial towards advancing the rate and scalability of future quantum communications systems.

  20. Applications of a solid phase radioimmunoassay (SPRIA) to the micro-determination of ABO blood group

    International Nuclear Information System (INIS)

    Wu Fenqiang; Guo Jingyuan

    1995-01-01

    The authors report a simple, rapid, sensitive and accurate solid phase radioimmunoassay (SPRIA) method which has been improved. The research included the tests of its methodological parameters, sensitivity, accuracy, and the studies on its applications to the detection of blood group substances in varied forensic biological materials. The coefficient variation of intra-assay was 5.6%, and that of inter-assay was 10.15%. As to its applications to the forensic serology, the ABO blood groups of human bloodstain, hair follicular tissues and salivary stains had been tested and the results were satisfying. Later, 50 unknown type bloodly samples had been blind tested. The judging level used to identify the positive and negative wells was 800 cpm, that meant, if the radioactive count of a well were over 800 cpm, it was determined as a positive well, if that of a well were below 800 cpm, it was negative well. As SPRIA is a method of micro-determination which can micro-test the blood group antigens contained in varied forensic biological materials, it should has a good future of its applications to the forensic medicine fields

  1. Quantification of VX Nerve Agent in Various Food Matrices by Solid-Phase Extraction Ultra-Performance Liquid ChromatographyTime-of-Flight Mass Spectrometry

    Science.gov (United States)

    2016-04-01

    QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE...TITLE AND SUBTITLE Quantification of VX Nerve Agent in Various Food Matrices by Solid - Phase Extraction Ultra-Performance Liquid Chromatography...QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID - PHASE EXTRACTION ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY–TIME-OF-FLIGHT MASS

  2. Solid-phase extraction assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet to determine sildenafil and its analogues in dietary supplements.

    Science.gov (United States)

    Li, Jing; Roh, Si Hun; Shaodong, Jia; Hong, Ji Yeon; Lee, Dong-Kyu; Shin, Byong-Kyu; Park, Jeong Hill; Lee, Jeongmi; Kwon, Sung Won

    2017-08-01

    A novel analytical method for the simultaneous determination of the concentration of sildenafil and its five analogues in dietary supplements using solid-phase extraction assisted reversed-phase dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ion-pairing liquid chromatography with an ultraviolet detector was developed. Parameters that affect extraction efficiency were systematically investigated, including the type of solid-phase extraction cartridge, pH of the extraction environment, and the type and volume of extraction and dispersive solvent. The method linearity was in the range of 5.0-100 ng/mL for sildenafil, homosildenafil, udenafil, benzylsildenafil, and thiosildenafil and 10-100 ng/mL for acetildenafil. The coefficients of determination were ≥0.996 for all regression curves. The sensitivity values expressed as limit of detection were between 2.5 and 7.5 ng/mL. Furthermore, intraday and interday precisions expressed as relative standard deviations were less than 5.7 and 9.9%, respectively. The proposed method was successfully applied to the analysis of sildenafil and its five analogues in complex dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Fibrous flexible solid-type dye-sensitized solar cells without transparent conducting oxide

    International Nuclear Information System (INIS)

    Fan Xing; Chu Zengze; Chen Lin; Zhang Chao; Wang Fuzhi; Tang Yanwei; Sun Jianliang; Zou Dechun

    2008-01-01

    We have explored a type of all-solid fibrous flexible dye-sensitized solar cells without transparent conducting oxide based on a CuI electrolyte. The working electrode's substrate is a metal wire. Cu wire counterelectrode is twisted with the dye-sensitized and CuI-coated working electrode. The cell's apparent diameter is about 150 μm. The cell's current-voltage output depends little on the incident angle of light. A 4-cm-long fibrous cell's open-circuit voltage and short-circuit current generate 304 mV and 0.032 mA, respectively. The interfacial interaction between the two electrodes has a significant influence on the inner charge transfer of the cell

  4. Differing results of direct and indirect solid phase radioimmunoassay for HBsAg in acute hepatitis

    International Nuclear Information System (INIS)

    Strohm, W.D.; Legler, K.; Gerlich, W.; Stamm, B.; Zimmer, S.; Biotest-Serum-Institut G.m.b.H., Frankfurt am Main; Goettingen Univ.

    1978-01-01

    In 54 patients suffering from active viral hepatitis the indirect solid phase radioimmunoassay (ind-SPRIA) for HBsAg was positive in 9 cases the direct solid phase radioimmunoassay (d-SPRIA) being negative. In 2 further cases ind-SPRIA was positive during several weeks but d-SPRIA only once. AntiHBc could be detected in 9 of these patients. In 7 patients the usual decrease of the transaminase activity was followed by a second elavation with prolongation of the disease. The unknown factor detected by ind-SPRIA suggests a special of acute hepatitis. (orig.) [de

  5. Differing results of direct and indirect solid phase radioimmunoassay for HBsAg in acute hepatitis

    Energy Technology Data Exchange (ETDEWEB)

    Strohm, W D; Legler, K; Gerlich, W; Stamm, B; Zimmer, S [Frankfurt Univ. (Germany, F.R.). Abt. fuer Gastroenterologie; Biotest-Serum-Institut G.m.b.H., Frankfurt am Main (Germany, F.R.); Goettingen Univ. (Germany, F.R.). Hygiene-Institut)

    1978-09-01

    In 54 patients suffering from active viral hepatitis the indirect solid phase radioimmunoassay (ind-SPRIA) for HBsAg was positive in 9 cases the direct solid phase radioimmunoassay (d-SPRIA) being negative. In 2 further cases ind-SPRIA was positive during several weeks but d-SPRIA only once. AntiHBc could be detected in 9 of these patients. In 7 patients the usual decrease of the transaminase activity was followed by a second elavation with prolongation of the disease. The unknown factor detected by ind-SPRIA suggests a special of acute hepatitis.

  6. Uncovering the Connection Between Low-Frequency Dynamics and Phase Transformation Phenomena in Molecular Solids

    Science.gov (United States)

    Ruggiero, Michael T.; Zhang, Wei; Bond, Andrew D.; Mittleman, Daniel M.; Zeitler, J. Axel

    2018-05-01

    The low-frequency motions of molecules in the condensed phase have been shown to be vital to a large number of physical properties and processes. However, in the case of disordered systems, it is often difficult to elucidate the atomic-level details surrounding these phenomena. In this work, we have performed an extensive experimental and computational study on the molecular solid camphor, which exhibits a rich and complex structure-dynamics relationship, and undergoes an order-disorder transition near ambient conditions. The combination of x-ray diffraction, variable temperature and pressure terahertz time-domain spectroscopy, ab initio molecular dynamics, and periodic density functional theory calculations enables a complete picture of the phase transition to be obtained, inclusive of mechanistic, structural, and thermodynamic phenomena. Additionally, the low-frequency vibrations of a disordered solid are characterized for the first time with atomic-level precision, uncovering a clear link between such motions and the phase transformation. Overall, this combination of methods allows for significant details to be obtained for disordered solids and the associated transformations, providing a framework that can be directly applied for a wide range of similar systems.

  7. Simultaneous Analysis of Simple Coumarins and Furocoumarines in Cigarettes by Solid-Phase Extraction with Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Zheng, Yang; Xu, Xiuli; Yuan, Fei; Yao, Meiyi; Ji, Shunli; Huang, Zhiqiang; Zhang, Feng

    2017-09-01

    A sensitive, high-throughput analytical method based on a GC-MS method was established for the simultaneous quantitative determination of two categories of harmful coumarins: simple coumarins (coumarin, 6-methylcoumarin, 7-methoxycoumarin, 3,4-dihydrocoumarin, and 7-ethoxy-4-methylcoumarin) and furocoumarines (psoralen, 8-methoxypsoralen, 5-methoxypsoralen, and trioxysalen). The nine analytes were extracted with ethyl acetate, purified with Oasis HLB solid-phase extraction (SPE) cartridges, and identified and quantitatively determined by GC-MS in selected-ion monitoring mode. The LODs and LOQs of these compounds were in the ranges of 12.5-21.2 and 41.6-70.0 μg/kg, respectively. Average recoveries for the nine analytes ranged from 72.7 to 86.6% at LOQ, 1.5× LOQ, and 2× LOQ spike levels, with RSDs that were typically lower than 5.1%. The SPE-GC-MS method developed in this study was initially applied to research coumarins in cigarette samples; it proved to be accurate, sensitive, convenient, and practical.

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

    Science.gov (United States)

    Tóth, Blanka; Horvai, George

    2012-01-01

    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.

  9. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  10. Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  11. Method development for determination of herbicides and insecticides in surface waters using solid-phase extraction and high performance liquid chromatography

    International Nuclear Information System (INIS)

    Lebre, Daniel Temponi

    2000-01-01

    Determination of low concentrations of pesticides in surface and ground waters requires high sensitivity analytical techniques. Solid-Phase Extraction (SPE) has been successfully employed to pre concentrate and extract pesticides compounds from water samples. High Performance Liquid Chromatography (HPLC) coupled with UV/Vis detector was used to separate and quantify the extracted compounds. In this work, samples of surface waters with known concentrations of herbicides (atrazine, simazine and trifluralin) and insecticides (aldicarb, carbofuran and carbaryl) were extracted by using SPE off-line technique. The compounds were separated and quantified by reverse phase HPLC with UV detection at 220 ηm. The extraction efficiency was compared between two columns filled with different materials: C 18 -bonded silica phase (500 mg) and copolymer styrenedivynilbenzene resin (250 mg). The results were evaluated as the percent recovery of compounds obtained using different solvents at different concentrations. The results showed that recovery of the analytes greater than 80 % were obtained in SPE columns filled with C 18 bonded silica phase with 6 mL of acetonitrile. Once the optimum conditions were chosen for simulate water samples, the method was validated through analytical and statistical procedures and applied for surface waters. The suitability of the method was verified for the studied compounds showing good sensitivity, i. e., concentrations within the range of 0.4 to 4.0 μgL -1 of pesticides could be quantified attending the limits proposed by official regulations. (author)

  12. An ordered metallic glass solid solution phase that grows from the melt like a crystal

    International Nuclear Information System (INIS)

    Chapman, Karena W.; Chupas, Peter J.; Long, Gabrielle G.; Bendersky, Leonid A.; Levine, Lyle E.; Mompiou, Frédéric; Stalick, Judith K.; Cahn, John W.

    2014-01-01

    We report structural studies of an Al–Fe–Si glassy solid that is a solid solution phase in the classical thermodynamic sense. We demonstrate that it is neither a frozen melt nor nanocrystalline. The glass has a well-defined solubility limit and rejects Al during formation from the melt. The pair distribution function of the glass reveals chemical ordering out to at least 12 Å that resembles the ordering within a stable crystalline intermetallic phase of neighboring composition. Under isothermal annealing at 305 °C the glass first rejects Al, then persists for approximately 1 h with no detectable change in structure, and finally is transformed by a first-order phase transition to a crystalline phase with a structure that is different from that within the glass. It is possible that this remarkable glass phase has a fully ordered atomic structure that nevertheless possesses no long-range translational symmetry and is isotropic

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

    Science.gov (United States)

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

    2016-07-01

    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.

  14. Development of andrographolide molecularly imprinted polymer for solid-phase extraction

    Science.gov (United States)

    Yin, Xiaoying; Liu, Qingshan; Jiang, Yifan; Luo, Yongming

    2011-06-01

    A method employing molecularly imprinted polymer (MIP) as selective sorbent for solid-phase extraction (SPE) to pretreat samples was developed. The polymers were prepared by precipitation polymerization with andrographolide as template molecule. The structure of MIP was characterized and its static adsorption capacity was measured by the Scatchard equation. In comparison with C 18-SPE and non-imprinted polymer (NIP) SPE column, MIP-SPE column displays high selectivity and good affinity for andrographolide and dehydroandrographolide for extract of herb Andrographis paniculata ( Burm.f.) Nees (APN). MIP-SPE column capacity was 11.9 ± 0.6 μmol/g and 12.1 ± 0.5 μmol/g for andrographolide and dehydroandrographolide, respectively and was 2-3 times higher than that of other two columns. The precision and accuracy of the method developed were satisfactory with recoveries between 96.4% and 103.8% (RSD 3.1-4.3%, n = 5) and 96.0% and 104.2% (RSD 2.9-3.7%, n = 5) for andrographolide and dehydroandrographolide, respectively. Various real samples were employed to confirm the feasibility of method. This developed method demonstrates the potential of molecularly imprinted solid phase extraction for rapid, selective, and effective sample pretreatment.

  15. A sensitive method for determining total vanadium in water samples using colorimetric-solid-phase extraction-fiber optic reflectance spectroscopy

    International Nuclear Information System (INIS)

    Filik, Hayati; Yanaz, Zeynep

    2009-01-01

    A selective colorimetric-solid-phase extraction (C-SPE) method for the determination of total vanadium in water samples was developed. This method introduced a new variation of C-SPE. The colour reaction is based on the reaction of vanadium(V) ternary complex formed with 1-(2-Pyridylazo)-2-naphtol (PAN) in the presence hydrogen peroxide (H 2 O 2 ). In this technique, the target analytes in samples are extracted onto solid matrix loaded with a colorimetric reagent and then quantified directly on the adsorbent surface by using a miniature fiber optic reflectance spectrometer. The measurements were carried out at a wavelength of 589.4 nm since it yielded the largest divergence different in reflectance spectra before and after reaction with the vanadium. The overall time required for the C-SPE procedure was ∼20 min. The amount of concentrated V is then determined in a few seconds by using miniature reflectance spectrometer. At the optimal conditions, a calibration curve was constructed, revealing a linear range of 0.05-0.52 mg L -1 and a detection limit as low as 0.01 mg L -1 while the RSD lower than 2.8%. In order to verify the accuracy of the method, a certified reference water samples (TMDA) were analysed and the results obtained were in good agreement with the certified values. The proposed method was applied to the determination of vanadium in tap water, seawater samples with a recovery for the spiked samples in the range of 98-102%.

  16. Method optimization for non-equilibrium solid phase microextraction sampling of HAPs for GC/MS analysis

    Science.gov (United States)

    Zawadowicz, M. A.; Del Negro, L. A.

    2010-12-01

    Hazardous air pollutants (HAPs) are usually present in the atmosphere at pptv-level, requiring measurements with high sensitivity and minimal contamination. Commonly used evacuated canister methods require an overhead in space, money and time that often is prohibitive to primarily-undergraduate institutions. This study optimized an analytical method based on solid-phase microextraction (SPME) of ambient gaseous matrix, which is a cost-effective technique of selective VOC extraction, accessible to an unskilled undergraduate. Several approaches to SPME extraction and sample analysis were characterized and several extraction parameters optimized. Extraction time, temperature and laminar air flow velocity around the fiber were optimized to give highest signal and efficiency. Direct, dynamic extraction of benzene from a moving air stream produced better precision (±10%) than sampling of stagnant air collected in a polymeric bag (±24%). Using a low-polarity chromatographic column in place of a standard (5%-Phenyl)-methylpolysiloxane phase decreased the benzene detection limit from 2 ppbv to 100 pptv. The developed method is simple and fast, requiring 15-20 minutes per extraction and analysis. It will be field-validated and used as a field laboratory component of various undergraduate Chemistry and Environmental Studies courses.

  17. Combination of (M)DSC and surface analysis to study the phase behaviour and drug distribution of ternary solid dispersions.

    Science.gov (United States)

    Meeus, Joke; Scurr, David J; Chen, Xinyong; Amssoms, Katie; Davies, Martyn C; Roberts, Clive J; Van den Mooter, Guy

    2015-04-01

    Miscibility of the different compounds that make up a solid dispersion based formulation play a crucial role in the drug release profile and physical stability of the solid dispersion as it defines the phase behaviour of the dispersion. The standard technique to obtain information on phase behaviour of a sample is (modulated) differential scanning calorimetry ((M)DSC). However, for ternary mixtures (M)DSC alone is not sufficient to characterize their phase behaviour and to gain insight into the distribution of the active pharmaceutical ingredient (API) in a two-phased polymeric matrix. MDSC was combined with complementary surface analysis techniques, specifically time-of-flight secondary ion mass spectrometry (ToF-SIMS) and atomic force microscopy (AFM). Three spray-dried model formulations with varying API/PLGA/PVP ratios were analyzed. MDSC, TOF-SIMS and AFM provided insights into differences in drug distribution via the observed surface coverage for 3 differently composed ternary solid dispersions. Combining MDSC and surface analysis rendered additional insights in the composition of mixed phases in complex systems, like ternary solid dispersions.

  18. Safety profile of avelumab in patients with advanced solid tumors: A pooled analysis of data from the phase 1 JAVELIN solid tumor and phase 2 JAVELIN Merkel 200 clinical trials

    OpenAIRE

    Kelly, K; Infante, JR; Taylor, MH; Patel, MR; Wong, DJ; Iannotti, N; Mehnert, JM; Loos, AH; Koch, H; Speit, I; Gulley, JL

    2018-01-01

    © 2018 The Authors. Cancer published by Wiley Periodicals, Inc. on behalf of American Cancer Society. BACKGROUND: Antibodies targeting the programmed death-ligand 1 (PD-L1)/programmed cell death protein 1 (PD-1) checkpoint may cause adverse events (AEs) that are linked to the mechanism of action of this therapeutic class and unique from those observed with conventional chemotherapy. METHODS: Patients with advanced solid tumors who were enrolled in the phase 1 JAVELIN Solid Tumor (1650 patient...

  19. Improving the sensitivity of J coupling measurements in solids with application to disordered materials

    International Nuclear Information System (INIS)

    Guerry, Paul; Brown, Steven P.; Smith, Mark E.

    2016-01-01

    It has been shown previously that for magic angle spinning (MAS) solid state NMR the refocused INADEQUATE spin-echo (REINE) experiment can usefully quantify scalar (J) couplings in disordered solids. This paper focuses on the two z filter components in the original REINE pulse sequence, and investigates by means of a product operator analysis and fits to density matrix simulations the effects that their removal has on the sensitivity of the experiment and on the accuracy of the extracted J couplings. The first z filter proves unnecessary in all the cases investigated here and removing it increases the sensitivity of the experiment by a factor ∼1.1–2.0. Furthermore, for systems with broad isotropic chemical shift distributions (namely whose full widths at half maximum are greater than 30 times the mean J coupling strength), the second z filter can also be removed, thus allowing whole-echo acquisition and providing an additional √2 gain in sensitivity. Considering both random and systematic errors in the values obtained, J couplings determined by fitting the intensity modulations of REINE experiments carry an uncertainty of 0.2–1.0 Hz (∼1−10 %).

  20. Phase-enhanced defect sensitivity for EUV mask inspection

    Science.gov (United States)

    Wang, Yow-Gwo; Miyakawa, Ryan; Chao, Weilun; Goldberg, Kenneth; Neureuther, Andy; Naulleau, Patrick

    2014-10-01

    In this paper, we present a complete study on mask blank and patterned mask inspection utilizing the Zernike phase contrast method. The Zernike phase contrast method provides in-focus inspection ability to study phase defects with enhanced defect sensitivity. However, the 90 degree phase shift in the pupil will significantly reduce the amplitude defect signal at focus. In order to detect both types of defects with a single scan, an optimized phase shift instead of 90 degree on the pupil plane is proposed to achieve an acceptable trade-off on their signal strengths. We can get a 70% of its maximum signal strength at focus for both amplitude and phase defects with a 47 degree phase shift. For SNR, the tradeoff between speckle noise and signal strength has to be considered. The SNR of phase and amplitude defects at focus can both reach 11 with 13 degree phase shift and 50% apodization. Moreover, the simulation results on patterned mask inspection of partially hidden phase defects with die-to-database inspection approach on the blank inspection tool show that the improvement of the Zernike phase method is more limited. A 40% enhancement of peak signal strength can be achieved with the Zernike phase contrast method when the defect is centered in the space, while the enhancement drops to less than 10% when it is beneath the line.

  1. Deposition of hole-transport materials in solid-state dye-sensitized solar cells by doctor-blading

    KAUST Repository

    Ding, I-Kang

    2010-07-01

    We report using doctor-blading to replace conventional spin coating for the deposition of the hole-transport material spiro-OMeTAD (2,20,7,70-tetrakis-(N, N-di-p-methoxyphenylamine)- 9,90-spirobifluorene) in solid-state dye-sensitized solar cells. Doctor-blading is a roll-to-roll compatible, large-area coating technique, is capable of achieving the same spiro-OMeTAD pore filling fraction as spin coating, and uses much less material. The average power conversion efficiency of solid-state dye-sensitized solar cells made from doctorblading is 3.0% for 2-lm thick films and 2.0% for 5-lm thick films, on par with devices made with spin coating. Directions to further improve the filling fraction are also suggested. © 2010 Elsevier B.V. All rights reserved.

  2. Sensitive singular-phase optical detection without phase measurements with Tamm plasmons

    Science.gov (United States)

    Boriskina, Svetlana V.; Tsurimaki, Yoichiro

    2018-06-01

    Spectrally-tailored interactions of light with material interfaces offer many exciting applications in sensing, photo-detection, and optical energy conversion. In particular, complete suppression of light reflectance at select frequencies accompanied by sharp phase variations in the reflected signal forms the basis for the development of ultra-sensitive singular-phase optical detection schemes such as Brewster and surface plasmon interferometry. However, both the Brewster effect and surface-plasmon-mediated absorption on planar interfaces are limited to one polarization of the incident light and oblique excitation angles, and may have limited bandwidth dictated by the material dielectric index and plasma frequency. To alleviate these limitations, we design narrow-band super-absorbers composed of plasmonic materials embedded into dielectric photonic nanostructures with topologically-protected interfacial Tamm plasmon states. These structures have planar geometry and do not require nanopatterning to achieve perfect absorption of both polarizations of the incident light in a wide range of incident angles, including the normal incidence. Their absorption lines are tunable across a very broad spectral range via engineering of the photon bandstructure of the dielectric photonic nanostructures to achieve reversal of the geometrical phase across the interface with the plasmonic absorber. We outline the design strategy to achieve perfect absorptance in Tamm structures with dissipative losses via conjugate impedance matching. We further demonstrate via modeling how these structures can be engineered to support sharp asymmetric amplitude resonances, which can be used to improve the sensitivity of optical sensors in the amplitude-only detection scheme that does not require use of bulky and expensive ellipsometry equipment.

  3. Solvent-free sample preparation by headspace solid-phase microextraction applied to the tracing of n-butyl nitrite abuse.

    Science.gov (United States)

    Tytgat, J; Daenens, P

    1996-01-01

    The most common alkyl nitrites encountered in forensic toxicology are iso-butyl, n-butyl and iso-pentyl(amyl) nitrites. All have become popular as an aphrodisiac, especially among the homosexual population. Alkyl nitrites are a volatile and unstable group of compounds, which hydrolyse in aqueous matrices to the alcohol and nitrite ion. Here we describe a fast, clean and sensitive procedure for the detection of hydrolysed n-butyl nitrite in whole human blood using a new, solvent-free sampling technique, the headspace solid-phase micro-extraction (HSPME), combined with GC/FID analysis. Sample preparation was investigated using two different stationary phases (100 microns polydimethylsiloxane and 85 microns polyacrylate), coating a fused silica fibre. The effect of different sampling times at fixed temperatures was also studied. Our results demonstrate that the HSPME/GC/FID procedure allows tracing of n-butyl nitrite abuse and detects hydrolysed n-butyl nitrite, i.e., released n-butanol, in whole blood at the 1 ng/mL level.

  4. [Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Huang, Juan; Chen, Guosong; Zhang, Xiaoyan; Shen, Chongyu; Lü, Chen; Wu, Bin; Liu, Yan; Chen, Huilan; Ding, Tao

    2012-11-01

    A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm x4. 6 mm, 2.6 microm) with a gradient elution using 0.3% per hundred ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N= 3) and the limit of quantification (LOQ, S/N = 10) were 20 microg/kg and 50 microg/kg, respectively. A good linearity (r > 0.99) was achieved for the target compound over the range of 20-1000 pg/L. The recoveries at the three spiked levels (50, 100, 500 microg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, cassava and wheat, were varied from 75.6% to 111.0% with the relative standard deviations no more than 13. 0%. The method is accurate, efficient, sensitive and practical. The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

  5. Study on the solid phase extraction and spectrophotometric determination of cobalt with 5-(2-benzothiazolylazo-8-hydroxyquinolene

    Directory of Open Access Journals (Sweden)

    Alaa S. Amin

    2014-11-01

    Full Text Available A highly sensitive, selective and rapid method for the determination of cobalt based on the rapid reaction of cobalt(II with 5-(2-benzothiazolylazo-8-hydroxyquinolene BTAHQ and the solid phase extraction of the Co(II-BTAHQ complex with C18 membrane disks were developed. In the presence of pH = 6.4 buffer solution and cetylpyridenium chloride (CPC medium, BTAHQ reacts with cobalt to form a deep violet complex with a molar ratio of 1:1 (cobalt to BTAHQ. This complex was enriched by the solid phase extraction with C18 membrane disks. An enrichment factor of 100 was obtained by elution of the complex from the disks with a minimal amount of isopentyl alcohol. In isopentyl alcohol medium, the molar absorptivity of the complex is 2.42 × 105 L mol−1 cm−1 at 658 nm. Beer’s law is obeyed in the range of 0.01–0.38 μg mL−1 in the measured solution. The relative standard deviation for 11 replicate samples of 0.20 μg mL−1 level is 1.37%. The detection and quantification limits reach 3.1 and 9.7 ng mL−1 in the original samples. This method was applied for the determination of cobalt in biological, water, soil and pharmaceutical preparation samples with good results.

  6. Developments of sensitive immunoassays for detection of antibodies against hepatitis B surface antigen

    Energy Technology Data Exchange (ETDEWEB)

    Ionescu-Matiu, I; Sanchez, Y; Dreesman, G R [Baylor Univ., Houston, TX (USA). Coll. of Medicine; Fields, H A [Centers for Disease Control, Public Health Service, Department of Health and Human Services, Phoenix, AZ (USA)

    1983-01-01

    Three micro solid phase immunoassays (a micro-SPRIA and two ELISA techniques) were developed and tested for the detection of anti-HBs antibodies. Two different crosslinkers (glutaraldehyde and N-succinimidyl 3-(2-pyridyldithio) propionate) were used to couple a goat anti-mouse IgG reagent to alkaline phosphatase for use as enzyme-labeled probes in the two ELISA tests. With the latter cross-linker, a defined conjugate with a 1 : 1 antibody-enzyme molar ratio was obtained. The sensitivities of micro-SPRIA and the two types of ELISA were compared to that of the commercial solid phase radioimmunoassay AUSAB test. All three microtests were significantly more sensitive than the AUSAB test. The ELISA using the glutaraldehyde cross-linked conjugate was 3-5 times less sensitive than micro-SPRIA, while the ELISA using the disulfide-linked conjugate was 2.6-4.0 times more sensitive than micro-SPRIA.

  7. Electronic structure of elements and compounds and electronic phases of solids

    International Nuclear Information System (INIS)

    Nadykto, B.A.

    2000-01-01

    The paper reviews technique and computed energies for various electronic states of many-electron multiply charged ions, molecular ions, and electronic phases of solids. The model used allows computation of the state energy for free many-electron multiply charged ions with relative accuracy ∼10 -4 suitable for analysis of spectroscopy data

  8. Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

    Science.gov (United States)

    Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

    2018-04-01

    This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Ultra trace analysis of PAHs by designing simple injection of large amounts of analytes through the sample reconcentration on SPME fiber after magnetic solid phase extraction.

    Science.gov (United States)

    Khodaee, Nader; Mehdinia, Ali; Esfandiarnejad, Reyhaneh; Jabbari, Ali

    2016-01-15

    A simple solventless injection method was introduced based on the using of a solid-phase microextraction (SPME) fiber for injection of large amounts of the analytes extracted by the magnetic solid phase extraction (MSPE) procedure. The resulted extract from MSPE procedure was loaded on a G-coated SPME fiber, and then the fiber was injected into the gas chromatography (GC) injection port. This method combines the advantages of exhaustive extraction property of MSPE and the solvent-less injection of SPME to improve the sensitivity of the analysis. In addition, the analytes were re-concentrated prior to inject into the gas chromatography (GC) inlet because of the organic solvent removing from the remaining extract of MSPE technique. Injection of the large amounts of analytes was made possible by using the introduced procedure. Fourteen polycyclic aromatic hydrocarbons (PAHs) with different volatility were used as model compounds to investigate the method performance for volatile and semi-volatile compounds. The introduced method resulted in the higher enhancement factors (5097-59376), lower detection limits (0.29-3.3pgmL(-1)), and higher sensitivity for the semi-volatile compounds compared with the conventional direct injection method. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Homogeneous nucleation in phase separation of solid 3He-4He mixtures

    International Nuclear Information System (INIS)

    Poole, M.; Smith, A.; Maidanov, V.A.; Rudavskii, E.Ya.; Grigor'ev, V.N.; Slezov, V.V.; Saunders, J.; Cowan, B.

    2003-01-01

    NMR and pressure have been measured during phase separation in solid 3 He- 4 He mixtures. Spin echoes were used to observe bounded diffusion and to estimate the diffusion coefficient, size and nuclei concentration in the 3 He-enriched phase. The characteristic phase separation time constant of the mixture was found from pressure measurements. The results argue convincingly for homogeneous nucleation. The surface tension of the nuclei is found independently from NMR and from pressure measurements; the two determinations agree well and yield a surface tension coefficient of 4.9x10 -6 J m -2

  11. Dispersive solid-phase imprinting of proteins for the production of plastic antibodies

    DEFF Research Database (Denmark)

    Ashley, Jon; Feng, Xiaotong; Halder, Arnab

    2018-01-01

    We describe a novel dispersive solid-phase imprinting technique for the production of nano-sized molecularly imprinted polymers (nanoMIPs) as plastic antibodies. The template was immobilized on in-house synthesized magnetic microspheres instead of conventional glass beads. As a result, high...

  12. Rapid and convenient semi-automated microwave-assisted solid-phase synthesis of arylopeptoids

    DEFF Research Database (Denmark)

    Rasmussen, Jakob Ewald; Boccia, Marcello Massimo; Nielsen, John

    2014-01-01

    A facile and expedient route to the synthesis of arylopeptoid oligomers (N-alkylated aminomethyl benz-amides) using semi-automated microwave-assisted solid-phase synthesis is presented. The synthesis was optimized for the incorporation of side chains derived from sterically hindered or unreactive...

  13. Chemically and geographically distinct solid-phase iron pools in the Southern Ocean

    CSIR Research Space (South Africa)

    Mtshali, TN

    2012-11-01

    Full Text Available Iron is a limiting nutrient in many parts of the oceans, including the unproductive regions of the Southern Ocean. Although the dominant fraction of the marine iron pool occurs in the form of solid-phase particles, its chemical speciation...

  14. Long-wave equivalent viscoelastic solids for porous rocks saturated by two-phase fluids

    Science.gov (United States)

    Santos, J. E.; Savioli, G. B.

    2018-04-01

    Seismic waves traveling across fluid-saturated poroelastic materials with mesoscopic-scale heterogeneities induce fluid flow and Biot's slow waves generating energy loss and velocity dispersion. Using Biot's equations of motion to model these type of heterogeneities would require extremely fine meshes. We propose a numerical upscaling procedure to determine the complex and frequency dependent P-wave and shear moduli of an effective viscoelastic medium long-wave equivalent to a poroelastic solid saturated by a two-phase fluid. The two-phase fluid is defined in terms of capillary pressure and relative permeability flow functions. The P-wave and shear effective moduli are determined using harmonic compressibility and shear experiments applied on representative samples of the bulk material. Each experiment is associated with a boundary value problem that is solved using the finite element method. Since a poroelastic solid saturated by a two-phase fluid supports the existence of two slow waves, this upscaling procedure allows to analyze their effect on the mesoscopic-loss mechanism in hydrocarbon reservoir formations. Numerical results show that a two-phase Biot medium model predicts higher attenuation than classic Biot models.

  15. An in-line clean system for the solid-phase extraction of emerging contaminants in natural waters

    OpenAIRE

    Sodré, Fernando F.; Locatelli, Marco Antonio F.; Jardim, Wilson F.

    2010-01-01

    A solid-phase in-line extraction system for water samples containing low levels of emerging contaminants is described. The system was specially developed for large volume samples (up to 4 L) using commercial solid-phase extraction (SPE) cartridges. Four sets containing PTFE-made connectors, brass adapters and ball valves were used to fit SPE cartridges and sample bottles to a 4-port manifold attached to a 20 L carboy. A lab-made vacuum device was connected to the manifold cap. The apparatus i...

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

    DEFF Research Database (Denmark)

    Mathiessen, Bente; Zhuravlev, Fedor

    2013-01-01

    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.......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...

  17. Kinetics of solid-phase in ion exchange on tin hydrogen phosphate

    International Nuclear Information System (INIS)

    Kislitsyn, M.N.; Ketsko, V.A.; Yaroslavtsev, A.B.

    2004-01-01

    Solid state reactions in mixture of tin hydrogen phosphate and alkali metal (M=Na, K, Cs) chlorides have been studied both in the mode of polythermal heating and at a fixed temperature, using data of X-ray phase and thermogravimetric analyses. In the range 400-750 Deg C solid state ion exchange reactions occur in the systems studied and yield mono-- and dialkali phosphates MHSn(PO 4 ) 2 and M 2 Sn(PO 4 ) 2 . Counter diffusion coefficients for alkali metal cations and protons in the matrices of compositions MHSn(PO 4 ) 2 and M 2 Sn(PO 4 ) 2 have been determined [ru

  18. Solid-phase extraction (SPE) of Iron using Lanthanum Silicate ion exchange

    International Nuclear Information System (INIS)

    Kiarostami, V.; Husain, W.

    2002-01-01

    Solid-phase extraction (SPE) is gaining wide use as an effective and speedy technique which reduces solvent usage, disposal costs and extraction time. The analyte is adsorbed from solution onto a solid adsorbent, which is followed by elution of the analyte with a solvent appropriate for instrumental analysis. However, there is an increasing need for new selective adsorbents to expand the area of this technique. Lanthanum silicate ion exchanger, which shows unusual selectivity elements and in this study, it was employed to develop a SPE method for iron ion. Special experiments such as determination of distribution coefficient for iron ion in different solvent systems have been determined

  19. Separation of phenolic acids from sugarcane rind by online solid-phase extraction with high-speed counter-current chromatography.

    Science.gov (United States)

    Geng, Ping; Fang, Yingtong; Xie, Ronglong; Hu, Weilun; Xi, Xingjun; Chu, Qiao; Dong, Genlai; Shaheen, Nusrat; Wei, Yun

    2017-02-01

    Sugarcane rind contains some functional phenolic acids. The separation of these compounds from sugarcane rind is able to realize the integrated utilization of the crop and reduce environment pollution. In this paper, a novel protocol based on interfacing online solid-phase extraction with high-speed counter-current chromatography (HSCCC) was established, aiming at improving and simplifying the process of phenolic acids separation from sugarcane rind. The conditions of online solid-phase extraction with HSCCC involving solvent system, flow rate of mobile phase as well as saturated extent of absorption of solid-phase extraction were optimized to improve extraction efficiency and reduce separation time. The separation of phenolic acids was performed with a two-phase solvent system composed of butanol/acetic acid/water at a volume ratio of 4:1:5, and the developed online solid-phase extraction with HSCCC method was validated and successfully applied for sugarcane rind, and three phenolic acids including 6.73 mg of gallic acid, 10.85 mg of p-coumaric acid, and 2.78 mg of ferulic acid with purities of 60.2, 95.4, and 84%, respectively, were obtained from 150 mg sugarcane rind crude extracts. In addition, the three different elution methods of phenolic acids purification including HSCCC, elution-extrusion counter-current chromatography and back-extrusion counter-current chromatography were compared. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Numerical simulation of polishing U-tube based on solid-liquid two-phase

    Science.gov (United States)

    Li, Jun-ye; Meng, Wen-qing; Wu, Gui-ling; Hu, Jing-lei; Wang, Bao-zuo

    2018-03-01

    As the advanced technology to solve the ultra-precision machining of small hole structure parts and complex cavity parts, the abrasive grain flow processing technology has the characteristics of high efficiency, high quality and low cost. So this technology in many areas of precision machining has an important role. Based on the theory of solid-liquid two-phase flow coupling, a solid-liquid two-phase MIXTURE model is used to simulate the abrasive flow polishing process on the inner surface of U-tube, and the temperature, turbulent viscosity and turbulent dissipation rate in the process of abrasive flow machining of U-tube were compared and analyzed under different inlet pressure. In this paper, the influence of different inlet pressure on the surface quality of the workpiece during abrasive flow machining is studied and discussed, which provides a theoretical basis for the research of abrasive flow machining process.

  1. Basal plane shift as an order parameter of transitions between antiferromagnetic phases of solid oxygen

    International Nuclear Information System (INIS)

    Gomonay, E.V.; Loktev, V.M.

    2005-01-01

    A phenomenological model in the spirit of the Landau theory of phase transitions is derived, and the conditions for existence and phase transitions between different magnetocrystal structures of solid oxygen are analyzed for wide ranges of pressure, temperature and external magnetic field

  2. Characteristics of transfer of europium ions from phosphoric acid solution into the CaSO4·O.5H2O solid phase

    International Nuclear Information System (INIS)

    Berdonosova, D.G.; Burlakova, E.V.; Yasenkova, M.A.; Ivanov, L.N.; Melikhov, I.V.

    1989-01-01

    The mechanism of formation of the precipitated CaSO 4 ·0.5H 2 O phase was studied in detail; the precipitation was performed at 80 degree, equimolar solutions of Ca(H 2 PO 4 ) 2 and H 2 SO 4 in phosphoric acid of 38% concentration being used. The availability of detailed information on the mechanism of formation of CaSO 4 ·0.5H 2 O precipitates determined the choice of conditions of study of capture of rare earths. In particular, H 3 PO 4 of 38% P 2 O 5 concentration was used as the medium of formation of the calcium sulfate precipitate. Europium was chosen as the rare earth. Its behavior in the liquid and solid phases was studied by radiometric and luminescence methods. The radionuclide 152 Eu is convenient as a radioactive tracer while luminescence of europium is structure-sensitive; therefore, europium is often used in physicochemical investigations as a luminescent probe. It follows from the data that most of the europium captured by the precipitate during coagulation of the ultramicrocrystals is retained firmly by the solid phase. Therefore, in order to diminish capture of europium (and other rare earths) by the precipitate coagulation of the latter should be prevented

  3. On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue

    Energy Technology Data Exchange (ETDEWEB)

    Ensafi, Ali A. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)], E-mail: Ensafi@cc.iut.ac.ir; Ghaderi, Ali R. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)

    2007-09-05

    An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5 M HNO{sub 3} and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 {mu}g of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5 M HNO{sub 3} solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ng mL{sup -1} Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ng mL{sup -1} Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments.

  4. On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue

    International Nuclear Information System (INIS)

    Ensafi, Ali A.; Ghaderi, Ali R.

    2007-01-01

    An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5 M HNO 3 and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 μg of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5 M HNO 3 solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ng mL -1 Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ng mL -1 Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments

  5. Liquid-solid surface phase transformation of fluorinated fullerene on monolayer tungsten diselenide

    KAUST Repository

    Song, Zhibo

    2018-04-04

    Hybrid van der Waals heterostructures constructed by the integration of organic molecules and two-dimensional (2D) transition metal dichalcogenide (TMD) materials have useful tunable properties for flexible electronic devices. Due to the chemically inert and atomically smooth nature of the TMD surface, well-defined crystalline organic films form atomically sharp interfaces facilitating optimal device performance. Here, the surface phase transformation of the supramolecular packing structure of fluorinated fullerene (C60F48) on single-layer tungsten diselenide (WSe2) is revealed by low-temperature scanning tunneling microscopy, from thermally stable liquid to solid phases as the coverage increases. Statistical analysis of the intermolecular interaction potential reveals that the repulsive dipole-dipole interaction induced by interfacial charge transfer and substrate-mediated interactions play important roles in stabilizing the liquid C60F48 phases. Theoretical calculations further suggest that the dipole moment per C60F48 molecule varies with the surface molecule density, and the liquid-solid transformation could be understood from the perspective of the thermodynamic free energy for open systems. This study offers insights into the growth behavior at 2D organic/TMD hybrid heterointerfaces.

  6. Liquid-solid surface phase transformation of fluorinated fullerene on monolayer tungsten diselenide

    Science.gov (United States)

    Song, Zhibo; Wang, Qixing; Li, Ming-Yang; Li, Lain-Jong; Zheng, Yu Jie; Wang, Zhuo; Lin, Tingting; Chi, Dongzhi; Ding, Zijing; Huang, Yu Li; Thye Shen Wee, Andrew

    2018-04-01

    Hybrid van der Waals heterostructures constructed by the integration of organic molecules and two-dimensional (2D) transition metal dichalcogenide (TMD) materials have useful tunable properties for flexible electronic devices. Due to the chemically inert and atomically smooth nature of the TMD surface, well-defined crystalline organic films form atomically sharp interfaces facilitating optimal device performance. Here, the surface phase transformation of the supramolecular packing structure of fluorinated fullerene (C60F48 ) on single-layer tungsten diselenide (WSe2) is revealed by low-temperature scanning tunneling microscopy, from thermally stable liquid to solid phases as the coverage increases. Statistical analysis of the intermolecular interaction potential reveals that the repulsive dipole-dipole interaction induced by interfacial charge transfer and substrate-mediated interactions play important roles in stabilizing the liquid C60F48 phases. Theoretical calculations further suggest that the dipole moment per C60F48 molecule varies with the surface molecule density, and the liquid-solid transformation could be understood from the perspective of the thermodynamic free energy for open systems. This study offers insights into the growth behavior at 2D organic/TMD hybrid heterointerfaces.

  7. Process for forming a homogeneous oxide solid phase of catalytically active material

    Science.gov (United States)

    Perry, Dale L.; Russo, Richard E.; Mao, Xianglei

    1995-01-01

    A process is disclosed for forming a homogeneous oxide solid phase reaction product of catalytically active material comprising one or more alkali metals, one or more alkaline earth metals, and one or more Group VIII transition metals. The process comprises reacting together one or more alkali metal oxides and/or salts, one or more alkaline earth metal oxides and/or salts, one or more Group VIII transition metal oxides and/or salts, capable of forming a catalytically active reaction product, in the optional presence of an additional source of oxygen, using a laser beam to ablate from a target such metal compound reactants in the form of a vapor in a deposition chamber, resulting in the deposition, on a heated substrate in the chamber, of the desired oxide phase reaction product. The resulting product may be formed in variable, but reproducible, stoichiometric ratios. The homogeneous oxide solid phase product is useful as a catalyst, and can be produced in many physical forms, including thin films, particulate forms, coatings on catalyst support structures, and coatings on structures used in reaction apparatus in which the reaction product of the invention will serve as a catalyst.

  8. Improved detection limits for phthalates by selective solid-phase micro-extraction

    KAUST Repository

    Zia, Asif I.

    2016-03-30

    Presented research reports on an improved method and enhanced limits of detection for phthalates; a hazardous additive used in the production of plastics by solid-phase micro-extraction (SPME) polymer in comparison to molecularly imprinted solid-phase extraction (MISPE) polymer. The polymers were functionalized on an interdigital capacitive sensor for selective binding of phthalate molecules from a complex mixture of chemicals. Both polymers owned predetermined selectivity by formation of valuable molecular recognition sites for Bis (2-ethylhexyl) phthalate (DEHP). Polymers were immobilized on planar electrochemical sensor fabricated on a single crystal silicon substrate with 500 nm sputtered gold electrodes fabricated using MEMS fabrication techniques. Impedance spectra were obtained using electrochemical impedance spectroscopy (EIS) to determine sample conductance for evaluation of phthalate concentration in the spiked sample solutions with various phthalate concentrations. Experimental results revealed that the ability of SPME polymer to adsorb target molecules on the sensing surface is better than that of MISPE polymer for phthalates in the sensing system. Testing the extracted samples using high performance liquid chromatography with photodiode array detectors validated the results.

  9. Determination of solid- and liquid-phase gastric emptying half times in cats by use of nuclear scintigraphy.

    Science.gov (United States)

    Costello, M; Papasouliotis, K; Barr, F J; Gruffydd-Jones, T J; Caney, S M

    1999-10-01

    To use nuclear scintigraphy to establish a range of gastric emptying half times (t1/2) following a liquid or solid meal in nonsedated cats. 12 clinically normal 3-year-old domestic shorthair cats. A test meal of 75 g of scrambled eggs labeled with technetium Tc 99m tin colloid was fed to 10 of the cats, and solid-phase gastric emptying t1/2 were determined by use of nuclear scintigraphy. In a separate experiment, 8 of these cats plus an additional 2 cats were fed 18 ml (n = 5) or 36 ml (n = 5) of a nutrient liquid meal labeled with technetium Tc 99m pentetate. Liquid-phase gastric emptying t1/2 then were determined by use of scintigraphy. Solid-phase gastric emptying t1/2 were between 210 and 769 minutes (median, 330 minutes). Median liquid-phase gastric emptying t1/2 after ingestion of 18 or 36 ml of the test meal were 67 minutes (range, 60 to 96 minutes) and 117 minutes (range, 101 to 170 minutes), respectively. The median t1/2 determined for cats receiving 18 ml of the radiolabeled liquid was significantly less than that determined for cats receiving 36 ml of the test meal. The protocol was tolerated by nonsedated cats. Solid-phase gastric emptying t1/2 were prolonged, compared with liquid-phase t1/2, and a major factor governing the emptying rate of liquids was the volume consumed. Nuclear scintigraphy may prove useful in assessing gastric motility disorders in cats.

  10. DNA microarray-based solid-phase RT-PCR for rapid detection and identification of influenza virus type A and subtypes H5 and H7

    DEFF Research Database (Denmark)

    Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

    2011-01-01

    of RNA extract in the liquid phase with sequence-specific nested PCR on the solid phase. A simple ultraviolet cross-linking method was used to immobilize the DNA probes over an unmodified glass surface, which makes solid-phase PCR a convenient possibility for AIV screening. The testing of 33 avian fecal....... In this article, a DNA microarray-based solid-phase polymerase chain reaction (PCR) approach has been developed for rapid detection of influenza virus type A and for simultaneous identification of pathogenic virus subtypes H5 and H7. This solid-phase RT-PCR method combined reverse-transcription amplification...

  11. The Chemistry, Crystallization, Physicochemical Properties and Behavior of Sodium Aluminosilicate Solid Phases: Final Report

    International Nuclear Information System (INIS)

    Rosencrance, S.

    2003-01-01

    The synthesis of sodium aluminosilicate solids phases precipitated from NO 2 /NO 3 -free and NO 2 /NO 3 -rich liquors has been performed. Four sodium aluminosilicate precipitation products were formed. These are (1) X-ray/electron diffraction-indifferent amorphous phase; (2) crystalline zeolite A; (3)NO 2 /NO 3 -rich crystalline sodalite; and (4) NO 2 /NO 3 -rich crystalline cancrinite phase. Characterization of the physicochemical properties for these phases has been performed under conditions simulating Westinghouse Savannah River Company liquid waste processing

  12. Fluorine incorporation during Si solid phase epitaxy

    International Nuclear Information System (INIS)

    Impellizzeri, G.; Mirabella, S.; Romano, L.; Napolitani, E.; Carnera, A.; Grimaldi, M.G.; Priolo, F.

    2006-01-01

    We have investigated the F incorporation and segregation in preamorphized Si during solid phase epitaxy (SPE) at different temperatures and for several implanted-F energies and fluences. The Si samples were amorphized to a depth of 550 nm by implanting Si at liquid nitrogen temperature and then enriched with F at different energies (65-150 keV) and fluences (0.07-5 x 10 14 F/cm 2 ). Subsequently, the samples were regrown by SPE at different temperatures: 580, 700 and 800 deg. C. We have found that the amount of F incorporated after SPE strongly depends on the SPE temperature and on the energy and fluence of the implanted-F, opening the possibility to tailor the F profile during SPE

  13. A combination of solid-phase extraction and dispersive solid-phase extraction effectively reduces the matrix interference in liquid chromatography-ultraviolet detection during pyraclostrobin analysis in perilla leaves.

    Science.gov (United States)

    Farha, Waziha; Rahman, Md Musfiqur; Abd El-Aty, A M; Jung, Da-I; Kabir, Md Humayun; Choi, Jeong-Heui; Kim, Sung-Woo; Im, So Jeong; Lee, Young-Jun; Shin, Ho-Chul; Kwon, Chan-Hyeok; Son, Young-Wook; Lee, Kang-Bong; Shim, Jae-Han

    2015-12-01

    Perilla leaves contain many interfering substances; thus, it is difficult to protect the analytes during identification and integration. Furthermore, increasing the amount of sample to lower the detection limit worsens the situation. To overcome this problem, we established a new method using a combination of solid-phase extraction and dispersive solid-phase extraction to analyze pyraclostrobin in perilla leaves by liquid chromatography with ultraviolet absorbance detection. The target compound was quantitated by external calibration with a good determination coefficient (R(2) = 0.997). The method was validated (in triplicate) with three fortification levels, and 79.06- 89.10% of the target compound was recovered with a relative standard deviation <4. The limits of detection and quantification were 0.0033 and 0.01 mg/kg, respectively. The method was successfully applied to field samples collected from two different areas at Gwangju and Muan. The decline in the resiudue concentrations was best ascribed to a first-order kinetic model with half-lives of 5.7 and 4.6 days. The variation between the patterns was attributed to humidity. Copyright © 2015 John Wiley & Sons, Ltd.

  14. Comparative evaluation of various solid phases for the development of coated tube assays for the estimation of progesterone in human serum, bovine serum and bovine milk

    International Nuclear Information System (INIS)

    Karir, Tarveen; Samuel, Grace; Sivaprasad, N.; Venkatesh, Meera

    2009-01-01

    Immobilization of progesterone antibody using three polystyrene surfaces and two progesterone radiotracers for use in the development of a coated tube assay for the evaluation of progesterone levels in human serum, bovine serum and bovine milk was studied. The selection of the solid phase and the tracers were based on the maximum binding, non-specific binding, sensitivity and percentage recovery. Amongst the polystyrene tubes studied, streptavidin coated tubes showed the acceptable assay features such as low non-specific binding (0.5-1.0%), adequate sensitivity (0.13-0.16 ng/ml) and recovery (85-115%) for all the three sample matrices, human serum, bovine serum and bovine milk.

  15. Behaviour of solid phase ethyl cyanide in simulated conditions of Titan

    Science.gov (United States)

    Couturier-Tamburelli, I.; Toumi, A.; Piétri, N.; Chiavassa, T.

    2018-01-01

    In order to simulate different altitudes in the atmosphere of Titan, we investigated using infrared spectrometry and mass spectrometry the photochemistry of ethyl cyanide (CH3CH2CN) ices at different temperatures. Heating experiments of the solid phase until complete desorption showed up three phase transitions with a first one appearing to be approximately at the temperature of Titan's surface (94 K), measured by the Huygens probe. Ethyl cyanide, whose presence has been suggested in solid phase in Titan, can be considered as another nitrile for photochemical models of the Titan atmosphere after our first study (Toumi et al., 2016) concerning vinyl cyanide (CH2CHCN). The desorption energy of ethyl cyanide has been calculated to be 36.75 ( ± 0.55) kJ mol-1 using IRTF and mass spectroscopical techniques. High energetic photolysis (λ > 120 nm) have been performed and we identified ethyl isocyanide, vinyl cyanide, cyanoacetylene, ethylene, acetylene, cyanhydric acid and a methylketenimine form as photoproducts from ethyl cyanide. The branching ratios of the primary products were determined at characteristic temperatures of Titan thanks to the value of the νCN stretching band strength of ethyl cyanide that has been calculated to be 4.12 × 10-18 cm molecule-1. We also report here for the first time the values of the photodissociation cross sections of C2H5CN for different temperatures.

  16. Solid phase extraction using molecular imprinting polymers (MISPE for the determination of estrogens in surface water by HPLC

    Directory of Open Access Journals (Sweden)

    Viviane do Nascimento Bianchi

    2017-05-01

    Full Text Available Estrogens are emerging pollutants and traditional sewage treatments unable to remove them. They are harmful to human health and to the environment. It is therefore important to evaluate the presence and concentration of estrogens in water bodies and environmental matrices. This work presents the development and application of a methodology for the determination of E1, E3, EE2 and E2 in surface waters using solid phase extraction with molecular imprinting polymers (MISPE followed by identification and quantification by HPLC-DAD. Acetonitrile and water deionized acidified with phosphoric acid pH 3 (1:1, v/v, a flow rate of 1.0 ml min-1, at 40°C and an injection volume of 5 µL. The method was validated according to the protocol ICH Q2R. Reproducibility and repeatability tests resulted in a smaller variation coefficient of 10%; the calibration curves in the concentration ranged from 1 to 20 mg L-1, with return linearity values greater than 0.99. The limits of detection and quantification were less than 1 mg L-1 and the method was satisfactory for specificity and selectivity tests using caffeine, which is often found in water bodies receiving effluent, and DES, an estrogen used in the treatment of prostate cancer. Selected samples underwent clean-up and pre-concentration treatments using solid phase extraction with commercial phase (C18 and molecularly imprinted polymers (MISPE. The analysis of MISPE extracts indicate that it is possible to obtain results with greater sensitivity and precision for analyses of complex environmental matrices, demonstrating that the developed method can be applied in complex environmental matrices.

  17. Highly Selective Liquid-Phase Benzylation of Anisole with Solid-Acid Zeolite Catalysts

    DEFF Research Database (Denmark)

    Poreddy, Raju; Shunmugavel, Saravanamurugan; Riisager, Anders

    2015-01-01

    Zeolites were evaluated as solid acid catalysts for the liquid-phase benzylation of anisole with benzyl alcohol, benzyl bromide, and benzyl chloride at 80 °C. Among the examined zeolites, H-mordenite-10 (H-MOR-10) demonstrated particular high activity (>99 %) and excellent selectivity (>96...

  18. Solid-phase synthesis of an apoptosis-inducing tetrapeptide mimicking the Smac protein

    DEFF Research Database (Denmark)

    Le Quement, Sebastian Thordal; Ishøy, Mette; Petersen, Mette Terp

    2011-01-01

    An approach for the solid-phase synthesis of apoptosis-inducing Smac peptidomimetics is presented. Using a Rink linker strategy, tetrapeptides mimicking the N-4-terminal residue of the Smac protein [(N-Me)AVPF sequence] were synthesized on PEGA resin in excellent purities and yields. Following two...

  19. An enhanced electronic topology aimed at improving the phase sensitivity of GMI sensors

    International Nuclear Information System (INIS)

    Costa Silva, E; Gusmão, L A P; Hall Barbosa, C R; Costa Monteiro, E

    2014-01-01

    The giant magnetoimpedance effect (GMI) is used in the most recent technologies developed for the detection of magnetic fields, showing potential to be applied in the measurement of ultra-weak fields. GMI samples exhibit a huge dependency of their electrical impedance on the magnetic field, which makes them excellent magnetic sensors. In spite of GMI magnetometers being mostly based on magnitude impedance characteristics, it was previously verified that sensitivity could be significantly increased by reading the impedance phase. Pursuing this idea, a phase-based GMI magnetometer has been already developed as well as an electronic configuration capable of improving the phase sensitivity of GMI samples. However, when using this topology, it was noted that the sensitivity improvement comes at the cost of reduced voltage levels in the reading terminal, degrading the signal-to-noise ratio. Another drawback of the electronic configuration was that it was not capable of enforcing a linear behavior of the impedance phase in the function of the magnetic field in a given operation region. Aiming at overcoming those issues and then optimizing the behavior of the circuit developed to improve the phase sensitivity, this paper mathematically describes a completely new methodology, presents an enhanced newly developed electronic topology and exemplifies its application. (paper)

  20. Mechanism of Formation of Li 7 P 3 S 11 Solid Electrolytes through Liquid Phase Synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yuxing [Energy; Lu, Dongping [Energy; Bowden, Mark [Environmental; El Khoury, Patrick Z. [Environmental; Han, Kee Sung [Environmental; Deng, Zhiqun Daniel [Energy; Xiao, Jie [Energy; Zhang, Ji-Guang [Energy; Liu, Jun [Energy

    2018-01-22

    Crystalline Li7P3S11 is a promising solid electrolyte for all solid state lithium/lithium ion batteries. A controllable liquid phase synthesis of Li7P3S11 is more desirable compared to conventional mechanochemical synthesis, but recent attempts suffer from reduced ionic conductivities. Here we elucidate the formation mechanism of crystalline Li7P3S11 synthesized in the liquid phase (acetonitrile, or ACN). We conclude that the crystalline Li7P3S11 forms through a two-step reaction: 1) formation of solid Li3PS4∙ACN and amorphous Li2S∙P2S5 phases in the liquid phase; 2) solid-state conversion of the two phases. The implication of this two-step reaction mechanism to the morphology control and the transport properties of liquid phase synthesized Li7P3S11 is identified and discussed.

  1. Zirconia-based solid state chemical gas sensors

    CERN Document Server

    Zhuiykov, S

    2000-01-01

    This paper presents an overview of chemical gas sensors, based on solid state technology, that are sensitive to environmental gases, such as O sub 2 , SO sub x , NO sub x , CO sub 2 and hydrocarbons. The paper is focussed on performance of electrochemical gas sensors that are based on zirconia as a solid electrolyte. The paper considers sensor structures and selection of electrode materials. Impact of interfaces on sensor performance is discussed. This paper also provides a brief overview of electrochemical properties of zirconia and their effect on sensor performance. Impact of auxiliary materials on sensors performance characteristics, such as sensitivity, selectivity, response time and recovery time, is also discussed. Dual gas sensors that can be applied for simultaneous monitoring of the concentration of both oxygen and other gas phase components, are briefly considered

  2. Deposition of hole-transport materials in solid-state dye-sensitized solar cells by doctor-blading

    KAUST Repository

    Ding, I-Kang; Melas-Kyriazi, John; Cevey-Ha, Ngoc-Le; Chittibabu, Kethinni G.; Zakeeruddin, Shaik M.; Grä tzel, Michael; McGehee, Michael D.

    2010-01-01

    We report using doctor-blading to replace conventional spin coating for the deposition of the hole-transport material spiro-OMeTAD (2,20,7,70-tetrakis-(N, N-di-p-methoxyphenylamine)- 9,90-spirobifluorene) in solid-state dye-sensitized solar cells

  3. The kinetics of solid phase epitaxy in As-doped buried amorphous silicon layers

    International Nuclear Information System (INIS)

    McCallum, J.C.

    1999-01-01

    Ion implantation is the principal method used to introduce dopants into silicon for fabrication of semiconductor devices. During ion implantation, damage accumulates in the crystalline silicon lattice and amorphisation may occur over the depth range of the ions if the implant dose is sufficiently high. As device dimensions shrink, the need to produce shallower and shallower highly-doped layers increases and the probability of amorphisation also increases. To achieve dopant-activation, the amorphous or damaged material must be returned to the crystalline state by thermal annealing. Amorphous silicon layers can be crystallised by the solid-state process of solid phase epitaxy (SPE) in which the amorphous layer transforms to crystalline silicon (c-Si) layer by layer using the underlying c-Si as a seed. The atomic mechanism that is responsible for the crystallisation is thought to involve highly-localised bond-breaking and rearrangement processes at the amorphous/crystalline (a/c) interface but the defect responsible for these bond rearrangements has not yet been identified. Since the bond breaking process necessarily generates dangling bonds, it has been suggested that the crystallisation process may solely involve the formation and migration of dangling bonds at the interface. One of the key factors which may shed further light on the nature of the SPE defect is the observed dopant-dependence of the rate of crystallisation. It has been found that moderate concentrations of dopants enhance the SPE crystallisation rate while the presence of equal concentrations of an n-type and a p-type dopant (impurity compensation) returns the SPE rate to the intrinsic value. This provides crucial evidence that the SPE mechanism is sensitive to the position of the Fermi level in the bandgap of the crystalline and/or the amorphous silicon phases and may lead to identification of an energy level within the bandgap that can be associated with the defect. This paper gives details of SPE

  4. Phase-field-crystal model for magnetocrystalline interactions in isotropic ferromagnetic solids

    Science.gov (United States)

    Faghihi, Niloufar; Provatas, Nikolas; Elder, K. R.; Grant, Martin; Karttunen, Mikko

    2013-09-01

    An isotropic magnetoelastic phase-field-crystal model to study the relation between morphological structure and magnetic properties of pure ferromagnetic solids is introduced. Analytic calculations in two dimensions were used to determine the phase diagram and obtain the relationship between elastic strains and magnetization. Time-dependent numerical simulations in two dimensions were used to demonstrate the effect of grain boundaries on the formation of magnetic domains. It was shown that the grain boundaries act as nucleating sites for domains of reverse magnetization. Finally, we derive a relation for coercivity versus grain misorientation in the isotropic limit.

  5. Solid phase radioimmunoassay for detection of serum autoantibodies in systemic lupus erythematosus

    Energy Technology Data Exchange (ETDEWEB)

    Smith, K O; Harrington, J T; Gehle, W D

    1977-03-01

    Solid phase radioimmunoassay (RIA) methods for measuring autoantibodies in systemic lupus erythematosus (SLE) patients' serum were developed to improve the sensitvity and quantitative precision of the determinations. Two mechanical systems were studied: (1) acetone fixed cell monolayers in glass tubes and (2) antigen coated plastic beads. Both systems were senssitive and reproducible. The most sensitive, versatile system involves the coating of the plastic beads with nuclear antigen(s), incubation overnight with sera and labelling with /sup 125/I conjugated antihuman globulin. Linear binding of this radioactive tag is obtained over a wide range of SLE serum dilutions and the slopes of the serum dilution titration curves are almost identical for all SLE patients' sera tested. Therefore, a standard titration curve can be constructed from the results with a positive serum, and end-point dilutions of unknown sera estimated from results obtained with a single serum dilution. Alternatively, binding ratios of unknown sera can be usefully compared at fixed dilutions with standard positive and negative sera. For example, high binding ratios (>3.0) were obtained with 19/20 SLE sera and 0/20 control sera. Antigens used in these systems include crude, whole-cell lysates and lysates from purified nuclei.

  6. Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

    2012-02-01

    The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

  7. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

  8. Phase transitions in solid Kr-CH4 solutions and rotational excitations in phase II

    International Nuclear Information System (INIS)

    Bagatskii, M.I.; Mashchenko, D.A.; Dudkin, V.V.

    2007-01-01

    The heat capacity C p of solid Kr-n CH 4 solutions with the CH 4 concentrations n=0.82, 0.86, 0.90 as well as solutions with n=0.90, 0.95 doped with 0.002 O 2 impurity has been investigated under equilibrium vapor pressure over the internal 1-24 K. The (T,n)-phase diagram was refined and the region of two-phase states was determined for Kr-n CH 4 solid solutions. The contribution of the rotational subsystem, C r ot, to the heat capacity of the solutions has been separated. Analysis of C r ot(T) at T 1 and E 2 between the tunnel levels of the A-, T- and A-, E--nuclear-spin species of CH 4 molecules in the orientationally ordered subsystem, and to determine the effective energy gaps E 1 between lowest levels of the A- and T- species. The relations τ(n) and E 1 (n) stem from changes of the effective potential field caused as the replacement of CH 4 molecules by Kr atoms at sites of the ordered sublattices. The effective gaps E L between a group of tunnel levels of the ground-state liberation state and the nearest group of excited levels of the liberation state of the ordered CH 4 molecules in the solutions with n=0.90 (E L =52 K) and 0.95 (E L =55 K) has been estimated

  9. Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

    Science.gov (United States)

    Taherpour, Avat (Arman)

    2010-01-01

    Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

  10. Room-temperature solid phase ionic liquid (RTSPIL) coated Ω-transaminases: Development and application in organic solvents

    DEFF Research Database (Denmark)

    Grabner, B.; Nazario, M. A.; Gundersen, M. T.

    2018-01-01

    ω-Transaminases ATA-40, ATA-47 and ATA-82P were coated with room-temperature solid phase ionic liquids (RTSPILs) by means of three methods, melt coating, precipitation coating, and co‐lyophilization, and showed increased stability in all of the five tested organic solvents. Co‐lyophilization and ......ω-Transaminases ATA-40, ATA-47 and ATA-82P were coated with room-temperature solid phase ionic liquids (RTSPILs) by means of three methods, melt coating, precipitation coating, and co‐lyophilization, and showed increased stability in all of the five tested organic solvents. Co...

  11. Automated Online Solid-Phase Derivatization for Sensitive Quantification of Endogenous S-Nitrosoglutathione and Rapid Capture of Other Low-Molecular-Mass S-Nitrosothiols.

    Science.gov (United States)

    Wang, Xin; Garcia, Carlos T; Gong, Guanyu; Wishnok, John S; Tannenbaum, Steven R

    2018-02-06

    S-Nitrosothiols (RSNOs) constitute a circulating endogenous reservoir of nitric oxide and have important biological activities. In this study, an online coupling of solid-phase derivatization (SPD) with liquid chromatography-mass spectrometry (LC-MS) was developed and applied in the analysis of low-molecular-mass RSNOs. A derivatizing-reagent-modified polymer monolithic column was prepared and adapted for online SPD-LC-MS. Analytes from the LC autosampler flowed through the monolithic column for derivatization and then directly into the LC-MS for analysis. This integration of the online derivatization, LC separation, and MS detection facilitated system automation, allowing rapid, laborsaving, and sensitive detection of RSNOs. S-Nitrosoglutathione (GSNO) was quantified using this automated online method with good linearity (R 2 = 0.9994); the limit of detection was 0.015 nM. The online SPD-LC-MS method has been used to determine GSNO levels in mouse samples, 138 ± 13.2 nM of endogenous GSNO was detected in mouse plasma. Besides, the GSNO concentrations in liver (64.8 ± 11.3 pmol/mg protein), kidney (47.2 ± 6.1 pmol/mg protein), heart (8.9 ± 1.8 pmol/mg protein), muscle (1.9 ± 0.3 pmol/mg protein), hippocampus (5.3 ± 0.9 pmol/mg protein), striatum (6.7 ± 0.6 pmol/mg protein), cerebellum (31.4 ± 6.5 pmol/mg protein), and cortex (47.9 ± 4.6 pmol/mg protein) were also successfully quantified. When the derivatization was performed within 8 min, followed by LC-MS detection, samples could be rapidly analyzed compared with the offline manual method. Other low-molecular-mass RSNOs, such as S-nitrosocysteine and S-nitrosocysteinylglycine, were captured by rapid precursor-ion scanning, showing that the proposed method is a potentially powerful tool for capture, identification, and quantification of RSNOs in biological samples.

  12. Aspects pertinent to the usefulness of a solid phase radio-immuno-sorbent assay for the detection of spermatozoa antibodies in sera of infertility patients

    International Nuclear Information System (INIS)

    Hinrichs-Reiche, I.

    1987-01-01

    The solid phase Radio-Immuno-Sorbent Assay (RISA) is a highly sensitive and valid test to detect 125-iodinetagged antibodies to spermatozoa that allows qualitative and quantitative evaluations of sperm-incapacitating immunglobulin Ig G in sera from patients believed to be infertile for immunological reasons. The study failed to reveal any correlations between the results of RISA and those of micro-sperm-agglutination or micro-sperm-immobilisation tests. There was a major body of evidence pointing to possible links between female isoimmunity and male autoimmunity. (TRV) [de

  13. Investigating the Retention Mechanisms of Liquid Chromatography Using Solid-Phase Extraction Cartridges

    Science.gov (United States)

    O'Donnell, Mary E.; Musial, Beata A.; Bretz, Stacey Lowery; Danielson, Neil D.; Ca, Diep

    2009-01-01

    Liquid chromatography (LC) experiments for the undergraduate analytical laboratory course often illustrate the application of reversed-phase LC to solve a separation problem, but rarely compare LC retention mechanisms. In addition, a high-performance liquid chromatography instrument may be beyond what some small colleges can purchase. Solid-phase…

  14. An efficient digital phase sensitive detector for use in electron spin resonance spectroscopy

    International Nuclear Information System (INIS)

    Vistnes, A.I; Wormald, D.I.; Isachsen, S.

    1983-10-01

    A digital sensitive detector for a modified Bruker electron spin resonance spectrometer, equipped with an Aspect 2000 minicomputer, is described. Magnetic field modulation is derived from a clock in the computer, which makes it possible to perform the data acquisition fully synchronously with the modulation. The resulting high phase accuracy makes it possible to compress the data to a single modulation period before the Fourier transformation. Both the in-phase and the phase-quadrature signals (of the first or second harmonic) are recorded simultaneously. The system makes the data processing, including the Fourier transformation, approximately 1000 times faster than previously reported digital phase sensitive detector systems for electron spin resonance spectrometers

  15. Paper-based quasi-solid dye-sensitized solar cells

    International Nuclear Information System (INIS)

    Bella, Federico; Pugliese, Diego; Zolin, Lorenzo; Gerbaldi, Claudio

    2017-01-01

    Highlights: • Natural cellulose fibres as photoanode and electrolyte for dye-sensitized solar cells. • TiO_2-laden paper foils as photoanodes obtained by papermaking. • Nanoscale microfibrillated cellulose as polymer electrolyte. • Efficiencies as high as 3.55% under 1 sun irradiation. • Stability equal to 96% after 1000 h of accelerated aging test. - Abstract: Natural cellulose fibres are proposed as promising components for bioderived photoanodes and polymer electrolytes in dye-sensitized solar cells (DSSCs). In particular, TiO_2-laden paper foils, prepared by simple papermaking, can be applied to several substrates (conductive glass or plastics) instead of the high-temperature sintered traditional commercial pastes. In addition, nanoscale microfibrillated cellulose is used as reinforcing filler in acrylate/methacrylate-based thermo-set polymer electrolyte membranes prepared by means of fast, low-cost and green UV-induced free-radical photopolymerization. The laboratory-scale quasi-solid state paper-DSSCs assembled with cellulose-based electrodes and electrolytes guarantee sunlight conversion efficiencies as high as 3.55 and 5.20% at simulated light intensities of 1 and 0.2 sun, respectively, along with an excellent efficiency retention of 96% after 1000 h of accelerated aging test. The simple, low cost and green approach here specifically developed opens up intriguing prospects in the design of bio-inspired energy conversion devices showing high performance, outstanding durability and truly sustainable characteristics.

  16. Solid-phase synthesis of yttrium ferrites with structures of perovskite and garnet

    Energy Technology Data Exchange (ETDEWEB)

    Tkachenko, E V; Shapovalov, A G; Aksel' rod, N L; Pazdnikov, I P [Ural' skij Gosudarstvennyj Univ., Sverdlovsk (USSR)

    1980-09-01

    The solid phase synthesis of yttrium ferrites having a perovskite- and garnet-like structure has been investigated in the temperature range from 800 to 1500 deg C and temper times of up to 80 hours by reaction zone simulation and magnetic phase analysis. It is shown that for conversion degrees d<0.15 the reactions are diffusion-controlled. The rate constants and effective diffusion in the formation of YFeO/sub 3/ and Y/sub 3/Fe/sub 5/O/sub 12/ have been determined.

  17. Recent Developments and Applications of Solid Phase Microextraction (SPME in Food and Environmental Analysis—A Review

    Directory of Open Access Journals (Sweden)

    Sybille Merkle

    2015-06-01

    Full Text Available Solid-phase microextraction (SPME is a simple, sensitive, rapid and solvent-free technique for the extraction of analytes from gaseous, liquid and solid samples and takes a leading position among microextraction methods. Application of SPME in sample preparation has been increasing continuously over the last decade. It is most often used as an automatized fiber injection system coupled to chromatographic separation modules for the extraction of volatile and semivolatile organic compounds and also allows for the trace analysis of compounds in complex matrices. Since SPME was first introduced in the early 1990s, several modifications have been made to adapt the procedure to specific application requirements. More robust fiber assemblies and coatings with higher extraction efficiencies, selectivity and stability have been commercialized. Automation and on-line coupling to analytical instruments have been achieved in many applications and new derivatization strategies as well as improved calibration procedures have been developed to overcome existing limitations regarding quantitation. Furthermore, devices using tubes, needles or tips for extraction instead of a fiber have been designed. In the field of food analysis, SPME has been most often applied to fruit/vegetables, fats/oils, wine, meat products, dairy and beverages whereas environmental applications focus on the analysis of air, water, soil and sediment samples.

  18. Visual monitoring of solid-phase extraction using chromogenic fluorous synthesis supports.

    Science.gov (United States)

    Blackburn, Christopher

    2012-03-12

    Reductive aminations and further transformations of an azo dye and fluorous tagged aldehyde are described. The intensely colored 2,4-dialkoxybenzyl protected amines undergo Fmoc-based peptide coupling, Suzuki reactions, and sulfonamide formation with product isolation facilitated by visual monitoring of fluorous solid phase extraction. Target compounds are released from the supports in high yields and purities by treatment with trifluoroacetic acid (TFA).

  19. A Facile, Choline Chloride/Urea Catalyzed Solid Phase Synthesis of Coumarins via Knoevenagel Condensation

    Directory of Open Access Journals (Sweden)

    Hosanagara N. Harishkumar

    2011-01-01

    Full Text Available The influence of choline chloride/urea ionic liquid in solid phase on the Knoevenagel condensation is demonstrated. The active methylene compounds such as meldrum’s acid, diethylmalonate, ethyl cyanoacetate, dimethylmalonate, were efficiently condensed with various salicylaldehydes in presence of choline chloride/urea ionic liquid without using any solvents or additional catalyst. The reaction is remarkably facile because of the air and water stability of the catalyst, and needs no special precautions. The reactions were completed within 1hr with excellent yields (95%. The products formed were sufficiently pure, and can be easily recovered. The use of ionic liquid choline chloride/urea in solid phase offered several significant advantages such as low cost, greater selectivity and easy isolation of products.

  20. Development of Reverse-Phase HPLC Method for Simultaneous ...

    African Journals Online (AJOL)

    Erah

    Purpose: To develop a simple, sensitive and rapid reverse phase HPLC method for the simultaneous analysis of metoprolol succinate and hydrochlorothiazide in a solid dosage form. Methods: The .... Extraction was carried out three times with.

  1. All-optical WDM Regeneration of DPSK Signals using Optical Fourier Transformation and Phase Sensitive Amplification

    DEFF Research Database (Denmark)

    Guan, Pengyu; Røge, Kasper Meldgaard; Kjøller, Niels-Kristian

    2015-01-01

    We propose a novel all-optical WDM regeneration scheme for DPSK signals based on optical Fourier transformation and phase sensitive amplification. Phase regeneration of a WDM signal consisting of 4x10-Gbit/s phase noise degraded DPSK channels is demonstrated for the first time.......We propose a novel all-optical WDM regeneration scheme for DPSK signals based on optical Fourier transformation and phase sensitive amplification. Phase regeneration of a WDM signal consisting of 4x10-Gbit/s phase noise degraded DPSK channels is demonstrated for the first time....

  2. A Two-Phase Solid/Fluid Model for Dense Granular Flows Including Dilatancy Effects

    Science.gov (United States)

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

    2015-04-01

    We propose a thin layer depth-averaged two-phase model to describe solid-fluid mixtures such as debris flows. It describes the velocity of the two phases, the compression/dilatation of the granular media and its interaction with the pore fluid pressure, that itself modifies the friction within the granular phase (Iverson et al., 2010). 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., 2014). In particular, Pitman and Le 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 equations. We close the mixture equations by a weak compressibility relation involving a critical density, or equivalently a critical pressure. Moreover, we relax one boundary condition, making it possible for the fluid to escape the granular media when compression of the granular mass occurs. Furthermore, we introduce second order terms in the equations making it possible to describe the evolution of the pore fluid pressure in response to the compression/dilatation of the granular mass without prescribing an extra ad-hoc equation for the pore pressure. We prove that the energy balance associated with this Jackson closure is dissipative, as well as its thin layer associated model. We present several numerical tests for the 1D case that are compared to the

  3. Phase I study of afatinib combined with nintedanib in patients with advanced solid tumours.

    Science.gov (United States)

    Bahleda, Rastislav; Hollebecque, Antoine; Varga, Andrea; Gazzah, Anas; Massard, Christophe; Deutsch, Eric; Amellal, Nadia; Farace, Françoise; Ould-Kaci, Mahmoud; Roux, Flavien; Marzin, Kristell; Soria, Jean-Charles

    2015-11-17

    This Phase I study evaluated continuous- and intermittent-dosing (every other week) of afatinib plus nintedanib in patients with advanced solid tumours. In the dose-escalation phase (n=45), maximum tolerated doses (MTDs) were determined for continuous/intermittent afatinib 10, 20, 30 or 40 mg once daily plus continuous nintedanib 150 or 200 mg twice daily. Secondary objectives included safety and efficacy. Clinical activity of continuous afatinib plus nintedanib at the MTD was further evaluated in an expansion phase (n=25). The most frequent dose-limiting toxicities were diarrhoea (11%) and transaminase elevations (7%). Maximum tolerated doses were afatinib 30 mg continuously plus nintedanib 150 mg, and afatinib 40 mg intermittently plus nintedanib 150 mg. Treatment-related adverse events (mostly Grade⩽3) included diarrhoea (98%), asthenia (64%), nausea (62%) and vomiting (60%). In the dose-escalation phase, two patients had partial responses (PRs) and 27 (60%) had stable disease (SD). In the expansion phase, one complete response and three PRs were observed (all non-small cell lung cancer), with SD in 13 (52%) patients. No pharmacokinetic interactions were observed. MTDs of continuous or intermittent afatinib plus nintedanib demonstrated a manageable safety profile with proactive management of diarrhoea. Antitumour activity was observed in patients with solid tumours.

  4. Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

    Science.gov (United States)

    Herrero Latorre, C; Barciela García, J; García Martín, S; Peña Crecente, R M

    2013-12-04

    Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Diffusion relaxation times of nonequilibrium isolated small bodies and their solid phase ensembles to equilibrium states

    Science.gov (United States)

    Tovbin, Yu. K.

    2017-08-01

    The possibility of obtaining analytical estimates in a diffusion approximation of the times needed by nonequilibrium small bodies to relax to their equilibrium states based on knowledge of the mass transfer coefficient is considered. This coefficient is expressed as the product of the self-diffusion coefficient and the thermodynamic factor. A set of equations for the diffusion transport of mixture components is formulated, characteristic scales of the size of microheterogeneous phases are identified, and effective mass transfer coefficients are constructed for them. Allowing for the developed interface of coexisting and immiscible phases along with the porosity of solid phases is discussed. This approach can be applied to the diffusion equalization of concentrations of solid mixture components in many physicochemical systems: the mutual diffusion of components in multicomponent systems (alloys, semiconductors, solid mixtures of inert gases) and the mass transfer of an absorbed mobile component in the voids of a matrix consisting of slow components or a mixed composition of mobile and slow components (e.g., hydrogen in metals, oxygen in oxides, and the transfer of molecules through membranes of different natures, including polymeric).

  6. Solid-phase extraction of berries’ anthocyanins and evaluation of their antioxidative properties

    Czech Academy of Sciences Publication Activity Database

    Denev, P.; Číž, Milan; Ambrožová, Gabriela; Lojek, Antonín; Yanakieva, I.; Kratchanova, M.

    2010-01-01

    Roč. 123, č. 4 (2010), s. 1055-1061 ISSN 0308-8146 R&D Projects: GA MŠk(CZ) OC08058 Institutional research plan: CEZ:AV0Z50040507; CEZ:AV0Z50040702 Keywords : anthocyanins * solid-phase extraction * berry extracts Subject RIV: BO - Biophysics Impact factor: 3.458, year: 2010

  7. Solid-phase immunoradiometric assay for C-reactive protein using magnetisable cellulose particles

    International Nuclear Information System (INIS)

    Beer, F.C. de; Pepys, M.B.

    1982-01-01

    An immunoradiometric assay (IRMA) for C-reactive protein (CRP) was developed using magnetisable cellulose particles as the solid-phase support for anti-CRP antibodies. 125 I-labelled immunopurified anti-CRP antibody was used to quantitate the amount of CRP taken up by the solid phase. Unbound label was easily and rapidly removed by decantation after sedimenting the particles on a magnet. The assay could detect 1 μg CRP/l and had a range of up to 10 mg/l with the portion of the standard curve between 10 μg/l and 2-3 mg/l being linear. Fifty samples per hour could be processed manually from serum to CRP result with an intra-assay CV of 5.2% and an inter-assay CV of 10.0%, based on 5 replicates of 5 samples with CRP levels between 2 mg/l and 180 mg/l run in 5 separate assays. Fifty clinical samples were assayed in parallel with a standard electroimmunoassay and yielded a linear correlation coefficient (r) of 0.975 and a slope of 0.98. With its single, brief incubation step including all reagents and its simple phase separation procedure the present method may be the assay of choice when precise measurement of CRP concentrations is required rapidly. (Auth.)

  8. Solid-Phase and Oscillating Solution Crystallization Behavior of (+)- and (-)-N-Methylephedrine.

    Science.gov (United States)

    Tulashie, Samuel Kofi; Polenske, Daniel; Seidel-Morgenstern, Andreas; Lorenz, Heike

    2016-11-01

    This work involves the study of the solid-phase and solution crystallization behavior of the N-methylephedrine enantiomers. A systematic investigation of the melt phase diagram of the enantiomeric N-methylephedrine system was performed considering polymorphism. Two monotropically related modifications of the enantiomer were found. Solubilities and the ternary solubility phase diagrams of N-methylephedrine enantiomers in 2 solvents [isopropanol:water, 1:3 (Vol) and (2R, 3R)-diethyl tartrate] were determined in the temperature ranges between 15°C and 25°C, and 25°C and 40°C, respectively. Preferential nucleation and crystallization experiments at higher supersaturation leading to an unusual oscillatory crystallization behavior as well as a successful preferential crystallization experiment at lower supersaturation are presented and discussed. Copyright © 2016. Published by Elsevier Inc.

  9. A multilevel simulation approach to derive the slip boundary condition of the solid phase in two-fluid models

    Science.gov (United States)

    Feng, Zhi-Gang; Michaelides, Efstathios; Mao, Shaolin

    2011-11-01

    The simulation of particulate flows for industrial applications often requires the use of a two-fluid model (TFM), where the solid particles are considered as a separate continuous phase. One of the underlining uncertainties in the use of aTFM in multiphase computations comes from the boundary condition of the solid phase. The no-slip condition at a solid boundary is not a valid assumption for the solid phase. Instead, several researchers advocate a slip condition as a more appropriate boundary condition. However, the question on the selection of an exact slip length or a slip velocity coefficient is still unanswered. In the present work we propose a multilevel simulation approach to compute the slip length that is applicable to a TFM. We investigate the motion of a number of particles near a vertical solid wall, while the particles are in fluidization using a direct numerical simulation (DNS); the positions and velocities of the particles are being tracked and analyzed at each time step. It is found that the time- and vertical-space averaged values of the particle velocities converge, yielding velocity profiles that can be used to deduce the particle slip length close to a solid wall. This work was supported by a grant from the DOE-NETL (DE-NT0008064) and by a grant from NSF (HRD-0932339).

  10. Sensitivity and specificity of coherence and phase synchronization analysis

    International Nuclear Information System (INIS)

    Winterhalder, Matthias; Schelter, Bjoern; Kurths, Juergen; Schulze-Bonhage, Andreas; Timmer, Jens

    2006-01-01

    In this Letter, we show that coherence and phase synchronization analysis are sensitive but not specific in detecting the correct class of underlying dynamics. We propose procedures to increase specificity and demonstrate the power of the approach by application to paradigmatic dynamic model systems

  11. Determination of volatile compounds in grape distillates by solid-phase extraction and gas chromatography.

    Science.gov (United States)

    Lukić, Igor; Banović, Mara; Persurić, Dordano; Radeka, Sanja; Sladonja, Barbara

    2006-01-06

    Solid-phase extraction (SPE) procedure on octadecylsilica (C18) was developed for accumulation of volatile compounds from grape distillates. The procedure was optimised for final analysis by capillary gas chromatography. At mass concentrations in model solutions ranging from 0.1 to 50 mg/l solid-phase extraction recoveries of all analytes ranged from 69% for 2-phenylethanol to 102% for capric acid, with RSD values from 2 to 9%. SPE recoveries of internal standards to be added in the sample solution prior to extraction, higher alcohols 2-ethyl-1-hexanol and 1-undecanol, were 97 and 93%, respectively, with RSD values of 3%. Detection limits of analyzed compounds in model solutions ranged from 0.011 mg/l for isoamyl acetate to 0.037 mg/l for caproic acid. Method efficiency was tested in relation to acetic acid content, volume fraction of ethanol and possible matrix effects. A significant influence of matrix on SPE efficiency for geraniol, cis-2-hexen-1-ol and cis-3-hexen-1-ol was detected. For the same reason, 2-phenylethanol could not be determined by developed SPE method in samples of grape distillates. The developed solid-phase extraction method was successfully applied to determine the differences in volatile compound content in different grape distillates produced by the distillation of crushed, pressed and fermented grapes.

  12. Theoretical study on phase coexistence in ferroelectric solid solutions near the tricritical point

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Xiaoyan, E-mail: luxy@hit.edu.cn, E-mail: dzk@psu.edu; Li, Hui [Key Lab of Structures Dynamic Behavior and Control of the Ministry of Education, School of Civil Engineering, Harbin Institute of Technology, Harbin 150001 (China); Zheng, Limei [Condensed Matter Science and Technology Institute, Harbin Institute of Technology, Harbin 150001 (China); Cao, Wenwu [Condensed Matter Science and Technology Institute, Harbin Institute of Technology, Harbin 150001 (China); Department of Mathematics and Materials Research Institute, The Pennsylvania State University, University Park, Pennsylvania 16802 (United States)

    2015-04-07

    Phase coexistence in ferroelectric solid solutions near the tricritical point has been theoretically analyzed by using the Landau-Devonshire theory. Results revealed that different phases having similar potential wells could coexist in a narrow composition range near the tricritical point in the classical Pb(Zr{sub 1−x}Ti{sub x})O{sub 3} system. The potential barrier between potential wells increases with the decrease of temperature. Coexisting phases or different domains of the same phase can produce adaptive strains to maintain atomic coherency at the interfaces or domain walls. Such compatibility strains have influence on the energy potential as well as the stability of relative phases, leading to the appearance of energetically unfavorable monoclinic phases. Those competing and coexisting phases also construct an easy phase transition path with small energy barrier in between, so that very small stimuli can produce large response in compositions near the morphotropic phase boundary, especially near the tricritical point.

  13. Theoretical study on phase coexistence in ferroelectric solid solutions near the tricritical point

    International Nuclear Information System (INIS)

    Lu, Xiaoyan; Li, Hui; Zheng, Limei; Cao, Wenwu

    2015-01-01

    Phase coexistence in ferroelectric solid solutions near the tricritical point has been theoretically analyzed by using the Landau-Devonshire theory. Results revealed that different phases having similar potential wells could coexist in a narrow composition range near the tricritical point in the classical Pb(Zr 1−x Ti x )O 3 system. The potential barrier between potential wells increases with the decrease of temperature. Coexisting phases or different domains of the same phase can produce adaptive strains to maintain atomic coherency at the interfaces or domain walls. Such compatibility strains have influence on the energy potential as well as the stability of relative phases, leading to the appearance of energetically unfavorable monoclinic phases. Those competing and coexisting phases also construct an easy phase transition path with small energy barrier in between, so that very small stimuli can produce large response in compositions near the morphotropic phase boundary, especially near the tricritical point

  14. Multimodal Nonlinear Optical Imaging for Sensitive Detection of Multiple Pharmaceutical Solid-State Forms and Surface Transformations.

    Science.gov (United States)

    Novakovic, Dunja; Saarinen, Jukka; Rojalin, Tatu; Antikainen, Osmo; Fraser-Miller, Sara J; Laaksonen, Timo; Peltonen, Leena; Isomäki, Antti; Strachan, Clare J

    2017-11-07

    Two nonlinear imaging modalities, coherent anti-Stokes Raman scattering (CARS) and sum-frequency generation (SFG), were successfully combined for sensitive multimodal imaging of multiple solid-state forms and their changes on drug tablet surfaces. Two imaging approaches were used and compared: (i) hyperspectral CARS combined with principal component analysis (PCA) and SFG imaging and (ii) simultaneous narrowband CARS and SFG imaging. Three different solid-state forms of indomethacin-the crystalline gamma and alpha forms, as well as the amorphous form-were clearly distinguished using both approaches. Simultaneous narrowband CARS and SFG imaging was faster, but hyperspectral CARS and SFG imaging has the potential to be applied to a wider variety of more complex samples. These methodologies were further used to follow crystallization of indomethacin on tablet surfaces under two storage conditions: 30 °C/23% RH and 30 °C/75% RH. Imaging with (sub)micron resolution showed that the approach allowed detection of very early stage surface crystallization. The surfaces progressively crystallized to predominantly (but not exclusively) the gamma form at lower humidity and the alpha form at higher humidity. Overall, this study suggests that multimodal nonlinear imaging is a highly sensitive, solid-state (and chemically) specific, rapid, and versatile imaging technique for understanding and hence controlling (surface) solid-state forms and their complex changes in pharmaceuticals.

  15. Sensitive characterization of polyphenolic antioxidants in Polygonatum odoratum by selective solid phase extraction and high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Hu, Xin; Zhao, Huading; Shi, Shuyun; Li, Hui; Zhou, Xiaoling; Jiao, Feipeng; Jiang, Xinyu; Peng, Dongming; Chen, Xiaoqin

    2015-08-10

    The complexity of natural products always leads to the co-elution of interfering compounds with bioactive compounds, which then has a detrimental effect on structural elucidation. Here, a new method, based on selective solid phase extraction combined with 1,1-diphenyl-2-picrylhydrazyl radical (DPPH) spiking and high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS), is described for sensitive screening, selective extraction and identification of polyphenolic antioxidants in Polygonatum odoratum. First, 25 polyphenolic antioxidants (1-25) were screened by DPPH spiking with HPLC. Second, polydopamine coated Fe3O4 microspheres (Fe3O4@PDA) were prepared to selectively extract target antioxidants with extraction efficiency from 55% to 100% when the amount of Fe3O4@PDA, extraction time, desorption solvent and time were 10mg, 20 min, acetonitrile, and 5 min. Third, 25 antioxidants (10 cinnamides and 15 homoisoflavanones) were identified by HPLC-DAD-QTOF-MS/MS. Furthermore, the DPPH scavenging activities of purified compounds (IC50, 1.6-32.8 μg/mL) validated the method. Among the identified antioxidants, four of them (12, 13, 18 and 19) were new compounds, four of them (2, 4, 8 and 14) were first obtained from family Liliaceae, five of them (1, 3, 5, 7 and 9) were first reported in genus Polygonatum, while one compound (24) was first identified in this species. The results indicated that the proposed method was an efficient and sensitive approach to explore polyphenolic antioxidants from complex natural products. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Diffusionless phase transition with two order parameters in spin-crossover solids

    Energy Technology Data Exchange (ETDEWEB)

    Gudyma, Iurii, E-mail: yugudyma@gmail.com; Ivashko, Victor [Department of General Physics, Chernivtsi National University, 58012 Chernivtsi (Ukraine); Linares, Jorge [Groupe d' Etude de la Matière Condensée (GEMAC), UMR 8635, CNRS, Université de Versailles Saint Quentin, 45 avenue des Etats-Unis, 78035 Versailles (France)

    2014-11-07

    The quantitative analysis of the interface boundary motion between high-spin and low-spin phases is presented. The nonlinear effect of the switching front rate on the temperature is shown. A compressible model of spin-crossover solid is studied in the framework of the Ising-like model with two-order parameters under statistical approach, where the effect of elastic strain on interaction integral is considered. These considerations led to examination of the relation between the order parameters during temperature changes. Starting from the phenomenological Hamiltonian, entropy has been derived using the mean field approach. Finally, the phase diagram, which characterizes the system, is numerically analyzed.

  17. Chemical cleavage reactions of DNA on solid support: application in mutation detection

    Directory of Open Access Journals (Sweden)

    Cotton Richard GH

    2003-05-01

    Full Text Available Abstract Background The conventional solution-phase Chemical Cleavage of Mismatch (CCM method is time-consuming, as the protocol requires purification of DNA after each reaction step. This paper describes a new version of CCM to overcome this problem by immobilizing DNA on silica solid supports. Results DNA test samples were loaded on to silica beads and the DNA bound to the solid supports underwent chemical modification reactions with KMnO4 (potassium permanganate and hydroxylamine in 3M TEAC (tetraethylammonium chloride solution. The resulting modified DNA was then simultaneously cleaved by piperidine and removed from the solid supports to afford DNA fragments without the requirement of DNA purification between reaction steps. Conclusions The new solid-phase version of CCM is a fast, cost-effective and sensitive method for detection of mismatches and mutations.

  18. Critical micelle concentration values for different surfactants measured with solid-phase microextraction fibers

    NARCIS (Netherlands)

    Haftka, Joris J H; Scherpenisse, Peter; Oetter, G??nter; Hodges, Geoff; Eadsforth, Charles V.; Kotthoff, Matthias; Hermens, Joop L M

    The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibres were used in the present study to measure CMC values of twelve nonionic, anionic, cationic and zwitterionic surfactants. The SPME derived CMC

  19. Solid-phase cloning for high-throughput assembly of single and multiple DNA parts

    DEFF Research Database (Denmark)

    Lundqvist, Magnus; Edfors, Fredrik; Sivertsson, Åsa

    2015-01-01

    We describe solid-phase cloning (SPC) for high-throughput assembly of expression plasmids. Our method allows PCR products to be put directly into a liquid handler for capture and purification using paramagnetic streptavidin beads and conversion into constructs by subsequent cloning reactions. We ...

  20. Solution and solid-phase halogen and C-H hydrogen bonding to perrhenate.

    Science.gov (United States)

    Massena, Casey J; Riel, Asia Marie S; Neuhaus, George F; Decato, Daniel A; Berryman, Orion B

    2015-01-28

    (1)H NMR spectroscopic and X-ray crystallographic investigations of a 1,3-bis(4-ethynyl-3-iodopyridinium)benzene scaffold with perrhenate reveal strong halogen bonding in solution, and bidentate association in the solid state. A nearly isostructural host molecule demonstrates significant C-H hydrogen bonding to perrhenate in the same phases.

  1. Optimized Solid Phase-Assisted Synthesis of Dendrons Applicable as Scaffolds for Radiolabeled Bioactive Multivalent Compounds Intended for Molecular Imaging

    Directory of Open Access Journals (Sweden)

    Gabriel Fischer

    2014-05-01

    Full Text Available Dendritic structures, being highly homogeneous and symmetric, represent ideal scaffolds for the multimerization of bioactive molecules and thus enable the synthesis of compounds of high valency which are e.g., applicable in radiolabeled form as multivalent radiotracers for in vivo imaging. As the commonly applied solution phase synthesis of dendritic scaffolds is cumbersome and time-consuming, a synthesis strategy was developed that allows for the efficient assembly of acid amide bond-based highly modular dendrons on solid support via standard Fmoc solid phase peptide synthesis protocols. The obtained dendritic structures comprised up to 16 maleimide functionalities and were derivatized on solid support with the chelating agent DOTA. The functionalized dendrons furthermore could be efficiently reacted with structurally variable model thiol-bearing bioactive molecules via click chemistry and finally radiolabeled with 68Ga. Thus, this solid phase-assisted dendron synthesis approach enables the fast and straightforward assembly of bioactive multivalent constructs for example applicable as radiotracers for in vivo imaging with Positron Emission Tomography (PET.

  2. Solid-phase extraction NMR studies of chromatographic fractions of saponins from Quillaja saponaria.

    Science.gov (United States)

    Nyberg, Nils T; Baumann, Herbert; Kenne, Lennart

    2003-01-15

    The saponin mixture QH-B from the tree Quillaja saponaria var. Molina was fractionated by RP-HPLC in several steps. The fractions were analyzed by solid-phase extraction NMR (SPE-NMR), a technique combining the workup by solid-phase extraction with on-line coupling to an NMR flow probe. Together with MALDI-TOF mass spectrometry and comparison with chemical shifts of similar saponins, the structures of both major and minor components in QH-B could be obtained. The procedure described is a simple method to determine the structure of components in a complex mixture. The two major fractions of the mixture were found to contain at least 28 saponins, differing in the carbohydrate substructures. Eight of these have not previously been determined. The 28 saponins formed 14 equilibrium pairs by the migration of an O-acyl group between two adjacent positions on a fucosyl residue.

  3. Combination of sawdust from teak wood and rice husk activated carbon as adsorbent of Pb(II) ion and its analysis using solid-phase spectrophotometry (sps)

    Science.gov (United States)

    Saputro, S.; Mahardiani, L.; Wulandari, D. A.

    2018-03-01

    This research aimed to know the usage of sawdust of teak wood and rice husk waste as Pb (II) ion adsorbents in simulated liquid waste, the combined optimum mass required adsorbent to adsorb Pb(II) ion, the sensitivity of the solid-phase spectrophotometry (sps) method in determining the decrease of Pb (II) metal ion levels in the μg/L level. This research was conducted by experimental method in laboratory. Adsorbents used in this study were charcoal of sawdust sawdust activated using 15% ZnCl2 solution and activated rice husk using 2 N NaOH solution. The adsorption processes of sawdust and rice husk with Pb(II) solution was done by variation of mass combination with a ratio of 1: 0; 0: 1; 1: 1; 1: 2; and 2: 1. Analysis of Pb(II) ion concentration using SPS and characterization of sawdust and rice husk adsorbent ads using FTIR. The results showed that activated charcoal from sawdust of teak wood and rice husks can be used as Pb (II) metal ion adsorbents with adsorption capacity of 0.86 μg/L, charcoal from sawdust of teak wood and rice husk adsorbent with a combination of optimum mass contact of sawdust and rice husk is 2:1 as much as 3 grams can adsorb 42.80 μg/L. Solid-phase spectophotometry is a sensitive method for analysis of concentration decreasing levels of Pb(II) ion, after it was absorbed by sawdust of teak wood and rice husk with high sensitivity and has the limit of detection (LOD) of 0.06 μg/L.

  4. Separation of lanthanum (3) and samarium (3) extraction with tributylphosphate in the solvent presence of solid phase

    International Nuclear Information System (INIS)

    Korotkevich, I.B.; Kolesnikov, A.A.; Bomshtejn, V.E.

    1990-01-01

    Lanthanum (3) and samarium (3) extraction from nitric acid solutions by tributylphosphate in the presence of solid phase has been investigated. An increase in samarium α-nitrate distribution factor in the presence of solid phase with a decrease in its concentration in the initial solution and with lanthanum nitrate concentration increase is detected. The greatest effect of separation is observed in samarium nitrate microregion. The method of quantitative extraction of samarium from lanthanum nitrate solutions with samarium-lanthanum separation factor exceeding 50 has been suggested

  5. Treatment technologies of liquid and solid wastes from two-phase olive oil mills

    OpenAIRE

    Borja Padilla, Rafael; Raposo Bejines, Francisco; Rincón, Bárbara

    2006-01-01

    Over the last 10 years the manufacture of olive oil has undergone important evolutionary changes in the equipment used for the separation of olive oil from the remaining components. The latest development has been the introduction of a two-phase centrifugation process in which a horizontally-mounted centrifuge is used for a primary separation of the olive oil fraction from the vegetable solid material and vegetation water. Therefore, the new two-phase olive oil mills produce three ident...

  6. Treatment technologies of liquid and solid wastes from two-phase olive oil mills

    OpenAIRE

    Rincón, Bárbara; Raposo, Francisco; Borja, Rafael

    2006-01-01

    Over the last 10 years the manufacture of olive oil has undergone important evolutionary changes in the equipment used for the separation of olive oil from the remaining components. The latest development has been the introduction of a two-phase centrifugation process in which a horizontally-mounted centrifuge is used for a primary separation of the olive oil fraction from the vegetable solid material and vegetation water. Therefore, the new two-phase olive oil mills produce three identifiabl...

  7. Development of a solid-phase radioimmunoassay for antibody to antigens of Babesia bovis infected bovine erythrocytes

    Energy Technology Data Exchange (ETDEWEB)

    Kahl, L.P.; Anders, R.F.; Mitchell, G.F. (Walter and Eliza Hall Inst. of Medical Research, Parkville (Australia)); Callow, L.L.; Rodwell, B.J. (Animal Research Inst. Wacol (Australia). Tick Fever Research Centre)

    1982-06-01

    A quantitative solid-phase radioimmunoassay (RIA) has been developed for the purpose of ranking sera from exposed animals according to their titre of anti-B. bovis antibody. The antigen was a sonicate of lysed infected blood cells, and antibody binding was detected with /sup 125/I-labelled anti-bovine IgG. The assay was tested using sera from experimentally infected splenectomized and intact cattle and from animals resident in an endemic area. A high specificity for B. bovis was demonstrated. There was good agreement in identifying exposed cattle when the test was compared with an indirect fluorescent antibody (IFA) test although no correlation was seen between titres obtained in the two tests. Analysis of the effects of challenge infection with B. bovis on IFA and RIA titres in previously exposed animals illustrated that the RIA was a more sensitive test for detecting changes in antibody titre.

  8. Electrospun polymethylacrylate nanofibers membranes for quasi-solid-state dye sensitized solar cells

    Directory of Open Access Journals (Sweden)

    M. Fathy

    2016-06-01

    Full Text Available Polymethylacrylate (PMA nanofibers membranes are fabricated by electrospinning technique and applied to the polymer matrix in quasi-solid-state electrolytes for dye sensitized solar cells (DSSCs. There is no previous studies reporting the production of PMA nanofibers. The electrospinning parameters such as polymer concentration, applied voltage, feed rate, tip to collector distance and solvent were optimized. Electrospun PMA fibrous membrane with average fiber diameter of 350 nm was prepared from a 10 wt% solution of PMA in a mixture of acetone/N,N-dimethylacetamide (6:4 v/v at an applied voltage of 20 kV. It was then activated by immersing it in 0.5 M LiI, 0.05 M I2, and 0.5 M 4-tert-butylpyridine in 3-methoxyproponitrile to obtain the corresponding membrane electrolyte with an ionic conductivity of 2.4 × 10−3 S cm−1 at 25 °C. Dye sensitized solar cells (DSSCs employing the quasi solid-state electrolyte have an open-circuit voltage (Voc of 0.65 V and a short circuit current (Jsc of 6.5 mA cm−2 and photoelectric energy conversion efficiency (η of 1.4% at an incident light intensity of 100 mW cm−2.

  9. Novel chemically cross-linked solid state electrolyte for dye-sensitized solar cells

    International Nuclear Information System (INIS)

    Yin Xiong; Tan Weiwei; Xiang Wangchun; Lin Yuan; Zhang Jingbo; Xiao Xurui; Li Xueping; Zhou Xiaowen; Fang Shibi

    2010-01-01

    Poly(vinylpyridine-co-ethylene glycol methyl ether methacrylate) (P(VP-co-MEOMA)) and α,ω-diiodo poly(ethylene oxide-co-propylene oxide) (I[(EO) 0.8 -co-(PO) 0.2 ] y I) were synthesized and used as chemically cross-linked precursors of the electrolyte for dye-sensitized solar cells. Meanwhile, α-iodo poly(ethylene oxide-co-propylene oxide) methyl ether (CH 3 O[(EO) 0.8 -co-(PO) 0.2 ] x I) was synthesized and added into the electrolyte as an internal plasticizer. Novel polymer electrolyte resulting from chemically cross-linked precursors was obtained by the quaterisation at 90 o C for 30 min. The characteristics for this kind of electrolyte were investigated by means of ionic conductivity, thermogravimetric and photocurrent-voltage. The ambient ionic conductivity was significantly enhanced to 2.3 x 10 -4 S cm -1 after introducing plasticizer, modified-ionic liquid. The weight loss of the solid state electrolyte at 200 o C was 1.8%, and its decomposition temperature was 287 o C. Solid state dye-sensitized solar cell based on chemically cross-linked electrolyte presented an overall conversion efficiency of 2.35% under AM1.5 irradiation (100 mW cm -2 ). The as-fabricated device maintained 88% of its initial performance at room temperature even without sealing for 30 days, showing a good stability.

  10. Two-phase air-solid stationary turbulent flow in a cylindrical tube, with a high massive concentration

    International Nuclear Information System (INIS)

    Fortier, Andre; Chen, Che Pen

    1976-01-01

    The momentum theorem, applied separately to the two phases (fluid and solid particles), together with the equations of continuity, gives two differential equations by which the pressure and the concentration along the longitudinal profile x can be computed. These equations can be obtained by introduction of several averaging procedures of physical significance. These quantities are defined in a simple manner for the general case. Using experimental measurements of solid particle velocities in a horizontal tube by radio-tracers, it is shown how to determine the three average coefficients: Λsub(g) friction coefficient of gas, Λsub(s) momentum loss coefficient of solid particles by impacts, against the wall, and Csub(D) drag coefficient due to the velocity difference between the two phases. This determination is based on the numerical solution of the two differential equations conveniently simplified [fr

  11. Simple material physics experiment for studying phase diagrams and solid state transformations in alloys

    Energy Technology Data Exchange (ETDEWEB)

    Kaur, S; Kamal, R [Punjabi Univ., Patiala (India). Dept. of Physics

    1977-09-01

    Study of phase diagram and accompanying solid state transformations is essential to determine the best possible composition, manufacturing techniques and physical properties of an alloy. A simple technique having wide applications in metallurgical industry is to study the temperature--time curve of the alloy undergoing cooling with an uniform rate. An experiment which uses this technique is described. It is widely applicable in the fields of materials science, applied solid state physics, physical metallurgy and physical chemistry.

  12. Preparation of bioconjugates by solid-phase conjugation to ion exchange matrix-adsorbed carrier proteins

    DEFF Research Database (Denmark)

    Houen, G.; Olsen, D.T.; Hansen, P.R.

    2003-01-01

    A solid-phase conjugation method utilizing carrier protein bound to an ion exchange matrix was developed. Ovalbumin was adsorbed to an anion exchange matrix using a batch procedure, and the immobilized protein was then derivatized with iodoacetic acid N-hydroxysuccinimid ester. The activated......, and immunization experiments with the eluted conjugates showed that the more substituted conjugates gave rise to the highest titers of glutathione antibodies. Direct immunization with the conjugates adsorbed to the ion exchange matrix was possible and gave rise to high titers of glutathione antibodies. Conjugates...... of ovalbumin and various peptides were prepared in a similar manner and used for production of peptide antisera by direct immunization with the conjugates bound to the ion exchanger. Advantages of the method are its solid-phase nature, allowing fast and efficient reactions and intermediate washings...

  13. Development of a solid phase technic for radioimmunoassay of triiodothyronine (T3) in serum

    International Nuclear Information System (INIS)

    Hamada, M.M.; Mesquita, C.H.; Silva, C.P.G. da.

    1988-10-01

    We have developed a solid phase radioimmunoassay (RIA) system for triiodothyronine (T 3 ), by immobilizing triiodothyronine antibodies on the inner wall of reaction tubes. The antibody-coated tubes were made via reaction of antibody with glutaraldeyde residue pre coated on the inner wall of the tubes by alkaline self-polimerization. The quality of the coated tubes was tested through its performance in the RIA methodology, by analysing the following RIA parameters: minimum detectable dose (MDD), nonspecific binding (NSB), ''X 50% '', slope of the standard curve, intra and inter-assay precision, accuracy of the method and figure of merit. The serum levels of T 3 in hypothyroid and hyperthyroid patients and the normal values range were determined for the solid phase RIA system. The results are in agreement with found in the literature. (author) [pt

  14. [Improvement of the determination method of benzene, toluene, ethylbenzene and xylene(BTEX) in water using activated carbon fiber solid-phase microextraction/gas chromatography-mass spectrometry(GC-MS)].

    Science.gov (United States)

    Jia, Jin-ping; Feng, Xue; Fang, Neng-hu; Huang, Jia-liang

    2002-01-01

    The methods of direct injection, carbon disulfide extraction and activated carbon fiber solid-phase microextraction/GC-MS, usually used in the determination of BTEX in water matrix, are compared and discussed. Experimental data of linearity, precision and limit of detection illustrate that the last one is better than the two other methods. This method was tested by the practical sample experiments and expected to be a simple and sensitive new method for the analysis of BTEX in water.

  15. Flame atomic absorption spectrometric determination of zinc, nickel, iron and lead in different matrixes after solid phase extraction on sodium dodecyl sulfate (SDS)-coated alumina as their bis (2-hydroxyacetophenone)-1, 3-propanediimine chelates

    International Nuclear Information System (INIS)

    Ghaedi, M.; Tavallali, H.; Shokrollahi, A.; Zahedi, M.; Montazerozohori, M.; Soylak, M.

    2009-01-01

    A sensitive and simple solid phase extraction method for the simultaneous determination of trace and toxic metals in food samples has been reported. The method is based on the adsorption of zinc, nickel, iron and lead on sodium dodecyl sulfate (SDS)-coated alumina, which is also chelated with bis (2-hydroxyacetophenone)-1, 3-propanediimine (BHAPN). The retained analyte ions on modified solid phase were eluted using 8 mL of 4 mol L -1 HNO 3 . The analyte determinations were carried out by flame atomic absorption spectrometry. The influences of some metal ions and anions on the recoveries of understudy analyte ions were investigated. The proposed method has been successfully applied for the evaluation of these trace and toxic metals in some traditional food samples from Iran.

  16. Municipal solid waste development phases: Evidence from EU27.

    Science.gov (United States)

    Vujić, Goran; Gonzalez-Roof, Alvaro; Stanisavljević, Nemanja; Ragossnig, Arne M

    2015-12-01

    Many countries in the European Union (EU) have very developed waste management systems. Some of its members have managed to reduce their landfilled waste to values close to zero during the last decade. Thus, European Union legislation is very stringent regarding waste management for their members and candidate countries, too. This raises the following questions: Is it possible for developing and developed countries to comply with the European Union waste legislation, and under what conditions? How did waste management develop in relation to the economic development in the countries of the European Union? The correlation between waste management practices and economic development was analysed for 27 of the European Union Member States for the time period between 1995 and 2007. In addition, a regression analysis was performed to estimate landfilling of waste in relation to gross domestic product for every country. The results showed a strong correlation between the waste management variables and the gross domestic product of the EU27 members. The definition of the municipal solid waste management development phases followed a closer analysis of the relation between gross domestic product and landfilled waste. The municipal solid waste management phases are characterised by high landfilling rates at low gross domestic product levels, and landfilling rates near zero at high gross domestic product levels. Hence the results emphasize the importance of wider understanding of what is required for developing countries to comply with the European Union initiatives, and highlight the importance of allowing developing countries to make their own paths of waste management development. © The Author(s) 2015.

  17. The EPOS Implementation Phase: building thematic and integrated services for solid Earth sciences

    Science.gov (United States)

    Cocco, Massimo; Epos Consortium, the

    2015-04-01

    The European Plate Observing System (EPOS) has a scientific vision and approach aimed at creating a pan-European infrastructure for Earth sciences to support a safe and sustainable society. To follow this vision, the EPOS mission is integrating a suite of diverse and advanced Research Infrastructures (RIs) in Europe relying on new e-science opportunities to monitor and understand the dynamic and complex Earth system. To this goal, the EPOS Preparatory Phase has designed a long-term plan to facilitate integrated use of data and products as well as access to facilities from mainly distributed existing and new research infrastructures for solid Earth Science. EPOS will enable innovative multidisciplinary research for a better understanding of the Earth's physical processes that control earthquakes, volcanic eruptions, ground instability and tsunami as well as the processes driving tectonics and Earth surface dynamics. Through integration of data, models and facilities EPOS will allow the Earth Science community to make a step change in developing new concepts and tools for key answers to scientific and socio-economic questions concerning geo-hazards and geo-resources as well as Earth sciences applications to the environment and to human welfare. Since its conception EPOS has been built as "a single, Pan-European, sustainable and distributed infrastructure". EPOS is, indeed, the sole infrastructure for solid Earth Science in ESFRI and its pan-European dimension is demonstrated by the participation of 23 countries in its preparatory phase. EPOS is presently moving into its implementation phase further extending its pan-European dimension. The EPOS Implementation Phase project (EPOS IP) builds on the achievements of the successful EPOS preparatory phase project. The EPOS IP objectives are synergetic and coherent with the establishment of the new legal subject (the EPOS-ERIC in Italy). EPOS coordinates the existing and new solid Earth RIs within Europe and builds the

  18. An Organic D-π-A Dye for Record Efficiency Solid-State Sensitized Heterojunction Solar Cells

    KAUST Repository

    Cai, Ning; Moon, Soo-Jin; Cevey-Ha, Lê; Moehl, Thomas; Humphry-Baker, Robin; Wang, Peng; Zakeeruddin, Shaik M.; Grätzel, Michael

    2011-01-01

    The high molar absorption coefficient organic D-π-A dye C220 exhibits more than 6% certified electric power conversion efficiency at AM 1.5G solar irradiation (100 mW cm-2) in a solid-state dye-sensitized solar cell using 2,2′,7,7′-tetrakis

  19. Imaging of surface plasmon polariton interference using phase-sensitive scanning tunneling microscope

    NARCIS (Netherlands)

    Jose, J.; Segerink, Franciscus B.; Korterik, Jeroen P.; Herek, Jennifer Lynn; Offerhaus, Herman L.

    2011-01-01

    We report the surface plasmon polariton interference, generated via a ‘buried’ gold grating, and imaged using a phase-sensitive Photon Scanning Tunneling Microscope (PSTM). The phase-resolved PSTM measurement unravels the complex surface plasmon polariton interference fields at the gold-air

  20. Extinction Ratio and Gain Optimization of Dual- Pump Degenerate-Idler Phase Sensitive Amplifiers

    DEFF Research Database (Denmark)

    Kang, Ning; Lund-Hansen, Toke; Seoane, Jorge

    2011-01-01

    Numerical optimization of dual-pump degenerateidler phase sensitive amplifiers is performed for Al-doped and standard highly nonlinear fibers. Design considerations for operating the PSAs at an optimum combination of gain and extinction ratio are discussed.......Numerical optimization of dual-pump degenerateidler phase sensitive amplifiers is performed for Al-doped and standard highly nonlinear fibers. Design considerations for operating the PSAs at an optimum combination of gain and extinction ratio are discussed....

  1. Separation of lanthanum (3) and neodymium (3) by tributyl phosphate extraction in the presence of solid phase

    International Nuclear Information System (INIS)

    Korotkevich, I.B.; Kolesnikov, A.A.; Bomshtejn, V.E.; Shikhaleeva, N.N.

    1987-01-01

    Lanthanum (3) and neodymium (3) extraction from nitric acid solutions by tributyl phosphate in the presence of solid phase of the element nitrates is investigated. An increase in distribution of neodymium nitrate in the presence of solid phase with the decrease in its concentration in the initial solution and with the increase in lanthanum nitrate concentration is detected. The highest effect of extractive-crystallizational separation is observed in the range of neodymium nitrate microconcentrations. A method of neodymium quantitative extraction from lanthanum nitrate solutions with neodymium - lanthanum separation coefficient exceeding 25 is suggested

  2. Solid-phase extraction and HPLC assay of nicotine and cotinine in plasma and brain.

    Science.gov (United States)

    Dawson, Ralph; Messina, S M; Stokes, C; Salyani, S; Alcalay, N; De Fiebre, N C; De Fiebre, C M

    2002-01-01

    The aim of this study was to develop a simple and reliable assay for nicotine (NIC) and its major metabolite, cotinine (COT), in plasma and brain. A method was developed that uses an extraction method compatible with reverse-phase high-performance liquid chromatography (HPLC) separation and ultraviolet (UV) detection. Sequential solid-phase extraction on silica columns followed by extraction using octadecyl (C18) columns resulted in mean percent recovery (n = 5) of 51 +/- 5, 64 +/- 10, and 52 +/- 10% for NIC, COT, and phenylimidazole (PI), respectively, in spiked 1-mL serum samples. Recovery (mean +/- SEM) of the internal standard (PI) from spiked samples of nicotine-injected rats averaged 64.1 +/- 1.5% (n = 138) from plasma, and 20.7+/-0.8% (n = 128) from brain. The limits of detection of NIC in plasma samples were approximately 8 ng per mL, and of COT, 13.6 ng per mL. Further optimization of our extraction method, using slower flow rates and solid-phase extraction on silica columns, followed by C18 column extraction, yielded somewhat better recoveries (38 +/-3%) for 1-mL brain homogenates. Interassay precision (coefficient of variation) was determined on the basis of daily calibrations for 2 months and was found to be 7%, 9%, and 9% for NIC, COT, and PI, respectively, whereas intra-assay variability was 3.9% for both NIC and COT. Limited studies were performed on analytical columns for comparison of retention, resolution, asymmetry, and column capacity. We concluded that a simple two-step solid-phase extraction method, coupled with HPLC separation and UV detection, can be used routinely to measure NIC and COT in biological fluids and tissues.

  3. Solid-state phase transitions in CuCl under hydrostatic pressures to 12.8 GPa

    International Nuclear Information System (INIS)

    Liebenberg, D.H.; Mills, R.L.; Huang, C.Y.; Olsen, C.; Schmidt, L.C.

    1981-01-01

    The phase transitions in solid CuCl under hydrostatic conditions at pressures to 12.8 GPa are examined. The transition at 4.4 GPa from zinc-blende to tetragonal is observed. Our negative observations for the upper transition at 8.2 GPa and for the formation of an opaque phase due to the disproportionation reaction support the contention that pressure gradients are important in affecting the behavior of pure CuCl

  4. Automated Solid-Phase Subcloning Based on Beads Brought into Proximity by Magnetic Force

    DEFF Research Database (Denmark)

    Hudson, Elton P.; Nikoshkov, Andrej; Uhlén, Mathias

    2012-01-01

    In the fields of proteomics, metabolic engineering and synthetic biology there is a need for high-throughput and reliable cloning methods to facilitate construction of expression vectors and genetic pathways. Here, we describe a new approach for solid-phase cloning in which both the vector and th...

  5. Sensitive determination of bisphenol A and bisphenol F in canned food using a solid-phase microextraction fibre coated with single-walled carbon nanotubes before GC/MS.

    Science.gov (United States)

    Rastkari, N; Ahmadkhaniha, R; Yunesian, M; Baleh, L J; Mesdaghinia, A

    2010-10-01

    A reliable and sensitive method for simultaneous determination of bisphenol A (BPA) and bisphenol F (BPF) in canned food by gas chromatography-mass spectrometry (GC/MS) is described after extraction and pre-concentration by a new solid-phase microextraction (SPME) adsorbent. The potential of single-walled carbon nanotubes (SWCNTs) as SPME adsorbent for the pre-concentration of environmental contaminants has been investigated in recent years. This work was carried out to investigate the feasibility of SWCNTs as a headspace SPME adsorbent for the determination of bisphenol derivatives in canned food. Potential factors affecting the extraction efficiency, including extraction time, extraction temperature, desorption time, desorption temperature, and salinity were optimized. Calibration curves were linear (r(2)> or = 0.994) over the concentration range from 0.30 to 60 microg kg(-1). For both target analytes, the limit of detection (LOD) at signal-to-noise (S/N) ratio of 3 was 0.10 microg kg(-1). In addition, a comparative study between the SWCNT and a commercial polydimethylsiloxane (PDMS) SPME fibre for the determination of bisphenol derivatives in canned food was conducted. SWCNT fibre showed higher extraction capacity, better thermal stability (over 350 degrees C) and longer life span (over 150 times) than the commercial PDMS fibre. The method was successfully applied to determine BPA in canned food samples which were purchased from local markets. BPA was found in some of the samples within the concentration range from 0.5 to 5.2 microg kg(-1).

  6. Radioimmunoassay of diagoxin with the aid of the solid phase - microtitre plating technique

    International Nuclear Information System (INIS)

    Scheidt, C.

    1982-01-01

    Preliminary results are reported here on the development of a digoxin-radioimmunoassay with an anti-digoxin antibody (goat) in a solid phase technique (mictrotitre plate). The advantages compared to conventional RIAs are: Cross reactions towards digoxin is minimal, both in vitro and in vivo. The calibraton range extends from 0.25 to 8 ng/ml. The radioactive load could be reduced significantly by use of smaller amounts of tracer (0.004 μCi/single determination) and by reduction of waste volume (solid), waste weight (solid) and liquid waste. The DIGOXIN RIA BIOTEST MTP is, in addition, the only digoxin radioimmunoassay where radioactive waste is produced in a sealed form. The test is a simple one and can be carried out without the need for complicated apparatus and techniques. (orig./MG) [de

  7. A new selective chromogenic reagent for the spectrophotometric determination of thallium(I) and (III) and its separation using flotation and the solid-phase extraction on polyurethane foam.

    Science.gov (United States)

    Abou-El-Sherbini, Khaled S; Mostafa, Gamal A E; Hassanien, Mohamed M

    2003-09-01

    A new sensitive chromogenic reagent, 9,10-phenanthaquinone monoethylthiosemicarbazone (PET), has been synthesized and used in the spectrophotometric determination of Tl(III). In HNO3, H2SO4 or H3PO4 acids, PET can react immediately at room temperature with Tl(III) to form a red 2:1 complex with a maximum absorption at 516 nm. The different analytical parameters affecting the extraction and determination processes have been examined. The calibration curve was found to be linear over the range 0.2-10 microg cm(-3) with a molar absorptivity of 2.2 x 10(4) dm3 mol(-1) cm(-1). Sandell's sensitivity was found to be 0.0093 microg cm(-2). No interference from macroamounts of foreign ions was detected, except for Pd(II). However, Pd(II) does not affect the determination process, because its complex with PET has its lambda(max) at 625 nm. The proposed method has been applied to the determination of Tl(I and III) in synthetic and natural samples after separation by flotation (in oleic acid/kerosene) and solid-phase extraction (on polyurethane foam) techniques. The two methods were found to be accurate and not subject to random error, but solid-phase extraction was preferred because it is cheap, simpler and there is no contamination risk coming from flotation reagents.

  8. Fifty years of solid-phase extraction in water analysis--historical development and overview.

    Science.gov (United States)

    Liska, I

    2000-07-14

    The use of an appropriate sample handling technique is a must in an analysis of organic micropollutants in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior to their detection have a long history. Since the first experimental trials using activated carbon filters that were performed 50 years ago, solid-phase extraction (SPE) has become an established sample preparation technique. The initial experimental applications of SPE resulted in widespread use of this technique in current water analysis and also to adoption of SPE into standardized analytical methods. During the decades of its evolution, chromatographers became aware of the advantages of SPE and, despite many innovations that appeared in the last decade, new SPE developments are still expected in the future. A brief overview of 50 years of the history of the use of SPE in organic trace analysis of water is given in presented paper.

  9. Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Berlin, Katja, E-mail: katja.berlin@pdi-berlin.de; Trampert, Achim

    2017-07-15

    Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge{sub 1}Sb{sub 2}Te{sub 4} thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

  10. Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

    International Nuclear Information System (INIS)

    Berlin, Katja; Trampert, Achim

    2017-01-01

    Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge 1 Sb 2 Te 4 thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

  11. Mycoestrogen determination in cow milk: Magnetic solid-phase extraction followed by liquid chromatography and tandem mass spectrometry analysis.

    Science.gov (United States)

    Capriotti, Anna Laura; Cavaliere, Chiara; Foglia, Patrizia; La Barbera, Giorgia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

    2016-12-01

    Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe 3 O 4 , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. NMR relaxation and phase transitions in solid methane and deuterated derivatives

    International Nuclear Information System (INIS)

    Putten, D. van der.

    1984-01-01

    This thesis describes an investigation of properties of solid methane at high pressure (till 10 kbar) with temperatures ranging from 2 until 100 K. The high inverse moment of inertia of the molecule combined with low ordering potentials gives rise to properties for which quantum effects play an important role: e.g. the transition temperature to a partially ordered phase shows an isotope effect of 35% when CH 4 protons are substituted by deuterons. Interpretation of NMR properties of solid methane also show quantum effects. First, a helium cryostat is developed and described and NMR results for CH 4 , CH 2 D 2 and CD 4 are given. The influence of discrete tunnel states on the spin-lattice relaxation is studied theoretically. Application of group theory has simplified the calculations considerably. (G.J.P.)

  13. Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Dugo, Paola [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy)

    2013-04-03

    Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented.

  14. Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

    International Nuclear Information System (INIS)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

    2013-01-01

    Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented

  15. Simultaneous Determination of Parathion, Malathion, Diazinon, and Pirimiphos Methyl in Dried Medicinal Plants Using Solid-Phase Microextraction Fibre Coated with Single-Walled Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Reza Ahmadkhaniha

    2012-01-01

    Full Text Available A reliable and sensitive headspace solid-phase microextraction gas chromatography-mass spectrometry method for simultaneous determination of different organophosphorus pesticides in dried medicinal plant samples is described. The analytes were extracted by single-walled carbon nanotubes as a new solid-phase microextraction adsorbent. The developed method showed good performance. For diazinon and pirimiphos methyl calibration, curves were linear (r2≥0.993 over the concentration ranges from 1.5 to 300 ng g−1, and the limit of detection at signal-to-noise ratio of 3 was 0.3 ng g−1. For parathion and malathion, the linear range and limit of detection were 2.5–300 (r2≥0.991 and 0.5 ng g−1, respectively. In addition, a comparative study between the single-walled carbon nanotubes and a commercial polydimethylsiloxane fibre for the determination of target analytes was carried out. Single-walled carbon nanotubes fibre showed higher extraction capacity, better thermal stability (over 350∘C, and longer lifespan (over 250 times than the commercial polydimethylsiloxane fibre. The developed method was successfully applied to determine target organophosphorus pesticides in real samples.

  16. Solid state dye-sensitized solar cells. Current state of the art. Challenges and opportunities

    Energy Technology Data Exchange (ETDEWEB)

    Lenzmann, F.O.; Olson, C.L.; Goris, M.J.A.A.; Kroon, J.M. [ECN Solar Energy, Petten (Netherlands)

    2008-09-15

    The first generation of dye-sensitized solar cell technology is based on a liquid electrolyte component. Today, this technology is on the verge of commercialization. The step towards the market and real applications is supported by the prospect of low manufacturing costs, good efficiency as well as the expectation that the current stability level of this technology is at least sufficient for applications in mobile electronics. These favorable developments may be reinforced and accelerated even further, if the corrosive liquid electrolyte could be replaced by a non-corrosive solid, since this would ease a number of stringent requirements in the production process. A successful exchange of the liquid electrolyte by a solid-state holeconductor requires to at least maintain, preferably improve, the most relevant technical parameters of the solar cell (efficiency, stability, cost). First pioneering work with solid-state hole conductors was carried out 10 years ago with an initial efficiency level below 1%. Until 2007, the record efficiency could be improved to 5%. This paper gives an overview of the solid-state concept as an early stage approach with good perspectives for the mid-term future (5-10 years)

  17. How fast are the ultra-fast nano-scale solid-liquid phase transitions induced by energetic particles in solids?

    International Nuclear Information System (INIS)

    Lopasso, E.M.; Caro, A.; Caro, M.

    2003-01-01

    We study the thermodynamic forces acting on the evolution of the nanoscale regions excited by collisions of energetic particles into solid targets. We analyze the role of diffusion, thermo-migration, and the liquidus-solidus two-phase field crossing, as the system cools down from the collision-induced melt under different conditions of energy deposition. To determine the relevance of these thermodynamic forces, solute redistribution is evaluated using molecular dynamics simulations of equilibrium Au-Ni solid solutions. At low collision energies, our results show that the quenching of spherical cascades is too fast to allow for solute redistribution according to equilibrium solidification as determined from the equilibrium phase diagram (zone refining effect), and only thermo-migration is observed. At higher energies instead, in the cylindrical symmetry of ion tracks, quenching rate is in a range that shows the combined effects of thermo-migration and solute redistribution that, depending on the material, can reinforce or cancel each other. These results are relevant for the interpretation of the early stage of radiation damage in alloys, and show that the combination of ultra-fast but nano-scale characteristics of these processes can still be described in terms of linear response of the perturbed system

  18. Homogeneous synthesis of cellulose acrylate-g-poly (n-alkyl acrylate) solid-solid phase change materials via free radical polymerization.

    Science.gov (United States)

    Qian, Yong-Qiang; Han, Na; Bo, Yi-Wen; Tan, Lin-Li; Zhang, Long-Fei; Zhang, Xing-Xiang

    2018-08-01

    A novel solid-solid phase change materials, namely, cellulose acrylate-g-poly (n-alkyl acrylate) (CA-g-PAn) (n = 14, 16 and 18) were successfully synthesized by free radical polymerization in N, N-dimethylacetamide (DMAc). The successful grafting was confirmed by fourier transform infrared spectra (FT-IR) and nuclear magnetic resonance (NMR). The properties of the CA-g-PAn copolymers were investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA). The phase change temperatures and the melting enthalpies of CA-g-PAn copolymers are in the range of 10.1-53.2 °C and 15-95 J/g, respectively. It can be adjusted by the contents of poly (n-alkyl acrylate) and the length of alkyl side-chain. The thermal resistant temperatures of CA-g-PA14, 16 and 18 copolymers are 308 °C, 292 °C and 273 °C, respectively. It show that all of grafting materials exhibit good thermal stability and shape stability. Therefore, it is expected to be applied in the cellulose-based thermos-regulating field. Copyright © 2018 Elsevier Ltd. All rights reserved.

  19. Conditioning of radioactive ash residue in a wave of solid-phase exothermal reactions

    International Nuclear Information System (INIS)

    Karlina, O.K.; Varlakova, G.A.; Ozhovan, M.I.; Tivanskij, V.M.; Dmitriev, S.A.

    2001-01-01

    The abilities for utilization of exothermic reaction heat in solid phase for conditioning the ash residue produced as a result of solid radioactive waste burning are analyzed. It is shown that the process of ash residue making monolithic with obtaining the glass-like finish product containing 50-60 mass % of ash residue which meets the requirements for solidified radioactive wastes may be realized without energy supplying from external heat sources. The conditioning is realized in a special crucible furnace-container designed not only for the process conducting but also for subsequent storage or disposal of the finish product [ru

  20. Nanostructured TiO2 microspheres for dye-sensitized solar cells employing a solid state polymer electrolyte

    International Nuclear Information System (INIS)

    Jung, Hun-Gi; Nagarajan, Srinivasan; Kang, Yong Soo; Sun, Yang-Kook

    2013-01-01

    Bimodal mesoporous, anatase TiO 2 microspheres with particle sizes ranging from 0.3 to 2 μm were synthesized using a facile solvothermal method. The photovoltaic performance of TiO 2 microspheres in dye-sensitized solar cells (DSSCs) using a solid state electrolyte was investigated. The solid state electrolyte DSSC device based on the TiO 2 microspheres exhibits an energy conversion efficiency of 4.2%, which is greater than that of commercial P25 TiO 2 (3.6%). The higher photocurrent density was primarily achieved as a result of the greater specific surface area and pore size, which resulted in an increase in the dye uptake of the TiO 2 microspheres and easy transport of solid electrolyte through mesopores. In addition, the greater electron lifetime and superior light scattering ability also enhanced the photovoltaic performance of the TiO 2 microsphere-based, solid state DSSCs