Evaluation of purity with its uncertainty value in high purity lead stick by conventional and electro-gravimetric methods.

PubMed

Singh, Nahar; Singh, Niranjan; Tripathy, S Swarupa; Soni, Daya; Singh, Khem; Gupta, Prabhat K

2013-06-26

A conventional gravimetry and electro-gravimetry study has been carried out for the precise and accurate purity determination of lead (Pb) in high purity lead stick and for preparation of reference standard. Reference materials are standards containing a known amount of an analyte and provide a reference value to determine unknown concentrations or to calibrate analytical instruments. A stock solution of approximate 2 kg has been prepared after dissolving approximate 2 g of Pb stick in 5% ultra pure nitric acid. From the stock solution five replicates of approximate 50 g have been taken for determination of purity by each method. The Pb has been determined as PbSO4 by conventional gravimetry, as PbO2 by electro gravimetry. The percentage purity of the metallic Pb was calculated accordingly from PbSO4 and PbO2. On the basis of experimental observations it has been concluded that by conventional gravimetry and electro-gravimetry the purity of Pb was found to be 99.98 ± 0.24 and 99.97 ± 0.27 g/100 g and on the basis of Pb purity the concentration of reference standard solutions were found to be 1000.88 ± 2.44 and 1000.81 ± 2.68 mg kg-1 respectively with 95% confidence level (k = 2). The uncertainty evaluation has also been carried out in Pb determination following EURACHEM/GUM guidelines. The final analytical results quantifying uncertainty fulfills this requirement and gives a measure of the confidence level of the concerned laboratory. Gravimetry is the most reliable technique in comparison to titremetry and instrumental method and the results of gravimetry are directly traceable to SI unit. Gravimetric analysis, if methods are followed carefully, provides for exceedingly precise analysis. In classical gravimetry the major uncertainties are due to repeatability but in electro-gravimetry several other factors also affect the final results.

Large-scale synthesis of high-purity well-aligned carbon nanotubes using pyrolysis of iron(II) phthalocyanine and acetylene

NASA Astrophysics Data System (ADS)

Liu, B. C.; Lee, T. J.; Lee, S. H.; Park, C. Y.; Lee, C. J.

2003-08-01

Well-aligned carbon nanotubes (CNTs) with high purity have been produced by pyrolysis of iron(II) phthalocyanine and acetylene at 800 °C. The synthesized CNTs have a length of 75 μm and diameters ranging from 20 to 60 nm. The CNTs have a bamboo-like structure and exhibit good crystallinity of graphite sheets. The growth rate of the CNTs was rapidly increased with adding C 2H 2. Our results demonstrate that the proposed growth method is suitable to large-scale synthesis of high-purity well-aligned CNTs on various substrates.

Low cost routes to high purity silicon and derivatives thereof

DOEpatents

Laine, Richard M; Krug, David James; Marchal, Julien Claudius; Mccolm, Andrew Stewart

2013-07-02

The present invention is directed to a method for providing an agricultural waste product having amorphous silica, carbon, and impurities; extracting from the agricultural waste product an amount of the impurities; changing the ratio of carbon to silica; and reducing the silica to a high purity silicon (e.g., to photovoltaic silicon).

Electrolytic production of high purity aluminum using ceramic inert anodes

DOEpatents

Ray, Siba P.; Liu, Xinghua; Weirauch, Douglas A.; DiMilia, Robert A.; Dynys, Joseph M.; Phelps, Frankie E.; LaCamera, Alfred F.

2002-01-01

A method of producing commercial purity aluminum in an electrolytic reduction cell comprising ceramic inert anodes is disclosed. The method produces aluminum having acceptable levels of Fe, Cu and Ni impurities. The ceramic inert anodes used in the process may comprise oxides containing Fe and Ni, as well as other oxides, metals and/or dopants.

Sorting of Semiconducting Single-Walled Carbon Nanotubes in Polar Solvents with an Amphiphilic Conjugated Polymer Provides General Guidelines for Enrichment.

PubMed

Ouyang, Jianying; Ding, Jianfu; Lefebvre, Jacques; Li, Zhao; Guo, Chang; Kell, Arnold J; Malenfant, Patrick R L

2018-02-27

Conjugated polymer extraction (CPE) has been shown to be a highly effective method to isolate high-purity semiconducting single-walled carbon nanotubes (sc-SWCNTs). In both literature reports and industrial manufacturing, this method has enabled enrichment of sc-SWCNTs with high purity (≥99.9%). High selectivity is typically obtained in nonpolar aromatic solvents, yet polar solvents may provide process improvements in terms of yield, purity and efficiency. Using an amphiphilic fluorene-alt-pyridine conjugated copolymer with hydrophilic side chains, we have investigated the enrichment of sc-SWCNTs in polar solvents. Various conditions such as polymer/SWCNT ratio, solvent polarity, solvent dielectric constant as well as polymer solubility and SWCNT dispersibility were explored in order to optimize the purity and yield of the enriched product. Herein, we provide insights on CPE by demonstrating that a conjugated polymer having a hydrophobic backbone and hydrophilic oligo(ethylene oxide) side chains provides near full recovery (95%) of sc-SWCNTs using a multiextraction protocol. High purity is also obtained, and differences in chiral selectivity compared to analogous hydrophobic systems were confirmed by optical absorption and Raman spectroscopy as well as photoluminescence excitation mapping. Taking into consideration the solvent dielectric constant, polarity index as well as polymer solubility and SWCNT dispersibility provides a better understanding of structure-property effects on sc-SWCNT enrichment. The resulting hydrophilic SWCNT dispersions demonstrate long-term colloidal stability, making them suitable for ink formulation and high-performance thin-film transistors fabrication.

Method and apparatus for producing high purity silicon

DOEpatents

Olson, Jerry M.

1984-01-01

A method for producing high purity silicon includes forming a copper silie alloy and positioning the alloy within an enclosure. A filament member is also placed within the enclosure opposite the alloy. The enclosure is then filled with a chemical vapor transport gas adapted for transporting silicon. Finally, both the filament member and the alloy are heated to temperatures sufficient to cause the gas to react with silicon at the alloy surface and deposit the reacted silicon on the filament member. In addition, an apparatus for carrying out this method is also disclosed.

Method and apparatus for producing high purity silicon

DOEpatents

Olson, J.M.

1983-05-27

A method for producing high purity silicon includes forming a copper silicide alloy and positioning the alloy within an enclosure. A filament member is also placed within the enclosure opposite the alloy. The enclosure is then filled with a chemical vapor transport gas adapted for transporting silicon. Finally, both the filament member and the alloy are heated to temperatures sufficient to cause the gas to react with silicon at the alloy surface and deposit the reacted silicon on the filament member. In addition, an apparatus for carrying out this method is also disclosed.

Creating high-purity angular-momentum-state Rydberg atoms by a pair of unipolar laser pulses

NASA Astrophysics Data System (ADS)

Xin, PeiPei; Cheng, Hong; Zhang, ShanShan; Wang, HanMu; Xu, ZiShan; Liu, HongPing

2018-04-01

We propose a method of producing high-purity angular-momentum-state Rydberg atoms by a pair of unipolar laser pulses. The first positive-polarity optical half-cycle pulse is used to prepare an excited-state wave packet while the second one is less intense, but with opposite polarity and time delayed, and is employed to drag back the escaping free electron and clip the shape of the bound Rydberg wave packet, selectively increasing or decreasing a fraction of the angular-momentum components. An intelligent choice of laser parameters such as phase and amplitude helps us to control the orbital-angular-momentum composition of an electron wave packet with more facility; thus, a specified angular-momentum state with high purity can be achieved. This scheme of producing high-purity angular-momentum-state Rydberg atoms has significant application in quantum-information processing.

Method of Separating Oxygen From Spacecraft Cabin Air to Enable Extravehicular Activities

NASA Technical Reports Server (NTRS)

Graf, John C.

2013-01-01

Extravehicular activities (EVAs) require high-pressure, high-purity oxygen. Shuttle EVAs use oxygen that is stored and transported as a cryogenic fluid. EVAs on the International Space Station (ISS) presently use the Shuttle cryo O2, which is transported to the ISS using a transfer hose. The fluid is compressed to elevated pressures and stored as a high-pressure gas. With the retirement of the shuttle, NASA has been searching for ways to deliver oxygen to fill the highpressure oxygen tanks on the ISS. A method was developed using low-pressure oxygen generated onboard the ISS and released into ISS cabin air, filtering the oxygen from ISS cabin air using a pressure swing absorber to generate a low-pressure (high-purity) oxygen stream, compressing the oxygen with a mechanical compressor, and transferring the high-pressure, high-purity oxygen to ISS storage tanks. The pressure swing absorber (PSA) can be either a two-stage device, or a single-stage device, depending on the type of sorbent used. The key is to produce a stream with oxygen purity greater than 99.5 percent. The separator can be a PSA device, or a VPSA device (that uses both vacuum and pressure for the gas separation). The compressor is a multi-stage mechanical compressor. If the gas flow rates are on the order of 5 to 10 lb (.2.3 to 4.6 kg) per day, the compressor can be relatively small [3 16 16 in. (.8 41 41 cm)]. Any spacecraft system, or other remote location that has a supply of lowpressure oxygen, a method of separating oxygen from cabin air, and a method of compressing the enriched oxygen stream, has the possibility of having a regenerable supply of highpressure, high-purity oxygen that is compact, simple, and safe. If cabin air is modified so there is very little argon, the separator can be smaller, simpler, and use less power.

Development of high-throughput and high sensitivity capillary gel electrophoresis platform method for Western, Eastern, and Venezuelan equine encephalitis (WEVEE) virus like particles (VLPs) purity determination and characterization.

PubMed

Gollapudi, Deepika; Wycuff, Diane L; Schwartz, Richard M; Cooper, Jonathan W; Cheng, K C

2017-10-01

In this paper, we describe development of a high-throughput, highly sensitive method based on Lab Chip CGE-SDS platform for purity determination and characterization of virus-like particle (VLP) vaccines. A capillary gel electrophoresis approach requiring about 41 s per sample for analysis and demonstrating sensitivity to protein initial concentrations as low as 20 μg/mL, this method has been used previously to evaluate monoclonal antibodies, but this application for lot release assay of VLPs using this platform is unique. The method was qualified and shown to be accurate for the quantitation of VLP purity. Assay repeatability was confirmed to be less than 2% relative standard deviation of the mean (% RSD) with interday precision less than 2% RSD. The assay can evaluate purified VLPs in a concentration range of 20-249 μg/mL for VEE and 20-250 μg/mL for EEE and WEE VLPs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High purity silica reflective heat shield development

NASA Technical Reports Server (NTRS)

Nachtscheim, P. R.; Blome, J. C.

1976-01-01

A hyperpure vitreous silica material is being developed for use as a reflective and ablative heat shield for planetary entry. Various purity grades and forms of raw materials were evaluated along with various processing methods. Slip casting of high purity grain was selected as the best processing method, resulting in a highly reflective material in the wavelength bands of interest (the visible and ultraviolet regions). The selected material was characterized with respect to optical, mechanical and physical properties using a limited number of specimens. The process has been scaled up to produce a one-half scale heat shield (18 in. dia.) (45.72 cm) for a Jupiter entry vehicle. This work is now being extended to improve the structural safety factor of the heat shield by making hyperpure silica material tougher through the addition of silica fibers.

Method for preparing high purity vanadium

DOEpatents

Schmidt, Frederick; Carlson, O. Norman

1986-09-09

A method for preparing high purity vanadium having a low silicon content has been developed. Vanadium pentoxide is reduced with a stoichiometric, or slightly deficient amount of aluminum to produce a vanadium-aluminum alloy containing an excess of oxygen. Silicon is removed by electron-beam melting the alloy under oxidizing conditions to promote the formation of SiO which is volatile at elevated temperatures. Excess oxygen is removed by heating the alloy in the presence of calcium metal to form calcium oxide.

Method for preparing high purity vanadium

DOEpatents

Schmidt, F.; Carlson, O.N.

1984-05-16

A method for preparing high purity vanadium having a low silicon content has been developed. Vanadium pentoxide is reduced with a stoichiometric, or slightly deficient amount of aluminum to produce a vanadium-aluminum alloy containing an excess of oxygen. Silicon is removed by electron-beam melting the alloy under oxidizing conditions to promote the formation of SiO which is volatile at elevated temperatures. Excess oxygen is removed by heating the alloy in the presence of calcium metal to form calcium oxide.

Synthesis of Metal Phthalocyanine Sheet Polymers

NASA Technical Reports Server (NTRS)

Achar, B. N.; Fohlen, G. M.; Parker, J. A.

1986-01-01

New method for synthesizing metal phthalocyanine tetracarboxylic acids (MPTCA's) yields high purity end product. In addition, high-purity metal phthalocyanine sheet polymers synthesized from compounds. Monomer formed into sheet polymer by heating. Units of polymer linked in manner similar to phenyl-group linkages in biphenyl: Conjugation extends throughout macromolecule, thereby increasing delocalization of TT-electrons. Increases conductivity and thermal stability of polymer.

Isolation of high purity americium metal via distillation

NASA Astrophysics Data System (ADS)

Squires, Leah N.; King, James A.; Fielding, Randall S.; Lessing, Paul

2018-03-01

Pure americium metal is a crucial component for the fabrication of transmutation fuels. Unfortunately, americium in pure metal form is not available; however, a number of mixed metals and mixed oxides that include americium are available. In this manuscript a method is described to obtain high purity americium metal from a mixture of americium and neptunium metals with lead impurity via distillation.

Design, Fabrication, Characterization and Modeling of Integrated Functional Materials

DTIC Science & Technology

2014-10-01

oxide ( AAO ) membranes were fabricated from high purity aluminum foil (99.999%) by electrochemical route using a controlled two-step anodization ...deposition of Fe and Co in anodized alumina templates. We used commercially prepared AAO templates which had pore diameters of 100 nm (300 nm), an...a thermal decomposition method. The final product was suspended in high-purity hexane to create a ferrofluid. Custom highly ordered anodic aluminum

Establishing comparability and compatibility in the purity assessment of high purity zinc as demonstrated by the CCQM-P149 intercomparison

NASA Astrophysics Data System (ADS)

Vogl, Jochen; Kipphardt, Heinrich; Richter, Silke; Bremser, Wolfram; del Rocío Arvizu Torres, María; Manzano, Judith Velina Lara; Buzoianu, Mirella; Hill, Sarah; Petrov, Panayot; Goenaga-Infante, Heidi; Sargent, Mike; Fisicaro, Paola; Labarraque, Guillaume; Zhou, Tao; Turk, Gregory C.; Winchester, Michael; Miura, Tsutomu; Methven, Brad; Sturgeon, Ralph; Jährling, Reinhard; Rienitz, Olaf; Mariassy, Michal; Hankova, Zuzana; Sobina, Egor; Ivanovich Krylov, Anatoly; Anatolievich Kustikov, Yuri; Vladimirovich Smirnov, Vadim

2018-04-01

For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute’s applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100%, or 1 kg kg-1. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011%. The calculated reference value, w(Zn)  =  0.999 873 kg kg-1, was assigned an asymmetric combined uncertainty of  +0.000 025 kg kg-1 and  -0.000 028 kg kg-1. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition/dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity of less pure elements and/or for those elements suffering difficulties with the decomposition process.

Recycling of high purity selenium from CIGS solar cell waste materials

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

Gustafsson, Anna M.K., E-mail: anna.gustafsson@chalmers.se; Foreman, Mark R.StJ.; Ekberg, Christian

Highlights: • A new method for recycling of selenium from CIGS solar cell materials is presented. • Separation of selenium as selenium dioxide after heating in oxygen atmosphere. • Complete selenium separation after oxidation of <63 μm particles at 800 °C for 1 h. • After reduction of selenium dioxide the selenium purity was higher than 99.999 wt%. - Abstract: Copper indium gallium diselenide (CIGS) is a promising material in thin film solar cell production. To make CIGS solar cells more competitive, both economically and environmentally, in comparison to other energy sources, methods for recycling are needed. In addition tomore » the generally high price of the material, significant amounts of the metals are lost in the manufacturing process. The feasibility of recycling selenium from CIGS through oxidation at elevated temperatures was therefore examined. During oxidation gaseous selenium dioxide was formed and could be separated from the other elements, which remained in solid state. Upon cooling, the selenium dioxide sublimes and can be collected as crystals. After oxidation for 1 h at 800 °C all of the selenium was separated from the CIGS material. Two different reduction methods for reduction of the selenium dioxide to selenium were tested. In the first reduction method an organic molecule was used as the reducing agent in a Riley reaction. In the second reduction method sulphur dioxide gas was used. Both methods resulted in high purity selenium. This proves that the studied selenium separation method could be the first step in a recycling process aimed at the complete separation and recovery of high purity elements from CIGS.« less

Recent Progress in Obtaining Semiconducting Single-Walled Carbon Nanotubes for Transistor Applications.

PubMed

Islam, Ahmad E; Rogers, John A; Alam, Muhammad A

2015-12-22

High purity semiconducting single-walled carbon nanotubes (s-SWCNTs) with a narrow diameter distribution are required for high-performance transistors. Achieving this goal is extremely challenging because the as-grown material contains mixtures of s-SWCNTs and metallic- (m-) SWCNTs with wide diameter distributions, typically inadequate for integrated circuits. Since 2000, numerous ex situ methods have been proposed to improve the purity of the s-SWCNTs. The majority of these techniques fail to maintain the quality and integrity of the s-SWCNTs with a few notable exceptions. Here, the progress in realizing high purity s-SWCNTs in as-grown and post-processed materials is highlighted. A comparison of transistor parameters (such as on/off ratio and field-effect mobility) obtained from test structures establishes the effectiveness of various methods and suggests opportunities for future improvements. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Research about Preparation of High Purity Hexachlorodisilane

NASA Astrophysics Data System (ADS)

Wan, Ye; Zhao, Xiong; Yan, Dazhou; Zhao, Yu; Guo, Shuhu; Wang, Lei; Yang, Dian

2017-12-01

This article demonstrated a technology for producing high purity hexachlorodisilane what is one raw material of Semiconductor industry, which using the method of combination adsorption with rectification, whose material was from polysilicon residues of polysilicon company. This technology could remove most high boiling points chloro-silicane impurities and metal impurities effectively. The purity of Si2Cl6 produced by this technology can be up to 99.9%, the content of metal impurities can be low at 4ppb, which can meet the requirement of industy using completely. The technology extends the routes of Si2Cl6 in localization, having the advantages of simple process, continuous operation, and large capacity and so on.

Capillary gel electrophoresis for the quantification and purity determination of recombinant proteins in inclusion bodies.

PubMed

Espinosa-de la Garza, Carlos E; Perdomo-Abúndez, Francisco C; Campos-García, Víctor R; Pérez, Néstor O; Flores-Ortiz, Luis F; Medina-Rivero, Emilio

2013-09-01

In this work, a high-resolution CGE method for quantification and purity determination of recombinant proteins was developed, involving a single-component inclusion bodies (IBs) solubilization solution. Different recombinant proteins expressed as IBs were used to show method capabilities, using recombinant interferon-β 1b as the model protein for method validation. Method linearity was verified in the range from 0.05 to 0.40 mg/mL and a determination coefficient (r(2) ) of 0.99 was obtained. The LOQs and LODs were 0.018 and 0.006 mg/mL, respectively. RSD for protein content repeatability test was 2.29%. In addition, RSD for protein purity repeatability test was 4.24%. Method accuracy was higher than 90%. Specificity was confirmed, as the method was able to separate recombinant interferon-β 1b monomer from other aggregates and impurities. Sample content and purity was demonstrated to be stable for up to 48 h. Overall, this method is suitable for the analysis of recombinant proteins in IBs according to the attributes established on the International Conference for Harmonization guidelines. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigation of the plastic fracture of high strength steels

NASA Technical Reports Server (NTRS)

Cox, T. B.; Low, J. R., Jr.

1972-01-01

This investigation deals in detail with the three recognized stages of plastic fracture in high strength steels, namely, void initiation, void growth, and void coalescence. The particular steels under investigation include plates from both commercial purity and high purity heats of AISI 4340 and 18 Ni, 200 grade maraging steels. A scanning electron microscope equipped with an X-ray energy dispersive analyzer, together with observations made using light microscopy, revealed methods of improving the resistance of high strength steels to plastic fracture.

Facile synthesis of upconversion nanoparticles with high purity using lanthanide oleate compounds

NASA Astrophysics Data System (ADS)

Kang, Ning; Ai, Chao-Chao; Zhou, Ya-Ming; Wang, Zuo; Ren, Lei

2018-02-01

A novel strategy for preparing highly pure NaYF4-based upconversion nanoparticles (UCNPs) was developed using lanthanide oleate compounds [Ln(OA)3] as the precursor, denoted as the Ln-OA preparation method. Compared to the conventional solvothermal method for synthesizing UCNPs using lanthanide chloride compounds (LnCl3) as the precursor (denoted as the Ln-Cl method), the Ln-OA strategy exhibited the merits of high purity, reduced purification process and a uniform size in preparing core and core-shell UCNPs excited by a 980 or 808 nm near infrared (NIR) laser. This work sheds new insight on the preparation of UCNPs and promotes their application in biomedical fields.

Room temperature aluminum antimonide radiation detector and methods thereof

DOEpatents

Lordi, Vincenzo; Wu, Kuang Jen J.; Aberg, Daniel; Erhart, Paul; Coombs, III, Arthur W; Sturm, Benjamin W

2015-03-03

In one embodiment, a method for producing a high-purity single crystal of aluminum antimonide (AlSb) includes providing a growing environment with which to grow a crystal, growing a single crystal of AlSb in the growing environment which comprises hydrogen (H.sub.2) gas to reduce oxide formation and subsequent incorporation of oxygen impurities in the crystal, and adding a controlled amount of at least one impurity to the growing environment to effectively incorporate at least one dopant into the crystal. In another embodiment, a high energy radiation detector includes a single high-purity crystal of AlSb, a supporting structure for the crystal, and logic for interpreting signals obtained from the crystal which is operable as a radiation detector at a temperature of about 25.degree. C. In one embodiment, a high-purity single crystal of AlSb includes AlSb and at least one dopant selected from a group consisting of selenium (Se), tellurium (Te), and tin (Sn).

Japan Report, Science and Technology.

DTIC Science & Technology

1987-03-18

electromelting and desiliconizing method and the alkali melting method are conventional methods to manufacture zirconia powder . The former method is low...cost, but does not produce high purity zirconia powder . In contrast, the latter method produces high-strength and ultrafine zirconia powder , but is

Structural, microstructural and magnetic evolution in cryo milled carbon doped MnAl.

PubMed

Fang, Hailiang; Cedervall, Johan; Hedlund, Daniel; Shafeie, Samrand; Deledda, Stefano; Olsson, Fredrik; von Fieandt, Linus; Bednarcik, Jozef; Svedlindh, Peter; Gunnarsson, Klas; Sahlberg, Martin

2018-02-06

The low cost, rare earth free τ-phase of MnAl has high potential to partially replace bonded Nd 2 Fe 14 B rare earth permanent magnets. However, the τ-phase is metastable and it is experimentally difficult to obtain powders suitable for the permanent magnet alignment process, which requires the fine powders to have an appropriate microstructure and high τ-phase purity. In this work, a new method to make high purity τ-phase fine powders is presented. A high purity τ-phase Mn 0.55 Al 0.45 C 0.02 alloy was synthesized by the drop synthesis method. The drop synthesized material was subjected to cryo milling and  followed by a flash heating process. The crystal structure and microstructure of the drop synthesized, cryo milled and flash heated samples were studied by X-ray in situ powder diffraction, scanning electron microscopy, X-ray energy dispersive spectroscopy and electron backscatter diffraction. Magnetic properties and magnetic structure of the drop synthesized, cryo milled, flash heated  samples were characterized by magnetometry and neutron powder diffraction, respectively. The results reveal that the 2 and 4 hours cryo milled and flash heated samples both exhibit high τ-phase purity and micron-sized round particle shapes. Moreover, the flash heated samples display high saturation magnetization as well as increased coercivity.

Continuous separation of microparticles in a microfluidic channel via the elasto-inertial effect of non-Newtonian fluid.

PubMed

Nam, Jeonghun; Lim, Hyunjung; Kim, Dookon; Jung, Hyunwook; Shin, Sehyun

2012-04-07

Pure separation and sorting of microparticles from complex fluids are essential for biochemical analyses and clinical diagnostics. However, conventional techniques require highly complex and expensive labeling processes for high purity separation. In this study, we present a simple and label-free method for separating microparticles with high purity using the elasto-inertial characteristic of a non-Newtonian fluid in microchannel flow. At the inlet, particle-containing sample flow was pushed toward the side walls by introducing sheath fluid from the center inlet. Particles of 1 μm and 5 μm in diameter, which were suspended in viscoelastic fluid, were successfully separated in the outlet channels: larger particles were notably focused on the centerline of the channel at the outlet, while smaller particles continued flowing along the side walls with minimal lateral migration towards the centerline. The same technique was further applied to separate platelets from diluted whole blood. Through cytometric analysis, we obtained a purity of collected platelets of close to 99.9%. Conclusively, our microparticle separation technique using elasto-inertial forces in non-Newtonian fluid is an effective method for separating and collecting microparticles on the basis of size differences with high purity. This journal is © The Royal Society of Chemistry 2012

On the introduction of a measurement standard for high-purity germanium crystals to be used in radiation detectors

NASA Astrophysics Data System (ADS)

Darken, L.

1994-02-01

The IEEE and ANSI have recently approved "Standard Test Procedures for High-Purity Germanium Crystals for Radiation Detectors" proposed by the IEEE/NPSS/Nuclear Instruments and Detectors Committee. The standard addresses three aspects of the characterisation of high-purity germanium: (i) the determination by the van der Pauw method of the net carrier concentration and type; (ii) the measurement by capacitance transient techniques of the concentration of trapping levels; (iii) the description of the crystallographic properties revealed by preferential etching. In addition to describing the contents of this standard, the purpose of this work is also to place the issues faced in the context of professional consensus: points of agreement, points of disagreement, and subjects poorly understood.

Impurity rejection in the crystallization of ABT-510 as a method to establish starting material specifications.

PubMed

Tolle, John C; Becker, Calvin L; Califano, Jean C; Chang, Jane L; Gernhardt, Kevin; Napier, James J; Wittenberger, Steven J; Yuan, Judy

2009-01-01

Understanding impurity rejection in a drug substance crystallization process is valuable for establishing purity specifications for the starting materials used in the process. Impurity rejection has been determined for all known ABT-510 impurities and for many of the reasonable & conceivable impurities. Based on this study, a very high purity specification (e.g., > 99.7%) can be set for ABT-510 with a high level of confidence.

Production of high purity radiothallium

DOEpatents

Lebowitz, Elliot; Greene, Margaret W.

1976-11-23

The method of producing high purity thallium-201 for use as a myocardial scanning agent comprising the steps of irradiating a thallium target with protons to give the reaction .sup.203 Tl(p,3n) .sup.201.sub.Pb, separating in ion exchange columns the lead from the thallium isotopes, permitting the lead to decay, and then purifying the thallium solution and converting the thallium present to thallous form in which it can be used.

High-pressure-assisted synthesis of high-volume ZnGeP2 polycrystalline

NASA Astrophysics Data System (ADS)

Huang, Changbao; Wu, Haixin; Xiao, Ruichun; Chen, Shijing; Ma, Jiaren

2018-06-01

The pnictide and chalcogenide semiconductors are promising materials for the applications in the field of photoelectric. High-purity and high-volume polycrystalline required in the real-world applications is hard to be synthesized due to the high vapor pressure of phosphorus and sulfur components at high temperature. A new high-pressure-resisted method was used to investigate the synthesis of the nonlinear-optical semiconductor ZnGeP2. The high-purity ZnGeP2 polycrystalline material of approximately 500 g was synthesized in one run, which enables the preparation of nominally stoichiometric material. Since increasing internal pressure resistance of quartz crucible and reducing the reaction space, the high-pressure-resisted method can be used to rapidly synthesize other pnictide and chalcogenide semiconductors and control the components ratio.

Method for the production of high-purity triaminotrinitrobenzene

DOEpatents

Benziger, Theodore M.

1977-01-01

Triaminotrinitrobenzene is readily formed by the nitration of 1,3,5-trichlorobenzene to 1,3,5-trichloro-2,4,6-trinitrobenzene followed by amination to triaminotrinitrobenzene. The purity of the triaminotrinitrobenzene is significantly improved if, during the amination step, sufficient water is present that the byproduct ammonium chloride formed during the amination is rendered at least semideliquescent.

Preparation of uniform nanoparticles of ultra-high purity metal oxides, mixed metal oxides, metals, and metal alloys

DOEpatents

Woodfield, Brian F.; Liu, Shengfeng; Boerio-Goates, Juliana; Liu, Qingyuan; Smith, Stacey Janel

2012-07-03

In preferred embodiments, metal nanoparticles, mixed-metal (alloy) nanoparticles, metal oxide nanoparticles and mixed-metal oxide nanoparticles are provided. According to embodiments, the nanoparticles may possess narrow size distributions and high purities. In certain preferred embodiments, methods of preparing metal nanoparticles, mixed-metal nanoparticles, metal oxide nanoparticles and mixed-metal nanoparticles are provided. These methods may provide tight control of particle size, size distribution, and oxidation state. Other preferred embodiments relate to a precursor material that may be used to form nanoparticles. In addition, products prepared from such nanoparticles are disclosed.

Development of high purity large forgings for nuclear power plants

NASA Astrophysics Data System (ADS)

Tanaka, Yasuhiko; Sato, Ikuo

2011-10-01

The recent increase in the size of energy plants has been supported by the development of manufacturing technology for high purity large forgings for the key components of the plant. To assure the reliability and performance of the large forgings, refining technology to make high purity steels, casting technology for gigantic ingots, forging technology to homogenize the material and consolidate porosity are essential, together with the required heat treatment and machining technologies. To meet these needs, the double degassing method to reduce impurities, multi-pouring methods to cast the gigantic ingots, vacuum carbon deoxidization, the warm forging process and related technologies have been developed and further improved. Furthermore, melting facilities including vacuum induction melting and electro slag re-melting furnaces have been installed. By using these technologies and equipment, large forgings have been manufactured and shipped to customers. These technologies have also been applied to the manufacture of austenitic steel vessel components of the fast breeder reactors and components for fusion experiments.

Certification of caffeine reference material purity by ultraviolet/visible spectrophotometry and high-performance liquid chromatography with diode-array detection as two independent analytical methods.

PubMed

Shehata, A B; Rizk, M S; Rend, E A

2016-10-01

Caffeine reference material certified for purity is produced worldwide, but no research work on the details of the certification process has been published in the literature. In this paper, we report the scientific details of the preparation and certification of pure caffeine reference materials. Caffeine was prepared by extraction from roasted and ground coffee by dichloromethane after heating in deionized water mixed with magnesium oxide. The extract was purified, dried, and bottled in dark glass vials. Stratified random selection was applied to select a number of vials for homogeneity and stability studies, which revealed that the prepared reference material is homogeneous and sufficiently stable. Quantification of caffeine purity % was carried out using a calibrated UV/visible spectrophotometer and a calibrated high-performance liquid chromatography with diode-array detection method. The results obtained from both methods were combined to drive the certified value and its associated uncertainty. The certified value of the reference material purity was found to be 99.86% and its associated uncertainty was ±0.65%, which makes the candidate reference material a very useful calibrant in food and drug chemical analysis. Copyright © 2016. Published by Elsevier B.V.

Development and Validation of a High-Pressure Liquid Chromatography Method for the Determination of Chemical Purity and Radiochemical Purity of a [68Ga]-Labeled Glu-Urea-Lys(Ahx)-HBED-CC (Positron Emission Tomography) Tracer

PubMed Central

2017-01-01

Background: Prostate-specific membrane antigen (PSMA) has gained high attention as a useful biomarker in the imaging evaluation of prostate cancer with positron emission tomography (PET) during recent years. [68Ga]-labeled Glu-urea-Lys(Ahx)-HBED-CC ([68Ga]-PSMA-HBED-CC) is a novel PSMA inhibitor radiotracer which has demonstrated its suitability in detecting prostate cancer. Preparation conditions may influence the quality and in vivo behavior of this tracer, and no standard procedure for the quality control (QC) is available. The aim of this study was to develop a new rapid and simple high-pressure liquid chromatography method of analysis for the routine QCs of [68Ga]-PSMA-HBED-CC to guarantee the high quality of the radiopharmaceutical product before release. Methods: A stepwise approach was used based on the quality by design concept of the International Conference of Harmonisation Q2 (R1) and Q8 (Pharmaceutical Development) guidelines in accordance with the regulations and requirements of European Association of Nuclear Medicine, Society of Nuclear Medicine, International Atomic Energy Agency, World Health Organization, and Italian Association of Nuclear Medicine and Molecular Imaging. The developed analytical test method was validated because a specific monograph in the pharmacopoeia is not available for [68Ga]-PSMA-HBED-CC. Results: The purity and quality of the radiopharmaceutical obtained according to the proposed method resulted high enough to safely administrate it to patients. An excellent linearity was found between 0.8 and 5 μg/mL, with a detection limit of 0.2 μg/mL. Assay imprecision (% CV) was <2%. Conclusions: The developed method to assess the radiochemical and chemical purity of [68Ga]-PSMA-HBED-CC is rapid, accurate, and reproducible, allowing routinely the use of this PET tracer as a diagnostic tool for imaging prostate cancer and also assuring patient safety. PMID:29520394

Method of high purity silane preparation

DOEpatents

Tsuo, Y. Simon; Belov, Eugene P.; Gerlivanov, Vadim G.; Zadde, Vitali V.; Kleschevnikova, Solomonida I.; Korneev, Nikolai N.; Lebedev, Eugene N.; Pinov, Akhsarbek B.; Ryabenko, Eugene A.; Strebkov, Dmitry S.; Chernyshev, Eugene A.

2000-01-01

A process for the preparation of high purity silane, suitable for forming thin layer silicon structures in various semiconductor devices and high purity poly- and single crystal silicon for a variety of applications, is provided. Synthesis of high-purity silane starts with a temperature assisted reaction of metallurgical silicon with alcohol in the presence of a catalyst. Alcoxysilanes formed in the silicon-alcohol reaction are separated from other products and purified. Simultaneous reduction and oxidation of alcoxysilanes produces gaseous silane and liquid secondary products, including, active part of a catalyst, tetra-alcoxysilanes, and impurity compounds having silicon-hydrogen bonds. Silane is purified by an impurity adsorption technique. Unreacted alcohol is extracted and returned to the reaction with silicon. Concentrated mixture of alcoxysilanes undergoes simultaneous oxidation and reduction in the presence of a catalyst at the temperature -20.degree. C. to +40.degree. C. during 1 to 50 hours. Tetra-alcoxysilane extracted from liquid products of simultaneous oxidation and reduction reaction is directed to a complete hydrolysis. Complete hydrolysis of tetra-alcoxysilane results in formation of industrial silica sol and alcohol. Alcohol is dehydrated by tetra-alcoxysilane and returned to the reaction with silicon.

Color of Cultures of Staphylococcus epidermidis Determined by Spectral Reflectance Colorimetry

PubMed Central

Brown, Richard W.

1966-01-01

Brown, Richard W. (National Animal Disease Laboratory, Ames, Iowa). Color of cultures of Staphylococcus epidermidis determined by spectral reflectance colorimetry. J. Bacteriol. 91:911–918. 1966.—A colorimeter with a reflectance attachment was used to study pigment production by Staphylococcus epidermidis strains grown on a medium containing Trypticase Soy Agar (BBL) and cream. The color of each culture was first characterized by reflectance colorimetry for dominant wavelength, purity, and luminous reflectance (Y) and was then classified visually into 1 of 10 color grades. There was not complete agreement in grading colors by the two methods, inasmuch as cultures that were considered more pigmented in relation to other cultures by the reflectance method were sometimes graded visually as less pigmented, and vice versa. Nevertheless, when the cultures were visually graded as being more pigmented, there was a concomitant increase in the average values of dominant wavelength and purity with a decrease in Y for the cultures in each higher grade. Thus, the nonpigmented cultures had the lowest dominant wavelength and purity values but the highest Y (brightness) values, whereas the most pigmented cultures had the highest dominant wavelength and purity values, but the lowest Y values. These results indicated that the cultures did not produce pigments of different hues (greenish-yellow, yellow, yellowish-orange) each with high, medium, and low degrees of purity and brightness. The value (1 − z), where the chromaticity coordinate z = Z/(X + Y + Z), was found to be proportional to the purity value. An inverse relationship between the tristimulus Z and purity values was also demonstrated. All cultures tested by the reflectance method were also classified according to the type of spectral absorption curve obtained with pigments extracted from the cultures with methanol. A comparison of these methods indicated that determining the type of spectral absorption curve would be better for differentiating strains of S. epidermidis, whereas the use of the reflectance method would be better for determining differences of pigment production within strains. PMID:5932106

High-purity Cu nanocrystal synthesis by a dynamic decomposition method.

PubMed

Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

2014-12-01

Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

High-purity Cu nanocrystal synthesis by a dynamic decomposition method

NASA Astrophysics Data System (ADS)

Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

2014-12-01

Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

Primary culture of human Schwann and schwannoma cells: improved and simplified protocol.

PubMed

Dilwali, Sonam; Patel, Pratik B; Roberts, Daniel S; Basinsky, Gina M; Harris, Gordon J; Emerick, Kevin S; Stankovic, Konstantina M

2014-09-01

Primary culture of human Schwann cells (SCs) and vestibular schwannoma (VS) cells are invaluable tools to investigate SC physiology and VS pathobiology, and to devise effective pharmacotherapies against VS, which are sorely needed. However, existing culture protocols, in aiming to create robust, pure cultures, employ methods that can lead to loss of biological characteristics of the original cells, potentially resulting in misleading biological findings. We have developed a minimally manipulative method to culture primary human SC and VS cells, without the use of selective mitogens, toxins, or time-consuming and potentially transformative laboratory techniques. Schwann cell purity was quantified longitudinally using S100 staining in SC cultures derived from the great auricular nerve and VS cultures followed for 7 and 12 weeks, respectively. SC cultures retained approximately ≥85% purity for 2 weeks. VS cultures retained approximately ≥80% purity for the majority of the span of 12 weeks, with maximal purity of 87% at 2 weeks. The VS cultures showed high level of biological similarity (68% on average) to their respective parent tumors, as assessed using a protein array featuring 41 growth factors and receptors. Apoptosis rate in vitro negatively correlated with tumor volume. Our results, obtained using a faster, simplified culturing method than previously utilized, indicate that highly pure, primary human SC and VS cultures can be established with minimal manipulation, reaching maximal purity at 2 weeks of culture. The VS cultures recapitulate the parent tumors' biology to a great degree, making them relevant models to investigate VS pathobiology. Copyright © 2014 Elsevier B.V. All rights reserved.

Primary culture of human Schwann and schwannoma cells: Improved and simplified protocol

PubMed Central

Dilwali, Sonam; Patel, Pratik B.; Roberts, Daniel S.; Basinsky, Gina M.; Harris, Gordon J.; Emerick, Kevin; Stankovic, Konstantina M.

2014-01-01

Primary culture of human Schwann cells (SCs) and vestibular schwannoma (VS) cells are invaluable tools to investigate SC physiology and VS pathobiology, and to devise effective pharmacotherapies against VS, which are sorely needed. However, existing culture protocols, in aiming to create robust, pure cultures, employ methods that can lead to loss of biological characteristics of the original cells, potentially resulting in misleading biological findings. We have developed a minimally manipulative method to culture primary human SC and VS cells, without the use of selective mitogens, toxins, or time-consuming and potentially transformative laboratory techniques. Schwann cell purity was quantified longitudinally using S100 staining in SC cultures derived from the great auricular nerve and VS cultures followed for 7 and 12 weeks, respectively. SC cultures retained approximately ≥85% purity for 2 weeks. VS cultures retained approximately ≥80% purity for the majority of the span of 12 weeks, with maximal purity of 87% at 2 weeks. The VS cultures showed high level of biological similarity (68% on average) to their respective parent tumors, as assessed using a protein array featuring 41 growth factors and receptors. Apoptosis rate in vitro negatively correlated with tumor volume. Our results, obtained using a faster, simplified culturing method than previously utilized, indicate that highly pure, primary human SC and VS cultures can be established with minimal manipulation, reaching maximal purity at 2 weeks of culture. The VS cultures recapitulate the parent tumors' biology to a great degree, making them relevant models to investigate VS pathobiology. PMID:24910344

A comparative evaluation of six principal IgY antibody extraction methods.

PubMed

Ren, Hao; Yang, Wenjing; Thirumalai, Diraviyam; Zhang, Xiaoying; Schade, Rüdiger

2016-03-01

Egg yolk has been considered a promising source of antibodies. Our study was designed to compare six principal IgY extraction methods (water dilution, polyethylene glycol [PEG] precipitation, caprylic acid extraction, chloroform extraction, phenol extraction, and carrageenan extraction), and to assess their relative extraction efficiencies and the purity of the resulting antibodies. The results showed that the organic solvents (chloroform or phenol) minimised the lipid ratio in the egg yolk. The water dilution, PEG precipitation and caprylic acid extraction methods resulted in high yields, and antibodies purified with PEG and carrageenan exhibited high purity. Our results indicate that phenol extraction would be more suitable for preparing high concentrations of IgY for non-therapeutic usage, while the water dilution and carrageenan extraction methods would be more appropriate for use in the preparation of IgY for oral administration. 2016 FRAME.

Polycrystalline nanowires of gadolinium-doped ceria via random alignment mediated by supercritical carbon dioxide

PubMed Central

Kim, Sang Woo; Ahn, Jae-Pyoung

2013-01-01

This study proposes a seed/template-free method that affords high-purity semiconducting nanowires from nanoclusters, which act as basic building blocks for nanomaterials, under supercritical CO2 fluid. Polycrystalline nanowires of Gd-doped ceria (Gd-CeO2) were formed by CO2-mediated non-oriented attachment of the nanoclusters resulting from the dissociation of single-crystalline aggregates. The unique formation mechanism underlying this morphological transition may be exploited for the facile growth of high-purity polycrystalline nanowires. PMID:23572061

Surface preparation for high purity alumina ceramics enabling direct brazing in hydrogen atmospheres

DOEpatents

Cadden, Charles H.; Yang, Nancy Yuan Chi; Hosking, Floyd M.

2001-01-01

The present invention relates to a method for preparing the surface of a high purity alumina ceramic or sapphire specimen that enables direct brazing in a hydrogen atmosphere using an active braze alloy. The present invention also relates to a method for directly brazing a high purity alumina ceramic or sapphire specimen to a ceramic or metal member using this method of surface preparation, and to articles produced by this brazing method. The presence of silicon, in the form of a SiO.sub.2 -containing surface layer, can more than double the tensile bond strength in alumina ceramic joints brazed in a hydrogen atmosphere using an active Au-16Ni-0.75 Mo-1.75V filler metal. A thin silicon coating applied by PVD processing can, after air firing, produce a semi-continuous coverage of the alumina surface with a SiO.sub.2 film. Room temperature tensile strength was found to be proportional to the fraction of air fired surface covered by silicon-containing films. Similarly, the ratio of substrate fracture versus interface separation was also related to the amount of surface silicon present prior to brazing. This process can replace the need to perform a "moly-manganese" metallization step.

Synthesis of a potential semiconductor neutron detector crystal LiGa(Se/Te)2: materials purity and compatibility effects

NASA Astrophysics Data System (ADS)

Stowe, Ashley C.; Morrell, J.; Battacharya, Pijush; Tupitsyn, Eugene; Burger, Arnold

2011-09-01

Lithium containing AIBIIICVI semiconductors are being considered as alternative materials for room temperature neutron detection. One of the primary challenges in growing a high quality crystal of such a material is the reactivity of lithium metal. The presence of nitrides, oxides, and a variety of alkali and alkaline earth metal impurities prevent pure synthesis and truncate crystal growth by introducing multiple nucleation centers during growth. Multiple lithium metal purification methods have been investigated which ultimately raised the metal purity to 99.996%. Multi-cycle vacuum distillation removed all but 40 ppm of metal impurities in lithium metal. LiGa(Se/Te)2 was then synthesized with the high purity lithium metal by a variety of conditions. Lithium metal reacts violently with many standard crucible materials, and thermodynamic studies were undertaken to insure that an appropriate crucible choice was made, with high purity iron and boron nitride crucibles being the least reactive practical materials. Once conditions were optimized for synthesis of the chalcopyrite, vertical Bridgman crystal growth resulted in red crystals. The optical, electronic, and thermodynamic properties were collected.

[Determination of optical purity of alpha-phenylethylamine by high performance liquid chromatography with pre-column derivatization].

PubMed

Wang, Jinzhao; Zeng, Su; Wang, Danhua; Hu, Gongyun

2009-05-01

A simple pre-column derivatization-high performance liquid chromatographic (HPLC) method was established for the determination of optical purity of alpha-phenylethylamine. The enantiomers of alpha-phenylethylamine were derivatized with 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyl isothiocyanate (GITC). The resulted diastereoisomers were separated on an Agilent Zorbax C18 column (250 mm x 4.6 mm, 5 microm) with a mobile phase of methanol-phosphate buffer (1.36 g/L aqueous solution of potassium dihydrogen phosphate, adjusted to pH 3.0 with concentrated phosphoric acid) (58:42, v/v). The flow rate was set at 1.0 mL/min and the detection wavelength was set at 241 nm. The method was linear from 0.15 - 15.0 mg/L for both enantiomers. The limit of detection and the limit of quantification were 0.05 mg/L and 0.15 mg/L, respectively. The relative standard deviations (RSDs) of inter- and intra-day determination were below 0.5%. The method is easy to handle, accurate, and suitable for the quality control of the optical purity of alpha-phenylethylamine.

Wide dynamic range enrichment method of semiconducting single-walled carbon nanotubes with weak field centrifugation

NASA Astrophysics Data System (ADS)

Reis, Wieland G.; Tomović, Željko; Weitz, R. Thomas; Krupke, Ralph; Mikhael, Jules

2017-03-01

The potential of single-walled carbon nanotubes (SWCNTs) to outperform silicon in electronic application was finally enabled through selective separation of semiconducting nanotubes from the as-synthesized statistical mix with polymeric dispersants. Such separation methods provide typically high semiconducting purity samples with narrow diameter distribution, i.e. almost single chiralities. But for a wide range of applications high purity mixtures of small and large diameters are sufficient or even required. Here we proof that weak field centrifugation is a diameter independent method for enrichment of semiconducting nanotubes. We show that the non-selective and strong adsorption of polyarylether dispersants on nanostructured carbon surfaces enables simple separation of diverse raw materials with different SWCNT diameter. In addition and for the first time, we demonstrate that increased temperature enables higher purity separation. Furthermore we show that the mode of action behind this electronic enrichment is strongly connected to both colloidal stability and protonation. By giving simple access to electronically sorted SWCNTs of any diameter, the wide dynamic range of weak field centrifugation can provide economical relevance to SWCNTs.

Methods for Isolation and Purification of Murine Liver Sinusoidal Endothelial Cells: A Systematic Review.

PubMed

Meyer, Jeremy; Gonelle-Gispert, Carmen; Morel, Philippe; Bühler, Léo

2016-01-01

To study the biological functions of liver sinusoidal endothelial cells (LSEC) and to identify their interplay with blood or liver cells, techniques allowing for the isolation and purification of LSEC have been developed over the last decades. The objective of the present review is to summarize and to compare the efficiency of existing methods for isolating murine LSEC. Toward this end, the MEDLINE database was searched for all original articles describing LSEC isolation from rat and mouse livers. Out of the 489 publications identified, 23 reported the main steps and outcomes of the procedure and were included in our review. Here, we report and analyse the technical details of the essential steps of the techniques used for LSEC isolation. The correlations between the prevalence of some steps and the efficiency of LSEC isolation were also identified. We found that centrifugal elutriation, selective adherence and, more recently, magnetic-activated cell sorting were used for LSEC purification. Centrifugal elutriation procured high yields of pure LSEC (for rats 30-141.9 million cells for 85-98% purities; for mice 9-9.25 million cells for >95% purities), but the use of this method remained limited due to its high technical requirements. Selective adherence showed inconsistent results in terms of cell yields and purities in rats (5-100 million cells for 73.7-95% purities). In contrast, magnetic-activated cell sorting allowed for the isolation of highly pure LSEC, but overall lower cell yields were reported (for rats 10.7 million cells with 97.6% purity; for mice 0.5-9 million cells with 90-98% purities). Notably, the controversies regarding the accuracy of several phenotypic markers for LSEC should be considered and their use for both magnetic sorting and characterization remain doubtful. It appears that more effort is needed to refine and standardize the procedure for LSEC isolation, with a focus on the identification of specific antigens. Such a procedure is required to identify the molecular mechanisms regulating the function of LSEC and to improve our understanding of their role in complex cellular processes in the liver.

Methods for Isolation and Purification of Murine Liver Sinusoidal Endothelial Cells: A Systematic Review

PubMed Central

Meyer, Jeremy; Gonelle-Gispert, Carmen; Morel, Philippe; Bühler, Léo

2016-01-01

To study the biological functions of liver sinusoidal endothelial cells (LSEC) and to identify their interplay with blood or liver cells, techniques allowing for the isolation and purification of LSEC have been developed over the last decades. The objective of the present review is to summarize and to compare the efficiency of existing methods for isolating murine LSEC. Toward this end, the MEDLINE database was searched for all original articles describing LSEC isolation from rat and mouse livers. Out of the 489 publications identified, 23 reported the main steps and outcomes of the procedure and were included in our review. Here, we report and analyse the technical details of the essential steps of the techniques used for LSEC isolation. The correlations between the prevalence of some steps and the efficiency of LSEC isolation were also identified. We found that centrifugal elutriation, selective adherence and, more recently, magnetic-activated cell sorting were used for LSEC purification. Centrifugal elutriation procured high yields of pure LSEC (for rats 30–141.9 million cells for 85–98% purities; for mice 9–9.25 million cells for >95% purities), but the use of this method remained limited due to its high technical requirements. Selective adherence showed inconsistent results in terms of cell yields and purities in rats (5–100 million cells for 73.7–95% purities). In contrast, magnetic-activated cell sorting allowed for the isolation of highly pure LSEC, but overall lower cell yields were reported (for rats 10.7 million cells with 97.6% purity; for mice 0.5–9 million cells with 90–98% purities). Notably, the controversies regarding the accuracy of several phenotypic markers for LSEC should be considered and their use for both magnetic sorting and characterization remain doubtful. It appears that more effort is needed to refine and standardize the procedure for LSEC isolation, with a focus on the identification of specific antigens. Such a procedure is required to identify the molecular mechanisms regulating the function of LSEC and to improve our understanding of their role in complex cellular processes in the liver. PMID:26992171

Recovery of high-purity metallic Pd from Pd(II)-sorbed biosorbents by incineration.

PubMed

Won, Sung Wook; Lim, Areum; Yun, Yeoung-Sang

2013-06-01

This work reports a direct way to recover metallic palladium with high purity from Pd(II)-sorbed polyethylenimine-modified Corynebacterium glutamicum biosorbent using a combined method of biosorption and incineration. This study is focused on the incineration part which affects the purity of recovered Pd. The incineration temperature and the amount of Pd loaded on the biosorbent were considered as major factors in the incineration process, and their effects were examined. The results showed that both factors significantly affected the enhancement of the recovery efficiency and purity of the recovered Pd. SEM-EDX and XRD analyses were used to confirm that Pd phase existed in the ash. As a result, the recovered Pd was changed from PdO to zero-valent Pd as the incineration temperature was increased from 600 to 900°C. Almost 100% pure metallic Pd was recovered with recovery efficiency above 99.0% under the conditions of 900°C and 136.9 mg/g. Copyright © 2013 Elsevier Ltd. All rights reserved.

High-purity silicon for solar cell applications

NASA Technical Reports Server (NTRS)

Dosaj, V. D.; Hunt, L. P.; Schei, A.

1978-01-01

The article discusses the production of solar cells from high-purity silicon. The process consists of reducing the level of impurities in the raw materials, preventing material contamination before and after entering the furnace, and performing orders-of-magnitude reduction of metal impurity concentrations. The high-purity raw materials are considered with reference to carbon reductants, silica, and graphite electrodes. Attention is also given to smelting experiments used to demonstrate, in an experimental-scale furnace, the production of high-purity SoG-Si. It is found that high-purity silicon may be produced from high-purity quartz and chemically purified charcoal in a 50-kVA arc furnace. The major contamination source is shown to be impurities from the carbon reducing materials.

Ionic liquid-based extraction followed by graphite-furnace atomic absorption spectrometry for the determination of trace heavy metals in high-purity iron metal.

PubMed

Matsumiya, Hiroaki; Kato, Tatsuya; Hiraide, Masataka

2014-02-01

The analysis of high-purity materials for trace impurities is an important and challenging task. The present paper describes a facile and sensitive method for the determination of trace heavy metals in high-purity iron metal. Trace heavy metals in an iron sample solution were rapidly and selectively preconcentrated by the extraction into a tiny volume of an ionic liquid [1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide] for the determination by graphite-furnace atomic absorption spectrometry (GFAAS). A nitrogen-donating neutral ligand, 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ), was found to be effective in the ionic liquid-based selective extraction, allowing the nearly complete (~99.8%) elimination of the iron matrix. The combination with the optimized GFAAS was successful. The detectability reached sub-μg g(-1) levels in iron metal. The novel use of TPTZ in ionic liquid-based extraction followed by GFAAS was successfully applied to the determination of traces of Co, Ni, Cu, Cd, and Pb in certified reference materials for high-purity iron metal. © 2013 Published by Elsevier B.V.

Simple HPLC method for detection of trace ephedrine and pseudoephedrine in high-purity methamphetamine.

PubMed

Makino, Yukiko

2012-03-01

A simple and sensitive HPLC technique was developed for the qualitative determination of ephedrine and pseudoephedrine (ephedrines), used as precursors of clandestine d-methamphetamine hydrochloride of high purity. Good separation of ephedrines from bulk d-methamphetamine was achieved, without any extraction or derivatization procedure on a CAPCELLPACK C18 MGII (250 × 4.6 mm) column. The mobile phase consisted of 50 mM KH2 PO4-acetonitrile (94:6 v/v %) using an isocratic pump system within 20 min for detecting two analytes. One run took about 50 min as it was necessary to wash out overloaded methamphetamine for column conditioning. The analytes were detected by UV absorbance measurement at 210 nm. A sample (20 mg) was simply dissolved in 1 mL of water, and a 50 μL aliquot of the solution was injected into the HPLC. The detection limits for ephedrine and pseudoephedrine in bulk d-methamphetamine were as low as 3 ppm each. This analytical separation technique made it possible to detect ephedrine and/or pseudoephedrine in seven samples of high-purity d-methamphetamine hydrochloride seized in Japan. The presence of trace ephedrines in illicit methamphetamine may strongly indicate a synthetic route via ephedrine in methamphetamine profiling. This method is simple and sensitive, requiring only commonly available equipment, and should be useful for high-purity methamphetamine profiling. Copyright © 2011 John Wiley & Sons, Ltd.

Simplified Method to Isolate Highly Pure Canine Pancreatic Islets

PubMed Central

Woolcott, Orison O.; Bergman, Richard N.; Richey, Joyce M.; Kirkman, Erlinda L.; Harrison, L. Nicole; Ionut, Viorica; Lottati, Maya; Zheng, Dan; Hsu, Isabel R.; Stefanovski, Darko; Kabir, Morvarid; Kim, Stella P.; Catalano, Karyn J.; Chiu, Jenny D.; Chow, Robert H.

2015-01-01

Objectives The canine model has been used extensively to improve the human pancreatic islet isolation technique. At the functional level, dog islets show high similarity to human islets and thus can be a helpful tool for islet research. We describe and compare 2 manual isolation methods, M1 (initial) and M2 (modified), and analyze the variables associated with the outcomes, including islet yield, purity, and glucose-stimulated insulin secretion (GSIS). Methods Male mongrel dogs were used in the study. M2 (n = 7) included higher collagenase concentration, shorter digestion time, faster shaking speed, colder purification temperature, and higher differential density gradient than M1 (n = 7). Results Islet yield was similar between methods (3111.0 ± 309.1 and 3155.8 ± 644.5 islets/g, M1 and M2, respectively; P = 0.951). Pancreas weight and purity together were directly associated with the yield (adjusted R2 = 0.61; P = 0.002). Purity was considerably improved with M2 (96.7% ± 1.2% vs 75.0% ± 6.3%; P = 0.006). M2 improved GSIS (P = 0.021). Independently, digestion time was inversely associated with GSIS. Conclusions We describe an isolation method (M2) to obtain a highly pure yield of dog islets with adequate β-cell glucose responsiveness. The isolation variables associated with the outcomes in our canine model confirm previous reports in other species, including humans. PMID:21792087

Simplified NaCl based (68)Ga concentration and labeling procedure for rapid synthesis of (68)Ga radiopharmaceuticals in high radiochemical purity.

PubMed

Mueller, Dirk; Klette, Ingo; Baum, Richard P; Gottschaldt, M; Schultz, Michael K; Breeman, Wouter A P

2012-08-15

A simple sodium chloride (NaCl) based (68)Ga eluate concentration and labeling method that enables rapid, high-efficiency labeling of DOTA conjugated peptides in high radiochemical purity is described. The method utilizes relatively few reagents and comprises minimal procedural steps. It is particularly well-suited for routine automated synthesis of clinical radiopharmaceuticals. For the (68)Ga generator eluate concentration step, commercially available cation-exchange cartridges and (68)Ga generators were used. The (68)Ga generator eluate was collected by use of a strong cation exchange cartridge. 98% of the total activity of (68)Ga was then eluted from the cation exchange cartridge with 0.5 mL of 5 M NaCl solution containing a small amount of 5.5 M HCl. After buffering with ammonium acetate, the eluate was used directly for radiolabeling of DOTATOC and DOTATATE. The (68)Ga-labeled peptides were obtained in higher radiochemical purity compared to other commonly used procedures, with radiochemical yields greater than 80%. The presence of (68)Ge could not be detected in the final product. The new method obviates the need for organic solvents, which eliminates the required quality control of the final product by gas chromatography, thereby reducing postsynthesis analytical effort significantly. The (68)Ga-labeled products were used directly, with no subsequent purification steps, such as solid-phase extraction. The NaCl method was further evaluated using an automated fluid handling system and it routinely facilitates radiochemical yields in excess of 65% in less than 15 min, with radiochemical purity consistently greater than 99% for the preparation of (68)Ga-DOTATOC.

Measurement of the detective quantum efficiency in digital detectors consistent with the IEC 62220-1 standard: Practical considerations regarding the choice of filter material.

PubMed

Ranger, Nicole T; Samei, Ehsan; Dobbins, James T; Ravin, Carl E

2005-07-01

As part of a larger evaluation we attempted to measure the detective quantum efficiency (DQE) of an amorphous silicon flat-panel detector using the method described in the International Electrotechnical Commission standard 62220-1 published in October 2003. To achieve the radiographic beam conditions specified in the standard, we purchased scientific-grade ultrahigh purity aluminum (99.999% purity, type-11999 alloy) filters in thicknesses ranging from 0.1 through 10.0 mm from a well-known, specialty metals supplier. Qualitative evaluation of flat field images acquired at 71 kV (RQA5 beam quality) with 21 mm of ultrahigh purity aluminum filtration demonstrated a low frequency mottle that was reproducible and was not observed when the measurement was repeated at 74 kV (RQA5 beam quality) with 21 mm of lower-purity aluminum (99.0% purity, type-1100 alloy) filtration. This finding was ultimately attributed to the larger grain size (approximately 1-2 mm) of high purity aluminum metal, which is a well-known characteristic, particularly in thicknesses greater than 1 mm. The impact of this low frequency mottle is to significantly overestimate the noise power spectrum (NPS) at spatial frequencies ⩽0.2mm-1, which in turn would cause an underestimation of the DQE in this range. A subsequent evaluation of ultrahigh purity aluminum, purchased from a second source, suggests, that reduced grain size can be achieved by the process of annealing. Images acquired with this sample demonstrated vertical striated nonuniformities that are attributed to the manufacturing method and which do not appear to appreciably impact the NPS at spatial frequencies ⩾0.5mm-1, but do result in an asymmetry in the x- and y-NPS at spatial frequencies ⩽0.2mm-1. Our observations of markedly visible nonuniformities in images acquired with high purity aluminum filtration suggest that the uniformity of filter materials should be carefully evaluated and taken into consideration when measuring the DQE. © 2005 American Association of Physicists in Medicine.

Method for the recovery of silver from silver zeolite

DOEpatents

Reimann, G.A.

1985-03-05

High purity silver is recovered from silver exchanged zeolite used to capture radioactive iodine from nuclear reactor and nuclear fuel reprocessing environments. The silver exchanged zeolite is heated with slag formers to melt and fluidize the zeolite and release the silver, the radioactivity removing with the slag. The silver containing metallic impurities is remelted and treated with oxygen and a flux to remove the metal impurities. About 98% of the silver in the silver exchanged zeolite having a purity of 99% or better is recoverable by the method.

Method for the recovery of silver from silver zeolite

DOEpatents

Reimann, George A.

1986-01-01

High purity silver is recovered from silver exchanged zeolite used to capture radioactive iodine from nuclear reactor and nuclear fuel reprocessing environments. The silver exchanged zeolite is heated with slag formers to melt and fluidize the zeolite and release the silver, the radioactivity removing with the slag. The silver containing metallic impurities is remelted and treated with oxygen and a flux to remove the metal impurities. About 98% of the silver in the silver exchanged zeolite having a purity of 99% or better is recoverable by the method.

Unique low-molecular-weight lignin with high purity extracted from wood by deep eutectic solvents (DES): a source of lignin for valorization

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

Alvarez-Vasco, Carlos; Ma, Ruoshui; Quintero, Melissa

This paper reports a new method of applying Deep Eutectic Solvents (DES) for extracting lignin from woody biomass with high yield and high purity. DES mixtures prepared from Choline Chloride (ChCl) and four hydrogen-bond donors–acetic acid, lactic acid, levulinic acid and glycerol–were evaluated for treatment of hardwood (poplar) and softwood (D. fir). It was found that these DES treatments can selectively extract a significant amount of lignin from wood with high yields: 78% from poplar and 58% from D. fir. The extracted lignin has high purity (95%) with unique structural properties. We discover that DES can selectively cleave ether linkagesmore » in wood lignin and facilitate lignin removal from wood. The mechanism of DES cleavage of ether bonds between phenylpropane units was investigated. The results from this study demonstrate that DES is a promising solvent for wood delignification and the production of a new source of lignin with promising potential applications.« less

Discussion on the application of high additional value of high purity and high quality direct reduced iron

NASA Astrophysics Data System (ADS)

Yue, Chongfeng; Bai, Lu; Hong, Yicheng; Xu, Lijun

2018-03-01

The high purity and high quality direct reduced iron(DRI) products which were produced by high grade and high quality iron powder, with a high grade and low impurity characteristics. This article introduced the application of high purity and high quality DRI in the fields of amorphous base material, atomized iron powder, powder superalloy, high purity and ultra-low carbon special metallurgy products, precision casting, super alloy and various iron-based alloys. It provides a reference for the high added value utilization of DRI.

Arsine flow requirement for the flow modulation growth of high purity GaAs using adduct-grade triethylgallium

NASA Astrophysics Data System (ADS)

Pitts, B. L.; Emerson, D. T.; Shealy, J. R.

1992-10-01

Using arsine and triethylgallium with flow modulation, organometallic vapor phase epitaxy can produce high purity GaAs layers with V/III molar ratios near unity. We have estimated that under appropriate growth conditions the arsine incorporation efficiency into epitaxial GaAs can exceed 30%. The arsine flow requirement for obtaining good morphology has been identified over a range of substrate temperatures using adduct-grade triethylgallium. The process described reduces the environmental impact and life safety risk of the hydride based organometallic vapor phase epitaxial method.

Establishment of the purity values of carbohydrate certified reference materials using quantitative nuclear magnetic resonance and mass balance approach.

PubMed

Quan, Can

2014-06-15

This work described the assignment of purity values to six carbohydrate certified reference materials, including glucose, fructose, galactose, lactose, xylose and sucrose, according to the ISO Guides 34 and 35. The CRMs' purity values were assigned based on the weighted average of quantitative nuclear magnetic resonance method and mass balance approach with high resolution liquid chromatography - evaporative light scattering detection. All the six CRMs with following value amount fractions: glucose (GBW10062) at a certified purity P ± U (k=2) of (0.99 ± 0.005)%; fructose (GBW10063) at (0.99 ± 0.005)%; galactose (GBW10064) at (0.99 ± 0.007)%; lactose (GBW10065) at (0.99 ± 0.008)%; xylose (GBW10066) at (0.99 ± 0.007)% and sucrose (GBW10067) at (0.99 ± 0.008)%, respectively were certified. The homogeneity of the CRMs was determined by an in-house validated liquid chromatographic method. Potential degradation during storage was also investigated and a shelf-life based on this value was established. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simplified method to isolate highly pure canine pancreatic islets.

PubMed

Woolcott, Orison O; Bergman, Richard N; Richey, Joyce M; Kirkman, Erlinda L; Harrison, L Nicole; Ionut, Viorica; Lottati, Maya; Zheng, Dan; Hsu, Isabel R; Stefanovski, Darko; Kabir, Morvarid; Kim, Stella P; Catalano, Karyn J; Chiu, Jenny D; Chow, Robert H

2012-01-01

The canine model has been used extensively to improve the human pancreatic islet isolation technique. At the functional level, dog islets show high similarity to human islets and thus can be a helpful tool for islet research. We describe and compare 2 manual isolation methods, M1 (initial) and M2 (modified), and analyze the variables associated with the outcomes, including islet yield, purity, and glucose-stimulated insulin secretion (GSIS). Male mongrel dogs were used in the study. M2 (n = 7) included higher collagenase concentration, shorter digestion time, faster shaking speed, colder purification temperature, and higher differential density gradient than M1 (n = 7). Islet yield was similar between methods (3111.0 ± 309.1 and 3155.8 ± 644.5 islets/g, M1 and M2, respectively; P = 0.951). Pancreas weight and purity together were directly associated with the yield (adjusted R(2) = 0.61; P = 0.002). Purity was considerably improved with M2 (96.7% ± 1.2% vs 75.0% ± 6.3%; P = 0.006). M2 improved GSIS (P = 0.021). Independently, digestion time was inversely associated with GSIS. We describe an isolation method (M2) to obtain a highly pure yield of dog islets with adequate β-cell glucose responsiveness. The isolation variables associated with the outcomes in our canine model confirm previous reports in other species, including humans.

Process for producing high purity silicon nitride by the direct reaction between elemental silicon and nitrogen-hydrogen liquid reactants

DOEpatents

Pugar, Eloise A.; Morgan, Peter E. D.

1990-01-01

A process is disclosed for producing, at a low temperature, a high purity reaction product consisting essentially of silicon, nitrogen, and hydrogen which can then be heated to produce a high purity alpha silicon nitride. The process comprises: reacting together a particulate elemental high purity silicon with a high purity nitrogen-hydrogen reactant in its liquid state (such as ammonia or hydrazine) having the formula: N.sub.n H.sub.(n+m) wherein: n=1-4 and m=2 when the nitrogen-hydrogen reactant is straight chain, and 0 when the nitrogen-hydrogen reactant is cyclic. High purity silicon nitride can be formed from this intermediate product by heating the intermediate product at a temperature of from about 1200.degree.-1700.degree. C. for a period from about 15 minutes up to about 2 hours to form a high purity alpha silicon nitride product. The discovery of the existence of a soluble Si-N-H intermediate enables chemical pathways to be explored previously unavailable in conventional solid state approaches to silicon-nitrogen ceramics.

Process for producing high purity silicon nitride by the direct reaction between elemental silicon and nitrogen-hydrogen liquid reactants

DOEpatents

Pugar, E.A.; Morgan, P.E.D.

1987-09-15

A process is disclosed for producing, at a low temperature, a high purity reaction product consisting essentially of silicon, nitrogen, and hydrogen which can then be heated to produce a high purity alpha silicon nitride. The process comprises: reacting together a particulate elemental high purity silicon with a high purity nitrogen-hydrogen reactant in its liquid state (such as ammonia or hydrazine) having the formula: N/sub n/H/sub (n+m)/ wherein: n = 1--4 and m = 2 when the nitrogen-hydrogen reactant is straight chain, and 0 when the nitrogen-hydrogen reactant is cyclic. High purity silicon nitride can be formed from this intermediate product by heating the intermediate product at a temperature of from about 1200--1700/degree/C for a period from about 15 minutes up to about 2 hours to form a high purity alpha silicon nitride product. The discovery of the existence of a soluble Si/endash/N/endash/H intermediate enables chemical pathways to be explored previously unavailable in conventional solid-state approaches to silicon-nitrogen ceramics

Fate of Colored Smoke Dyes

DTIC Science & Technology

1992-01-01

4.13] have been applied to their estimation. This approach has the advantages of sensitivity and of not requiring high purity and known structures...Chrom absorbance detector, and an Alltech Econosil C-18 (10 micrometer) column (4.6 mm X 25 cm with guard column). The mobile phase, HPLC-grade methanol...water partition coefficient or vice versa. The HPLC method is of similar precision and has the advantage that known structure and purity of the dye are

Preparation of High Purity CdTe for Nuclear Detector: Electrical and Nuclear Characterization

NASA Astrophysics Data System (ADS)

Zaiour, A.; Ayoub, M.; Hamié, A.; Fawaz, A.; Hage-ali, M.

High purity crystal with controllable electrical properties, however, control of the electrical properties of CdTe has not yet been fully achieved. Using the refined Cd and Te as starting materials, extremely high-purity CdTe single crystals were prepared by the traditional vertical THM. The nature of the defects involved in the transitions was studied by analyzing the position of the energy levels by TSC method. The resolution of 4.2 keV (FWHM) confirms the high quality and stability of the detectors: TSC spectrum was in coherence with detectors spectrum with a horizontal plate between 0.2 and 0.6 eV. The enhancement in resolution of detectors with a full width at half- maximum (less than 0.31 meV), lead to confirm that the combination of vacuum distillation and zone refining was very effective to obtain more purified CdTe single crystals for photovoltaic or nuclear detectors with better physical properties.

Germanium recovery from gasification fly ash: evaluation of end-products obtained by precipitation methods.

PubMed

Arroyo, Fátima; Font, Oriol; Fernández-Pereira, Constantino; Querol, Xavier; Juan, Roberto; Ruiz, Carmen; Coca, Pilar

2009-08-15

In this study the purity of the germanium end-products obtained by two different precipitation methods carried out on germanium-bearing solutions was evaluated as a last step of a hydrometallurgy process for the recovery of this valuable element from the Puertollano Integrated Gasification Combined Cycle (IGCC) fly ash. Since H(2)S is produced as a by-product in the gas cleaning system of the Puertollano IGCC plant, precipitation of germanium as GeS(2) was tested by sulfiding the Ge-bearing solutions. The technological and hazardous issues that surround H(2)S handling conducted to investigate a novel precipitation procedure: precipitation as an organic complex by adding 1,2-dihydroxy benzene pyrocatechol (CAT) and cetyltrimethylammonium bromide (CTAB) to the Ge-bearing solutions. Relatively high purity Ge end-products (90 and 93% hexagonal-GeO(2) purity, respectively) were obtained by precipitating Ge from enriched solutions, as GeS(2) sulfiding the solutions with H(2)S, or as organic complex with CAT/CTAB mixtures and subsequent roasting of the precipitates. Both methods showed high efficiency (>99%) to precipitate selectively Ge using a single precipitation stage from germanium-bearing solutions.

Development of a new ferulic acid certified reference material for use in clinical chemistry and pharmaceutical analysis.

PubMed

Yang, Dezhi; Wang, Fengfeng; Zhang, Li; Gong, Ningbo; Lv, Yang

2015-05-01

This study compares the results of three certified methods, namely differential scanning calorimetry (DSC), the mass balance (MB) method and coulometric titrimetry (CT), in the purity assessment of ferulic acid certified reference material (CRM). Purity and expanded uncertainty as determined by the three methods were respectively 99.81%, 0.16%; 99.79%, 0.16%; and 99.81%, 0.26% with, in all cases, a coverage factor (k) of 2 (P=95%). The purity results are consistent indicating that the combination of DSC, the MB method and CT provides a confident assessment of the purity of suitable CRMs like ferulic acid.

Boehmite nanostructures preparation by hydrothermal method from anodic aluminium oxide membrane.

PubMed

Yang, X; Wang, J Y; Pan, H Y

2009-02-01

Boehmite nanostructures were successfully synthesized from porous anodic aluminium oxide (AAO) membrane by a simple and efficient hydro-thermal method. The experiment used high purity alumina as raw material, and the whole reaction process avoided superfluous impurities to be introduced. Thus, the purity of Boehmite products was ensured. The examinations of the morphology and structure were carried out by atomic force microscope (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Composition of the specimens was analyzed using energy dispersive X-ray spectroscope (EDX) and X-ray diffraction (XRD). Based on these observations the growth process was analyzed.

Passive particle dosimetry. [silver halide crystal growth

NASA Technical Reports Server (NTRS)

Childs, C. B.

1977-01-01

Present methods of dosimetry are reviewed with emphasis on the processes using silver chloride crystals for ionizing particle dosimetry. Differences between the ability of various crystals to record ionizing particle paths are directly related to impurities in the range of a few ppm (parts per million). To understand the roles of these impurities in the process, a method for consistent production of high purity silver chloride, and silver bromide was developed which yields silver halides with detectable impurity content less than 1 ppm. This high purity silver chloride was used in growing crystals with controlled doping. Crystals were grown by both the Czochalski method and the Bridgman method, and the Bridgman grown crystals were used for the experiments discussed. The distribution coefficients of ten divalent cations were determined for the Bridgman crystals. The best dosimeters were made with silver chloride crystals containing 5 to 10 ppm of lead; other impurities tested did not produce proper dosimeters.

Tracking metastatic breast cancer: the future of biology in biosensors.

PubMed

Lim, Y C; Wiegmans, A P

2016-04-01

Circulating tumour cells associated with breast cancer (brCTCs) represent cells that have the capability to establish aggressive secondary metastatic tumours. The isolation and characterization of CTCs from blood in a single device is the future of oncology diagnosis and treatment. The methods of enrichment of CTCs have primarily utilized simple biological interactions with bimodal reporting with biased high purity and low numbers or low purity and high background. In this review, we will discuss the advances in microfluidics that has allowed the use of more complex selection criteria and biological methods to identify CTC populations. We will also discuss a potential new method of selection based on the response of the oncogenic DNA repair pathways within brCTCs. This method would allow insight into not only the oncogenic signalling at play but the chemoresistance mechanisms that could guide future therapeutic intervention at any stage of disease progression.

Multidimensional preparative liquid chromatography to isolate flavonoids from bergamot juice and evaluation of their anti-inflammatory potential.

PubMed

Russo, Marina; Dugo, Paola; Marzocco, Stefania; Inferrera, Veronica; Mondello, Luigi

2015-12-01

Important objectives of a high-performance liquid chromatography preparative process are: purity of products isolated, yield, and throughput. The multidimensional preparative liquid chromatography method used in this work was developed mainly to increase the throughput; moreover purity and yield are increased thanks to the automated collection of the molecules based on the intensity of a signal generated from the mass spectrometer detector, in this way only a specific product can be targeted. This preparative system allowed, in few analyses both in the first and second dimensions, the isolation of eight pure compounds present at very different concentration in the original sample with high purity (>95%) and yield, which showed how the system is efficient and versatile. Pure molecules were used to validate the analytical method and to test the anti-inflammatory and antiproliferative potential of flavonoids. The contemporary presence, in bergamot juice, of all the flavonoids together increases the anti-inflammatory effect with respect to the single compound alone. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Efficient conversion of sand to nano-silicon and its energetic Si-C composite anode design for high volumetric capacity lithium-ion battery

NASA Astrophysics Data System (ADS)

Furquan, Mohammad; Raj Khatribail, Anish; Vijayalakshmi, Savithri; Mitra, Sagar

2018-04-01

Silicon is an attractive anode material for Li-ion cells, which can provide energy density 30% higher than any of the today's commercial Li-ion cells. In the current study, environmentally benign, high abundant, and low cost sand (SiO2) source has been used to prepare nano-silicon via scalable metallothermic reduction method using micro wave heating. In this research, we have developed and optimized a method to synthesis high purity nano silicon powder that takes only 5 min microwave heating of sand and magnesium mixture at 800 °C. Carbon coated nano-silicon electrode material is prepared by a unique method of coating, polymerization and finally in-situ carbonization of furfuryl alcohol on to the high purity nano-silicon. The electrochemical performance of a half cell using the carbon coated high purity Si is showed a stable capacity of 1500 mAh g-1 at 6 A g-1 for over 200 cycles. A full cell is fabricated using lithium cobalt oxide having thickness ≈56 μm as cathode and carbon coated silicon thin anode of thickness ≈9 μm. The fabricated full cell of compact size exhibits excellent volumetric capacity retention of 1649 mAh cm-3 at 0.5 C rate (C = 4200 mAh g-1) and extended cycle life (600 cycles). The full cell is demonstrated on an LED lantern and LED display board.

Correlation between product purity and process parameters for the synthesis of Cu2ZnSnS4 nanoparticles using microwave irradiation

NASA Astrophysics Data System (ADS)

Ahmad, R.; Nicholson, K. S.; Nawaz, Q.; Peukert, W.; Distaso, M.

2017-07-01

Kesterites (CZT(S,Se)4) emerged as a favourable photovoltaic material, leading to solar cell efficiencies as high as 12.7%. The development of sustainable roll-to-roll printing processes that make use of Cu2ZnSnS4 (CZTS) nanoparticle inks requires the proper design of synthetic approaches and the understanding of the relation between process parameters and product purity. In the current paper, we developed this relationship by calculating a specific energy factor. A microwave-assisted synthetic method that operates at atmospheric pressure and makes use of eco-friendly solvents is established. Four solvents, i.e. ethylene glycol (EG), diethylene glycol (di-EG), triethylene glycol (tri-EG) and tetraethylene glycol (tet-EG) are compared and the temperature during the reaction is assessed by two different methods. In particular, two by-products have been identified, i.e. Cu2 - x S and a hexagonal phase. We show that the variation of reaction parameters such as power irradiation, type of solvent and precursor concentration influences the nanoparticles' sizes (from 12 to 6 nm) and also the temperature-time profile of reaction which, in turn, can be related to phase purity of CZTS nanoparticles. The results suggest that the product purity scales with the specific energy factor providing a useful tool to a rational design of high-quality CZTS nanoparticles.

A novel method to prepare L-Arabinose from xylose mother liquor by yeast-mediated biopurification

PubMed Central

2011-01-01

Background L-arabinose is an important intermediate for anti-virus drug synthesis and has also been used in food additives for diets-controlling in recent years. Commercial production of L-arabinose is a complex progress consisting of acid hydrolysis of gum arabic, followed by multiple procedures of purification, thus making high production cost. Therefore, there is a biotechnological and commercial interest in the development of new cost-effective and high-performance methods for obtaining high purity grade L-arabinose. Results An alternative, economical method for purifying L-arabinose from xylose mother liquor was developed in this study. After screening 306 yeast strains, a strain of Pichia anomala Y161 was selected as it could effectively metabolize other sugars but not L-arabinose. Fermentation in a medium containing xylose mother liquor permitted enrichment of L-arabinose by a significant depletion of other sugars. Biochemical analysis of this yeast strain confirmed that its poor capacity for utilizing L-arabinose was due to low activities of the enzymes required for the metabolism of this sugar. Response surface methodology was employed for optimization the fermentation conditions in shake flask cultures. The optimum conditions were: 75 h fermentation time, at 32.5°C, in a medium containing 21% (v/v) xylose mother liquor. Under these conditions, the highest purity of L-arabinose reached was 86.1% of total sugar, facilitating recovery of white crystalline L-arabinose from the fermentation medium by simple methods. Conclusion Yeast-mediated biopurification provides a dynamic method to prepare high purity of L-arabinose from the feedstock solution xylose mother liqour, with cost-effective and high-performance properties. PMID:21649890

Isotopic composition analysis and age dating of uranium samples by high resolution gamma ray spectrometry

NASA Astrophysics Data System (ADS)

Apostol, A. I.; Pantelica, A.; Sima, O.; Fugaru, V.

2016-09-01

Non-destructive methods were applied to determine the isotopic composition and the time elapsed since last chemical purification of nine uranium samples. The applied methods are based on measuring gamma and X radiations of uranium samples by high resolution low energy gamma spectrometric system with planar high purity germanium detector and low background gamma spectrometric system with coaxial high purity germanium detector. The ;Multigroup γ-ray Analysis Method for Uranium; (MGAU) code was used for the precise determination of samples' isotopic composition. The age of the samples was determined from the isotopic ratio 214Bi/234U. This ratio was calculated from the analyzed spectra of each uranium sample, using relative detection efficiency. Special attention is paid to the coincidence summing corrections that have to be taken into account when performing this type of analysis. In addition, an alternative approach for the age determination using full energy peak efficiencies obtained by Monte Carlo simulations with the GESPECOR code is described.

Comparison of different methods for radiochemical purity testing of [99mTc-EDDA-HYNIC-D-Phe1,Tyr3]-octreotide.

PubMed

von Guggenberg, Elisabeth; Penz, Barbara; Kemmler, Georg; Virgolini, Irene; Decristoforo, Clemens

2006-02-01

[99mTc-EDDA-HYNIC-D-Phe1,Tyr3]-octreotide (99mTc-EDDA-HYNIC-TOC) is an alternative radioligand for somatostatin receptor (SSTR) scintigraphy of neuroendocrine tumours. In order to allow a rapid and accurate determination of the quality in the clinical routine the aim of this study was to evaluate different methods of radiochemical purity (RCP) testing. Three different methods of RCP testing were compared: high-performance liquid chromatography (HPLC), thin layer chromatography (TLC) and minicolumn (Sep-Pak purification = SPE). HPLC was shown to be the most effective method for the quality control. The use of TLC and SPE is only recommended after sufficient practical labelling experience.

Nitrogen-atom endohedral fullerene synthesis with high efficiency by controlling plasma-ion irradiation energy and C60 internal energy

NASA Astrophysics Data System (ADS)

Cho, Soon Cheon; Kaneko, Toshiro; Ishida, Hiroyasu; Hatakeyama, Rikizo

2015-03-01

The nitrogen-atom endohedral fullerene (N@C60) has been synthesized by controlling the plasma ion irradiation energy (Ei) and fullerene (C60) behavior in the sublimation phase. We examined the relationship between the synthesis purity of N@C60 [molar concentration ratio of N@C60 to pristine fullerene (C60)] and Ei, which was controlled by changing the substrate bias voltages (Vsub) and gas pressure (PN2) during the plasma irradiation process. High-density nitrogen-molecular ions (N2+) with a suitable Ei near 80 eV are confirmed to be the optimum condition of the nitrogen plasma for the synthesis of high-purity N@C60. In addition, high sublimation of C60 contributes to a higher yield due to the high internal energy of C60 and the related cage defects that are present under these conditions. As a result, a purity of 0.83% is realized for the first time, which is almost two orders of magnitude higher than that using other methods.

First Measurement of the Radionuclide Purity of the Therapeutic Isotope 67Cu Produced by 68Zn(n,x) Reaction Using natC(d,n) Neutrons

NASA Astrophysics Data System (ADS)

Sato, Nozomi; Tsukada, Kazuaki; Watanabe, Satoshi; Ishioka, Noriko S.; Kawabata, Masako; Saeki, Hideya; Nagai, Yasuki; Kin, Tadahiro; Minato, Futoshi; Iwamoto, Nobuyuki; Iwamoto, Osamu

2014-07-01

We have for the first time studied the radionuclide purity of the therapeutic isotope 67Cu produced by the 68Zn(n,x)67Cu reaction. The neutrons were obtained by the natC(d,n) reaction using 40 MeV deuterons. We measured the γ-ray spectra of the reaction products produced by bombarding an enriched 68ZnO sample with the neutrons with a high-purity Ge detector. We found that the relative production yields of the impurity radionuclides 64Cu, 65Zn, and 69mZn to 67Cu are extremely low. The result indicates that the 68Zn(n,x)67Cu reaction is the most promising among those proposed routes until now for producing high-quality 67Cu, and could solve a longstanding problem of establishing an appropriate production method for 67Cu.

Co-precipitation of protein and polyester as a method to isolate high molecular weight DNA.

PubMed

Dixson, Jamie D

2005-02-01

DNA isolation is often the limiting step in genetic analysis using PCR and automated fragment analysis due to low quality or purity of DNA, the need to determine and adjust DNA concentrations after isolation etc. Several protocols have been developed which are either safe and provide good quality DNA or hazardous and provide excellent quality DNA. In this brief communication I describe a new and rapid method of DNA isolation which employs the co-precipitation of protein and polyester, in the presence of acetone, to remove contaminating proteins from a lysed-tissue sample, thus leaving high quality pure DNA. The advantages of this method are increased safety over the phenol:chloroform and the chaotrophic salt methods and increased purity over the salting-out method. Since the concentrations of DNA isolated using this method are relatively consistent regardless of the amount of starting tissue (within limits), adjustments of the DNA concentrations before use as templates in PCR's are not necessary.

A simple-rapid method to separate uranium, thorium, and protactinium for U-series age-dating of materials

PubMed Central

Knight, Andrew W.; Eitrheim, Eric S.; Nelson, Andrew W.; Nelson, Steven; Schultz, Michael K.

2017-01-01

Uranium-series dating techniques require the isolation of radionuclides in high yields and in fractions free of impurities. Within this context, we describe a novel-rapid method for the separation and purification of U, Th, and Pa. The method takes advantage of differences in the chemistry of U, Th, and Pa, utilizing a commercially-available extraction chromatographic resin (TEVA) and standard reagents. The elution behavior of U, Th, and Pa were optimized using liquid scintillation counting techniques and fractional purity was evaluated by alpha-spectrometry. The overall method was further assessed by isotope dilution alpha-spectrometry for the preliminary age determination of an ancient carbonate sample obtained from the Lake Bonneville site in western Utah (United States). Preliminary evaluations of the method produced elemental purity of greater than 99.99% and radiochemical recoveries exceeding 90% for U and Th and 85% for Pa. Excellent purity and yields (76% for U, 96% for Th and 55% for Pa) were also obtained for the analysis of the carbonate samples and the preliminary Pa and Th ages of about 39,000 years before present are consistent with 14C-derived age of the material. PMID:24681438

Uncertainty estimates of purity measurements based on current information: toward a "live validation" of purity methods.

PubMed

Apostol, Izydor; Kelner, Drew; Jiang, Xinzhao Grace; Huang, Gang; Wypych, Jette; Zhang, Xin; Gastwirt, Jessica; Chen, Kenneth; Fodor, Szilan; Hapuarachchi, Suminda; Meriage, Dave; Ye, Frank; Poppe, Leszek; Szpankowski, Wojciech

2012-12-01

To predict precision and other performance characteristics of chromatographic purity methods, which represent the most widely used form of analysis in the biopharmaceutical industry. We have conducted a comprehensive survey of purity methods, and show that all performance characteristics fall within narrow measurement ranges. This observation was used to develop a model called Uncertainty Based on Current Information (UBCI), which expresses these performance characteristics as a function of the signal and noise levels, hardware specifications, and software settings. We applied the UCBI model to assess the uncertainty of purity measurements, and compared the results to those from conventional qualification. We demonstrated that the UBCI model is suitable to dynamically assess method performance characteristics, based on information extracted from individual chromatograms. The model provides an opportunity for streamlining qualification and validation studies by implementing a "live validation" of test results utilizing UBCI as a concurrent assessment of measurement uncertainty. Therefore, UBCI can potentially mitigate the challenges associated with laborious conventional method validation and facilitates the introduction of more advanced analytical technologies during the method lifecycle.

Method for nuclear magnetic resonance imaging

DOEpatents

Kehayias, J.J.; Joel, D.D.; Adams, W.H.; Stein, H.L.

1988-05-26

A method for in vivo NMR imaging of the blood vessels and organs of a patient characterized by using a dark dye-like imaging substance consisting essentially of a stable, high-purity concentration of D/sub 2/O in a solution with water.

Impact of US and Canadian precursor regulation on methamphetamine purity in the United States.

PubMed

Cunningham, James K; Liu, Lon-Mu; Callaghan, Russell

2009-03-01

Reducing drug purity is a major, but largely unstudied, goal of drug suppression. This study examines whether US methamphetamine purity was impacted by the suppression policy of US and Canadian precursor chemical regulation. Autoregressive integrated moving average (ARIMA)-intervention time-series analysis. Continental United States and Hawaii (1985-May 2005). Interventions US federal regulations targeting precursors, ephedrine and pseudoephedrine, in forms used by large-scale producers were implemented in November 1989, August 1995 and October 1997. US regulations targeting precursors in forms used by small-scale producers (e.g. over-the-counter medications) were implemented in October 1996 and October 2001. Canada implemented federal precursor regulations in January 2003 and July 2003 and an essential chemical (e.g. acetone) regulation in January 2004. Monthly median methamphetamine purity series. US regulations targeting large-scale producers were associated with purity declines of 16-67 points; those targeting small-scale producers had little or no impact. Canada's precursor regulations were associated with purity increases of 13-15 points, while its essential chemical regulation was associated with a 13-point decrease. Hawaii's purity was consistently high, and appeared to vary little with the 1990s/2000s regulations. US precursor regulations targeting large-scale producers were associated with substantial decreases in continental US methamphetamine purity, while regulations targeting over-the-counter medications had little or no impact. Canada's essential chemical regulation was also associated with a decrease in continental US purity. However, Canada's precursor regulations were associated with purity increases: these regulations may have impacted primarily producers of lower-quality methamphetamine, leaving higher-purity methamphetamine on the market by default. Hawaii's well-known preference for 'ice' (high-purity methamphetamine) may have helped to constrain purity there to a high, attenuated range, possibly limiting its sensitivity to precursor regulation.

Catalytic asymmetric synthesis of chiral propargylic alcohols for the intramolecular Pauson-Khand cycloaddition.

PubMed

Turlington, Mark; Yue, Yang; Yu, Xiao-Qi; Pu, Lin

2010-10-15

Several methods for the catalytic asymmetric alkyne addition to aldehydes are used to prepare the propargylic alcohol-based chiral en-ynes. Protection of the propargylic alcohols with either an acetyl or a methyl group allows the resulting en-ynes to undergo the intramolecular Pauson-Khand reaction to form the corresponding optically active 5,5- and 5,6-fused bicyclic products with high diastereoselectivity and high enantiomeric purity. In the major product, the propargylic substituent and the bridgehead hydrogen are cis with respect to each other on the fused bicyclic rings. The enantiomeric purity of the propargylic alcohols generated from the asymmetric alkyne addition is maintained in the cycloaddition products. The allylic ethers of the chiral propargylic alcohols are prepared which can also undergo the highly diastereoselective Pauson-Khand cycloaddition with retention of the high enantiomeric purity. This study has shown that the size of the substituents at the propargylic position as well as on the alkyne is important for the diastereoselectivity with the greater bulkiness of the substituents giving higher diastereoselectivity.

High performance liquid chromatography with photo diode array for separation and analysis of naproxen and esomeprazole in presence of their chiral impurities: Enantiomeric purity determination in tablets.

PubMed

Ragab, Marwa A A; El-Kimary, Eman I

2017-05-12

A stereoselective high performance liquid chromatographic method with diode array detection (HPLC-DAD) was introduced for S-naproxen and esomeprazole determination in tablets. The separation was achieved on a Kromasil Cellucoat chiral column using a mobile phase consisting of hexane: isopropanol: trifluoroacetic acid (TFA) (90:9.9:0.1 v/v/v). The proposed system was found to be suitable for the enantioseparation of naproxen and omeprazole biologically active isomers. After optimization of the chromatographic conditions, resolution values of 3.84 and 2.17 could be obtained for naproxen and omeprazole isomers, respectively. The method was fully validated for the determination of S-isomers of each drug in their dosage form. Also, the enentiomeric purity was determined in commercial tablet containing S-naproxen and esomeprazole. The enantiomeric purity was calculated for each drug and the chiral impurities (R-isomers) could be determined at 1% level. The method was validated and good results with respect to linearity, precision, accuracy, selectivity and robustness were obtained. The limits of detection (LOD) and quantification (LOQ) were 2.00, 6.50 and 0.10, 0.35μgmL -1 for S-naproxen and esomeprazole, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

A comparative uncertainty study of the calibration of macrolide antibiotic reference standards using quantitative nuclear magnetic resonance and mass balance methods.

PubMed

Liu, Shu-Yu; Hu, Chang-Qin

2007-10-17

This study introduces the general method of quantitative nuclear magnetic resonance (qNMR) for the calibration of reference standards of macrolide antibiotics. Several qNMR experimental conditions were optimized including delay, which is an important parameter of quantification. Three kinds of macrolide antibiotics were used to validate the accuracy of the qNMR method by comparison with the results obtained by the high performance liquid chromatography (HPLC) method. The purities of five common reference standards of macrolide antibiotics were measured by the 1H qNMR method and the mass balance method, respectively. The analysis results of the two methods were compared. The qNMR is quick and simple to use. In a new medicine research and development process, qNMR provides a new and reliable method for purity analysis of the reference standard.

Titania nanospheres from supercritical fluids.

PubMed

Darr, J A; Kellici, S; Rehman, I U

2005-06-01

Surfactant-coated amorphous titania nanospheres have been synthesised using templating 'water-in-supercritical carbon dioxide' emulsion droplets; the process represents a clean and controlled method for the manufacture of high-purity nanoparticles.

Preparation of Sesquiterpenoids from Tussilago farfara L. by High-speed Counter-current Chromatography

PubMed Central

Cao, Kun; Xu, Yi; Zhao, Tian-Ming; Zhang, Qing

2016-01-01

Background: Sesquiterpenoids, such as tussilagone, has effects of raising blood pressure, antiplatelet aggregation, and anti-inflammation activities, which is regarded as index compound for quality control of Tussilago farfara L. Objective: This study was aimed to obtain an effective method for fast isolation of sesquiterpenoids from T. farfara L. by high-speed counter-current chromatography (HSCCC). Materials and Methods: A solvent optimization method for HSCCC was presented, i.e., the separation factors of compounds after the K values of solvent system should be investigated. Results: A ternary solvent system of n-hexane:methanol:water (5:8:2, v/v/v) was selected and applied for the HSCCC, and 56 mg of tussilagone (2) was isolated from T. farfara L., along with two other sesquiterpenoids 5.6 mg of 2,2-dimethyl-6-acetylchromanone (1) and 22 mg of 14-acetoxy-7 β-(3’-ethyl cis-crotonoyloxy)-lα-(2’-methylbutyryloxy)-notonipetranone (3) by HSCCC with high purities. Their chemical structures were elucidated by liquid chromatography-mass spectrometry and nuclear magnetic resonance experiments. Conclusion: These results offered an efficient strategy for preparation of potentially health-relevant phytochemicals from T. farfara L., which might be used for further chemical research and pharmacological studies by preparative HSCCC. SUMMARY The real separation efficiency has been verified by analytical HSCCC.A solvent optimization method for HSCCC was presented and applied to separate and prepare active compounds.A method for rapid and effective separation of target compound Tussilagone with high yield and purity from the flower buds of Tussilago farfara.Two other compounds 2,2-Dimethyl-6-acetylchromanone and 14-acetoxy-7β-(3’-ethyl cis-crotonoyloxy) -lα- (2’-methylbutyryloxy). notonipetranone hasbeen obtained with high purities from flower buds of Tussilago farfara. Abbreviations used: HSCCC: High-Speed Counter-Current Chromatography; LC-MS: Liquid Chromatograph-Mass Spectrometer; NMR: Nuclear Magnetic Resonance; TCM: Traditional Chinese Medicine; HPLC: High Performance Liquid Chromatography; ESI-MS: Electrospray Ionization Mass Spectrometry; PE: petroleum ether PMID:27867270

Methods to isolate extracellular vesicles for diagnosis

NASA Astrophysics Data System (ADS)

Kang, Hyejin; Kim, Jiyoon; Park, Jaesung

2017-12-01

Extracellular vesicles (EVs) are small membrane-bound bodies that are released into extracellular space by diverse cells, and are found in body fluids like blood, urine and saliva. EVs contain RNA, DNA and proteins, which can be biomarkers for diagnosis. EVs can be obtained by minimally-invasive biopsy, so they are useful in disease diagnosis. High yield and purity contribute to precise diagnosis of disease, but damaged EVs and impurities can cause confu sed results. However, EV isolation methods have different yields and purities. Furthermore, the isolation method that is most suitable to maximize EV recovery efficiency depends on the experimental conditions. This review focuses on merits and demerits of several types of EV isolation methods, and provides examples of how to diagnose disease by exploiting information obtained by analysis of EVs.

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

PubMed

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

2010-10-01

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

Selective sequential precipitation of dissolved metals in mine drainage from coal mine

NASA Astrophysics Data System (ADS)

Yim, Giljae; Bok, Songmin; Ji, Sangwoo; Oh, Chamteut; Cheong, Youngwook; Han, Youngsoo; Ahn, Joosung

2017-04-01

In abandoned mines in Korea, a large amount of mine drainage continues to flow out and spread pollution. In purification of the mine drainage a massive amount of sludge is generated as waste. Since this metal sludge contains high Fe, Al and Mn oxides, developing the treatment method to recover homogeneous individual metal with high purity may beneficial to recycle waste metals as useful resources and reduce the amount of sludge production. In this regard, we established a dissolved metals selective precipitation process to treat Waryong Industry's mine drainage. The process that selectively precipitates metals dissolved in mine drainage is a continuous Fe-buffer-Al process, and each process consists of the neutralization tank, the coagulation tank, and the settling tank. Based on this process, this study verified the operational applicability of the Fe and Al selective precipitation. Our previous study revealed that high-purity Fe and Al precipitates could be recovered at a flow rate of 1.5 ton/day, while the lower purity was achieved when the rate was increased to about 3 ton/day due to the difficulty in reagent dosage control. In the current study was conducted to increase the capacity of the system to recover Fe and Al as high-purity precipitates at a flow rate of 10 ton/day with the ensured continuous operations by introducing an automatic reagent injection system. The previous study had a difficulty in controlling the pH and operating system continuously due to the manually controlled reagent injection system. To upgrade this and ensure the optimal pH in a stable way, a continuous reagent injection system was installed. The result of operation of the 10 ton/day system confirmed that the scaled-up process could maintain the stable recovery rates and purities of precipitates on site.

Pulsed laser diffusion of thin hole-barrier contacts in high purity germanium for gamma radiation detectors

NASA Astrophysics Data System (ADS)

Maggioni, G.; Carturan, S.; Raniero, W.; Riccetto, S.; Sgarbossa, F.; Boldrini, V.; Milazzo, R.; Napoli, D. R.; Scarpa, D.; Andrighetto, A.; Napolitani, E.; De Salvador, D.

2018-03-01

A new method for the formation of hole-barrier contacts in high purity germanium (HPGe) is described, which consists in the sputter deposition of a Sb film on HPGe, followed by Sb diffusion produced through laser annealing of the Ge surface in the melting regime. This process gives rise to a very thin ( ≤ 100 nm) n-doped layer, as determined by SIMS measurement, while preserving the defect-free morphology of HPGe surface. A small prototype of gamma ray detector with a Sb laser-diffused contact was produced and characterized, showing low leakage currents and good spectroscopy data with different gamma ray sources.

The Production of High Purity Phycocyanin by Spirulina platensis Using Light-Emitting Diodes Based Two-Stage Cultivation.

PubMed

Lee, Sang-Hyo; Lee, Ju Eun; Kim, Yoori; Lee, Seung-Yop

2016-01-01

Phycocyanin is a photosynthetic pigment found in photosynthetic cyanobacteria, cryptophytes, and red algae. In general, production of phycocyanin depends mainly on the light conditions during the cultivation period, and purification of phycocyanin requires expensive and complex procedures. In this study, we propose a new two-stage cultivation method to maximize the quantitative content and purity of phycocyanin obtained from Spirulina platensis using red and blue light-emitting diodes (LEDs) under different light intensities. In the first stage, Spirulina was cultured under a combination of red and blue LEDs to obtain the fast growth rate until reaching an absorbance of 1.4-1.6 at 680 nm. Next, blue LEDs were used to enhance the concentration and purity of the phycocyanin in Spirulina. Two weeks of the two-stage cultivation of Spirulina yielded 1.28 mg mL(-1) phycocyanin with the purity of 2.7 (OD620/OD280).

Pulsed laser triggered high speed microfluidic fluorescence activated cell sorter†‡

PubMed Central

Wu, Ting-Hsiang; Chen, Yue; Park, Sung-Yong; Hong, Jason; Teslaa, Tara; Zhong, Jiang F.; Di Carlo, Dino; Teitell, Michael A.

2014-01-01

We report a high speed and high purity pulsed laser triggered fluorescence activated cell sorter (PLACS) with a sorting throughput up to 20 000 mammalian cells s−1 with 37% sorting purity, 90% cell viability in enrichment mode, and >90% purity in high purity mode at 1500 cells s−1 or 3000 beads s−1. Fast switching (30 μs) and a small perturbation volume (~90 pL) is achieved by a unique sorting mechanism in which explosive vapor bubbles are generated using focused laser pulses in a single layer microfluidic PDMS channel. PMID:22361780

Impact of metal-induced degradation on the determination of pharmaceutical compound purity and a strategy for mitigation.

PubMed

Dotterer, Sally K; Forbes, Robert A; Hammill, Cynthia L

2011-04-05

Case studies are presented demonstrating how exposure to traces of transition metals such as copper and/or iron during sample preparation or analysis can impact the accuracy of purity analysis of pharmaceuticals. Some compounds, such as phenols and indoles, react with metals in the presence of oxygen to produce metal-induced oxidative decomposition products. Compounds susceptible to metal-induced decomposition can degrade following preparation for purity analysis leading to falsely high impurity results. Our work has shown even metals at levels below 0.1 ppm can negatively impact susceptible compounds. Falsely low results are also possible when the impurities themselves react with metals and degrade prior to analysis. Traces of metals in the HPLC mobile phase can lead to chromatographic artifacts, affecting the reproducibility of purity results. To understand and mitigate the impact of metal induced decomposition, a proactive strategy is presented. The pharmaceutical would first be tested for reactivity with specific transition metals in the sample solvent/diluents and in the HPLC mobile phase. If found to be reactive, alternative sample diluents and/or mobile phases with less reactive solvents or addition of a metal chelator would be explored. If unsuccessful, glassware cleaning or sample solution refrigeration could be investigated. By employing this strategy during method development, robust purity methods would be delivered to the quality control laboratories, preventing future problems from potential sporadic contamination of glassware with metals. Copyright © 2010 Elsevier B.V. All rights reserved.

Production of metals and compounds by radiation chemistry

NASA Technical Reports Server (NTRS)

Marsik, S. J.; Philipp, W. H.

1969-01-01

Preparation of metals and compounds by radiation induced chemical reactions involves irradiation of metal salt solutions with high energy electrons. This technique offers a method for the preparation of high purity metals with minimum contamination from the container material or the cover gas.

Synthesis of oleoylethanolamide using lipase.

PubMed

Wang, Xiaosan; Wang, Xingguo; Wang, Tong

2012-01-11

An effective process for the enzymatic synthesis of oleoylethanolamide is described in this study. The process included purification of a commercial oleic acid product and then optimization of the reaction between the purified oleic acid and ethanolamine in the presence of hexane and a lipase. Under the optimal amidation reaction conditions identified, oleoylethanolamide was obtained with 96.6% purity. The synthesis was also conducted on a large scale (50 mmol of each of the reactants), and oleoylethanolamide purity and yield after crystallization purification were 96.1 and 73.5%, respectively. Compared to the previous studies, the current method of preparing high-purity oleoylethanolamide is more effective and economically feasible. The scalability and ease for such synthesis make it possible to study the biological and nutritional functions of the cannabinoid-like oleoylethanolamide in animal or human subjects.

Radiochemical purity of Mo and Tc solution obtained after irradiation and dissolution of Mo-100-enriched and ultra-high-purity natural Mo disks

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

Tkac, Peter; Gromov, Roman; Chemerisov, Sergey D.

2016-09-01

Four irradiations of ultra-high-purity natural Mo targets and one irradiation using 97.4% Mo-100-enriched material were performed. The purpose of these irradiations was to determine whether the presence of Sn stabilizer in the H 2O 2 used for the dissolution of sintered Mo disks can affect the radiochemical purity of the final K 2MoO 4 in 5M KOH solution. Results from radiochemical purity tests performed using thin-layer paper chromatography show that even 2– 3× excess of Sn-stabilized H 2O 2 typically used for dissolution of sintered Mo disks did not affect the radiochemical purity of the final product.

Nitrogen-atom endohedral fullerene synthesis with high efficiency by controlling plasma-ion irradiation energy and C{sub 60} internal energy

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

Cho, Soon Cheon; Kaneko, Toshiro, E-mail: kaneko@ecei.tohoku.ac.jp; Ishida, Hiroyasu

2015-03-28

The nitrogen-atom endohedral fullerene (N@C{sub 60}) has been synthesized by controlling the plasma ion irradiation energy (E{sub i}) and fullerene (C{sub 60}) behavior in the sublimation phase. We examined the relationship between the synthesis purity of N@C{sub 60} [molar concentration ratio of N@C{sub 60} to pristine fullerene (C{sub 60})] and E{sub i}, which was controlled by changing the substrate bias voltages (V{sub sub}) and gas pressure (P{sub N2}) during the plasma irradiation process. High-density nitrogen-molecular ions (N{sub 2}{sup +}) with a suitable E{sub i} near 80 eV are confirmed to be the optimum condition of the nitrogen plasma for themore » synthesis of high-purity N@C{sub 60}. In addition, high sublimation of C{sub 60} contributes to a higher yield due to the high internal energy of C{sub 60} and the related cage defects that are present under these conditions. As a result, a purity of 0.83% is realized for the first time, which is almost two orders of magnitude higher than that using other methods.« less

Enantioselective ultra high performance liquid and supercritical fluid chromatography: The race to the shortest chromatogram.

PubMed

Ciogli, Alessia; Ismail, Omar H; Mazzoccanti, Giulia; Villani, Claudio; Gasparrini, Francesco

2018-03-01

The ever-increasing need for enantiomerically pure chiral compounds has greatly expanded the number of enantioselective separation methods available for the precise and accurate measurements of the enantiomeric purity. The introduction of chiral stationary phases for liquid chromatography in the last decades has revolutionized the routine methods to determine enantiomeric purity of chiral drugs, agrochemicals, fragrances, and in general of organic and organometallic compounds. In recent years, additional efforts have been placed on faster, enantioselective analytical methods capable to fulfill the high throughput requirements of modern screening procedures. Efforts in this field, capitalizing on improved chromatographic particle technology and dedicated instrumentation, have led to highly efficient separations that are routinely completed on the seconds time scale. An overview of the recent achievements in the field of ultra-high-resolution chromatography on column packed with chiral stationary phases, both based on sub-2 μm fully porous and sub-3 μm superficially porous particles, will be given, with an emphasis on very recent studies on ultrafast chiral separations. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel method for the determination of chemical purity and assay of menaquinone-7. Comparison with the methods from the official USP monograph.

PubMed

Jedynak, Łukasz; Jedynak, Maria; Kossykowska, Magdalena; Zagrodzka, Joanna

2017-02-20

An HPLC method with UV detection and separation with the use of a C30 reversed phase analytical column for the determination of chemical purity and assay of menaquinone-7 (MK7) in one chromatographic run was developed. The method is superior to the methods published in the USP Monograph in terms of selectivity, sensitivity and accuracy, as well as time, solvent and sample consumption. The developed methodology was applied to MK7 samples of active pharmaceutical ingredient (API) purity, MK7 samples of lower quality and crude MK7 samples before purification. The comparison of the results revealed that the use of USP methodology could lead to serious overestimation (up to a few percent) of both purity and MK7 assay in menaquinone-7 samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Tumor purity and differential methylation in cancer epigenomics.

PubMed

Wang, Fayou; Zhang, Naiqian; Wang, Jun; Wu, Hao; Zheng, Xiaoqi

2016-11-01

DNA methylation is an epigenetic modification of DNA molecule that plays a vital role in gene expression regulation. It is not only involved in many basic biological processes, but also considered an important factor for tumorigenesis and other human diseases. Study of DNA methylation has been an active field in cancer epigenomics research. With the advances of high-throughput technologies and the accumulation of enormous amount of data, method development for analyzing these data has gained tremendous interests in the fields of computational biology and bioinformatics. In this review, we systematically summarize the recent developments of computational methods and software tools in high-throughput methylation data analysis with focus on two aspects: differential methylation analysis and tumor purity estimation in cancer studies. © The Author 2016. Published by Oxford University Press. All rights reserved. For permissions, please email: journals.permissions@oup.com.

Jerusalem artichoke powder: a useful material in producing high-optical-purity l-lactate using an efficient sugar-utilizing thermophilic Bacillus coagulans strain.

PubMed

Wang, Limin; Xue, Zhangwei; Zhao, Bo; Yu, Bo; Xu, Ping; Ma, Yanhe

2013-02-01

Jerusalem artichoke is a low-requirement crop, which does not interfere with food chain, and is a promising carbon source for industrial fermentation. Microbial conversion of such a renewable raw material to useful products, such as lactic acid, is an important objective in industrial biotechnology. In this study, high-optical-purity l-lactate was efficiently produced from the hydrolysates of Jerusalem artichoke powder by a thermophilic bacterium, Bacillus coagulans XZL4. High l-lactate production (134gl(-1)) was obtained using 267gl(-1) Jerusalem artichoke powder (total reducing sugars of 140gl(-1)) and 10gl(-1) of corn steep powder in fed-batch fermentation, with an average productivity of 2.5gl(-1)h(-1) and a yield of 0.96gg(-1) reducing sugars. The final product optical purity is 99%, which meets the requirement of lactic acid polymerization. Our study represents a cost-effective and promising method for polymer-grade l-lactate production using a cheap raw bio-resource. Copyright © 2012 Elsevier Ltd. All rights reserved.

Use of Electrodeposition for Sample Preparation and Rejection Rate Prediction for Assay of Electroformed Ultra High Purity Copper for 232Th and 238U Prior to Inductively Coupled Plasma Mass Spectrometry (ICP/MS)

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

Hoppe, Eric W.; Aalseth, Craig E.; Brodzinski, Ronald L.

The search for neutrinoless double beta decay in 76Ge has driven the need for ultra-low background Ge detectors shielded by electroformed copper of ultra-high radiopurity (<0.1µBq/kg). Although electrodeposition processes are almost sophisticated enough to produce copper of this purity, to date there are no methods sensitive enough to assay it. Inductively-coupled plasma mass spectrometry (ICP/MS) can detect thorium and uranium at femtogram levels, but in the past, this assay has been hindered by high copper concentrations in the sample. Electrodeposition of copper samples removes copper from the solution while selectively concentrating thorium and uranium contaminants to be assayed by ICP/MS.more » Spiking 232Th and 238U into the plating bath simulates low purity copper and allows for the calculation of the electrochemical rejection rate of thorium and uranium in the electroplating system. This rejection value will help to model plating bath chemistry.« less

Varied morphology carbon nanotubes and method for their manufacture

DOEpatents

Li, Wenzhi; Wen, Jian Guo; Ren, Zhi Feng

2007-01-02

The present invention describes the preparation of carbon nanotubes of varied morphology, catalyst materials for their synthesis. The present invention also describes reactor apparatus and methods of optimizing and controlling process parameters for the manufacture carbon nanotubes with pre-determined morphologies in relatively high purity and in high yields. In particular, the present invention provides methods for the preparation of non-aligned carbon nanotubes with controllable morphologies, catalyst materials and methods for their manufacture.

High-purity silica reflecting heat shield development

NASA Technical Reports Server (NTRS)

Congdon, W. M.

1974-01-01

A high-purity, fused-silica reflecting heat shield for the thermal protection of outer-planet probes was developed. Factors that strongly influence the performance of a silica heat shield were studied. Silica-bonded silica configurations, each prepared by a different technique, were investigated and rated according to its relative merits. Slip-casting was selected as the preferred fabrication method because it produced good reflectivity and good strength, and is relatively easy to scale up for a full-size outer-planet probe. The slips were cast using a variety of different particle sizes: continuous particle-size slips; monodisperse particle-size slips; and blends of monodisperse particle-size slips were studied. In general, smaller particles gave the highest reflectance. The monodisperse slips as well as the blend slips gave a higher reflectance than the continuous particle-size slips. An upgraded and fused natural quartz was used to study the effects of microstructure on reflectance and as the baseline to ascertain the increase in reflectance obtained from using a higher-purity synthetic material.

Preparation and characterization of (10)B boric acid with high purity for nuclear industry.

PubMed

Zhang, Weijiang; Liu, Tianyu; Xu, Jiao

2016-01-01

Boric acid is often added into coolant as neutron capture agent for pressurized water reactor, whose amount is influenced by its abundance and purity. Therefore, the preparation of enriched (10)B boric acid with high purity is beneficial to nuclear industry. (10)B is also used in developing tumor-specific boronated drugs in boron neutron capture therapy. The boronated drug can be administered to patient intravenously, intratumorally, or deposited at tumor site in surgical excision. Thus, enriched (10)B boric acid is of practical significance in the field of medicine. Self-made boron trifluoride-methanol-complex solution was selected as one of the experimental reagents, and the preparation of (10)B acid was realized by one-step reaction for the complexes with water and calcium chloride. The determination of electrical conductivity in reaction process proves that the optimum reaction time was 16-20 h. Furthermore, the effect of reaction time, ratio of calcium chloride to complex as well as the amount of water on the purity and yield of boric acid was investigated. Finally, the optimum reaction time was 20 h, the optimal solid-liquid ratio (molar ratio) was 3:1, and the amount of water was 1 L of deionized water for each mol of the complex. H2O2 was added in the reaction process to remove Fe(2+). After recrystallization, IR spectra of (10)B boric acid was measured and compared with standard to verify the product of boric acid. The feasibility of the preparation method was determined by the detection of XRD of boric acid. To observe the morphology by polarizing microscope, crystal structure was obtained. The purity of the final product is 99.95 %, and the yield is 96.47 %. The ion concentration of boric acid accords with the national standard of high purity, which was determined by ICP.

High-Purity Glasses Based on Arsenic Chalcogenides

DTIC Science & Technology

2001-06-01

Chemical interaction of chalcogenides and some impurities (CS 2, TeO2 ) with the quartz glass at high temperature leads to the thin layers formation...UNCLASSIFIED Defense Technical Information Center Compilation Part Notice ADPO1 1523 TITLE: High-Purity Glasses Based on Arsenic Chalcogenides...Materials Vol. 3, No. 2, June 2001, p. 341 - 349 HIGH-PURITY GLASSES BASED ON ARSENIC CHALCOGENIDES M. F. Churbanov, I. V. Scripachev, G. E. Snopatin, V. S

Method for nuclear magnetic resonance imaging using deuterum as a contrast agent

DOEpatents

Kehayias, Joseph J.; Joel, Darrel D.; Adams, William H.; Stein, Harry L.

1990-01-01

A method for in vivo NMR imaging of the blood vessels and organs of a patient characterized by using a dark dye-like imaging substance consisting essentially of a stable, high-purity concentration of D.sub.2 O in a solution with water.

Comparison of methods for extracting kafirin proteins from sorghum distillers dried grains with solubles.

PubMed

Wang, Ying; Tilley, Michael; Bean, Scott; Sun, X Susan; Wang, Donghai

2009-09-23

Use of coproducts generated during fermentation is important to the overall economics of biofuel production. The main coproduct from grain-based ethanol production is distillers dried grains with solubles (DDGS). High in protein, DDGS is a potential source of protein for many bioindustrial applications such as adhesives and resins. The objective of this research was to characterize the composition as well as chemical and physical properties of kafirin proteins from sorghum DDGS with various extraction methods including use of acetic acid, HCl-ethanol and NaOH-ethanol under reducing conditions. Extraction conditions affected purity and thermal properties of the extracted kafirin proteins. Extraction yields of 44.2, 24.2, and 56.8% were achieved by using acetic acid, HCl-ethanol and NaOH-ethanol, respectively. Acetic acid and NaOH-ethanol produced protein with higher purity than kafirins extracted with the HCl-ethanol protocol. The acetic acid extraction protocol produced protein with the highest purity, 98.9%. Several techniques were used to evaluate structural, molecular and thermal properties of kairin extracts. FTIR showed alpha-helix dominated in all three samples, with only a small portion of beta-sheet present. Electrophoresis results showed alpha(1), alpha(2) band and beta kafirins were present in all three extracts. Glass transition peaks of the extracts were shown by DSC to be approximately 230 degrees C. Kafirin degraded at 270-290 degrees C. Size exclusion chromatography revealed that the acetic acid and HCl-ethanol based extraction methods tended to extract more high molecular weight protein than the NaOH-ethanol based method. Reversed phase high-performance liquid chromatography showed that the gamma kafirins were found only in extracts from the NaOH-ethanol extraction method.

Accurate determination of non-metallic impurities in high purity tetramethylammonium hydroxide using inductively coupled plasma tandem mass spectrometry

NASA Astrophysics Data System (ADS)

Fu, Liang; Xie, Hualin; Shi, Shuyun; Chen, Xiaoqing

2018-06-01

The content of non-metallic impurities in high-purity tetramethylammonium hydroxide (HPTMAH) aqueous solution has an important influence on the yield, electrical properties and reliability of the integrated circuit during the process of chip etching and cleaning. Therefore, an efficient analytical method to directly quantify the content of non-metallic impurities in HPTMAH aqueous solutions is necessary. The present study was aimed to develop a novel method that can accurately determine seven non-metallic impurities (B, Si, P, S, Cl, As, and Se) in an aqueous solution of HPTMAH by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS). The samples were measured using a direct injection method. In the MS/MS mode, oxygen and hydrogen were used as reaction gases in the octopole reaction system (ORS) to eliminate mass spectral interferences during the analytical process. The detection limits of B, Si, P, S, Cl, As, and Se were 0.31, 0.48, 0.051, 0.27, 3.10, 0.008, and 0.005 μg L-1, respectively. The samples were analyzed by the developed method and the sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) was used for contrastive analysis. The values of these seven elements measured using ICP-MS/MS were consistent with those measured by SF-ICP-MS. The proposed method can be utilized to analyze non-metallic impurities in HPTMAH aqueous solution. Table S2 Multiple potential interferences on the analytes. Table S3 Parameters of calibration curve and the detection limit (DL). Table S4 Results obtained for 25% concentration high-purity grade TMAH aqueous solution samples (μg L-1, mean ± standard deviation, n = 10).

A simple-rapid method to separate uranium, thorium, and protactinium for U-series age-dating of materials.

PubMed

Knight, Andrew W; Eitrheim, Eric S; Nelson, Andrew W; Nelson, Steven; Schultz, Michael K

2014-08-01

Uranium-series dating techniques require the isolation of radionuclides in high yields and in fractions free of impurities. Within this context, we describe a novel-rapid method for the separation and purification of U, Th, and Pa. The method takes advantage of differences in the chemistry of U, Th, and Pa, utilizing a commercially-available extraction chromatographic resin (TEVA) and standard reagents. The elution behavior of U, Th, and Pa were optimized using liquid scintillation counting techniques and fractional purity was evaluated by alpha-spectrometry. The overall method was further assessed by isotope dilution alpha-spectrometry for the preliminary age determination of an ancient carbonate sample obtained from the Lake Bonneville site in western Utah (United States). Preliminary evaluations of the method produced elemental purity of greater than 99.99% and radiochemical recoveries exceeding 90% for U and Th and 85% for Pa. Excellent purity and yields (76% for U, 96% for Th and 55% for Pa) were also obtained for the analysis of the carbonate samples and the preliminary Pa and Th ages of about 39,000 years before present are consistent with (14)C-derived age of the material. Copyright © 2014 Elsevier Ltd. All rights reserved.

Analysis of trace halocarbon contaminants in ultra high purity helium

NASA Technical Reports Server (NTRS)

Fewell, Larry L.

1994-01-01

This study describes the analysis of ultra high purity helium. Purification studies were conducted and containment removal was effected by the utilization of solid adsorbent purge-trap systems at cryogenic temperatures. Volatile organic compounds in ultra high purity helium were adsorbed on a solid adsorbent-cryogenic trap, and thermally desorbed trace halocarbon and other contaminants were analyzed by combined gas chromatography-mass spectrometry.

SEPARATION OF THE MINOR FLAVONOLS FROM FLOS GOSSYPII BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY

PubMed Central

Yang, Yi; Zhao, Yongxin; Gu, Dongyu; Ayupbek, Amatjan; Huang, Yun; Dou, Jun; Ito, Yoichiro; Zhang, Tianyou; Aisa, Haji Akber

2010-01-01

An effective high-speed countercurrent chromatography (HSCCC) method was established for further separation and purification of four minor flavonols in addition to five major flavonols which were reported by our previous study from extracts of Flos Gossypii. HSCCC was performed with three two-phase solvent systems composed of n-hexane-ethyl acetate-methanol-water (7.5:15:6:7, v/v), (2.5:15:2:7, v/v) and (0:1:0:1, v/v). The separation was repeated 3 times, and 3.8 mg of 8-methoxyl-kaempferol-7-O-β-D-rhamnoside (HPLC purity 98.27%), 6.7 mg of astragalin (HPLC purity 94.18%), 3.3 mg of 4′-methoxyl-quercetin-7-O-β-D-glucoside (HPLC purity 94.30%) and 8.2 mg of hyperoside (HPLC purity 93.48%) were separated from 150 mg of the crude sample. The chemical structures of the flavonols were confirmed by MS, 1H NMR and 13C NMR. Meanwhile, the results indicated that the target compound with smaller K value (<0.5) can be separated by increasing column length of HSCCC. And four separation rules of flavonols according to the present study and references were summarized, which can be used as a useful guide for separation of flavonols by HSCCC. PMID:21494318

Influence of solvents on the changes in structure, purity, and in vitro characteristics of green-synthesized ZnO nanoparticles from Costus igneus

NASA Astrophysics Data System (ADS)

Nandhini, G.; Suriyaprabha, R.; Maria Sheela Pauline, W.; Rajendran, V.; Aicher, Wilhelm Karl; Awitor, Oscar Komla

2018-05-01

The present study is intended to produce high-purity zinc oxide nanoparticles from the leaves of Costus igneus and zinc acetate precursor via sustainable methods by the tribulation with three different solvents (hot water, methanol, and acetone) for the extraction of plant compounds. While examining the physico-chemical characteristics of ZnO nanoparticles incurred by the catalysis of plant bioactive compounds extracted from different solvents, the hot water extract-based green synthesis process yields higher purity (99.89%) and smaller particle size (94 nm) than other solvents. The optimization of the solvents used for the green synthesis of nanoparticles renders key identification in appropriate extraction of bioactive compounds suitable for the nucleation/production of nanoparticles in addition to annealing temperature. The impregnable usage of ZnO nanoparticles in clinical applications is further confirmed based on the treatment of particles (1-10 mg ml-1) against Gram-positive (S. aureus and S. epidermis) and Gram-negative bacteria (E. coli and K. pneumoniae) with respect to their growth inhibition. An in-force growth inhibition against particular S. aureus and S. epidermis imparted by the low concentration of ZnO nanoparticles signifies the utilization and consumption of green-synthesized high-purity nanoparticles for therapeutic and cosmetic applications.

Irradiation-induced sensitization and stress corrosion cracking of Type 304 stainless steel core-internal components

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

Chung, H.M.; Ruther, W.E.; Sanecki, J.E.

1991-08-01

High- and commercial-purity heats of Type 304 stainless steel, obtained from neutron absorber tubes after irradiation to fluence levels of up to 2 {times} 10{sup 21} n{center dot}cm{sup {minus}2} (E > 1 MeV) in two boiling water reactors, were examined by Auger electron spectroscopy to characterize irradiation-induced grain- boundary segregation and depletion of alloying and impurity elements. Segregation of Si, P, Ni, and an unidentified element or compound that gives rise to an Auger energy peak at 59 eV was observed in the commercial-purity heat. Such segregation was negligible in high-purity material, except for Ni. No evidence of S segregationmore » was observed in either material. Cr depletion was more pronounced in the high-purity material than in the commercial-purity material. These observations suggest a synergism between the significant level of impurities and Cr depletion in the commercial-purity heat. In the absence of such synergism, Cr depletion appears more pronounced in the high-purity heat. Initial results of constant-extension-rate tests conducted on the two heats in air an in simulated BWR water were correlated with the results from analysis by Auger electron spectroscopy. 15 refs., 10 figs.« less

Direct high-performance liquid chromatographic determination of the enantiomeric purity of levodopa and methyldopa: comparison with pharmacopoeial polarimetric methods.

PubMed

Dolezalová, M; Tkaczyková, M

1999-03-01

Chiral high-performance liquid chromatography was employed for determination of the enantiomeric purity of levodopa and methyldopa. The determination of D-DOPA in levodopa was accomplished using a chiral ligand-exchange chromatograpy with an ordinary C18 column and a chiral mobile phase containing N,N-dimethyl-L-phenylalanine and Cu(II) acetate or by means of LC on a teicoplanin column in conjunction with ethanol-water (65:35, v/v). Both methods gave good performance, however, the latter was faster and more convenient and suitable for routine analyses. For the determination of D-methyldopa a LC method based on the use of a teicoplanin column in polar organic mode with methanol-acetic acid-triethylamine (1,000:0.05:0.05, v/v/v) mobile phase was developed. The precision, accuracy, linearity and selectivity were satisfactory. In comparison with pharmacopoeial polarimetric methods (according to the European Pharmacopoeia and the Pharmacopoea Bohemoslovaca), the LC methods proved to be much more sensitive giving detection limits 0.04% of D-DOPA and 0.3% of D-methyldopa.

Technology for High Pure Aluminum Oxide Production from Aluminum Scrap

NASA Astrophysics Data System (ADS)

Ambaryan, G. N.; Vlaskin, M. S.; Shkolnikov, E. I.; Zhuk, A. Z.

2017-10-01

In this study a simple ecologically benign technology of high purity alumina production is presented. The synthesis process consists of three steps) oxidation of aluminum in water at temperature of 90 °C) calcinations of Al hydroxide in atmosphere at 1100 °C) high temperature vacuum processing of aluminum alpha oxide at 1750 °C. Oxidation of aluminum scrap was carried out under intensive mixing in water with small addition of KOH as a catalyst. It was shown that under implemented experimental conditions alkali was continuously regenerated during oxidation reaction and synergistic effect of low content alkali aqueous solution and intensive mixing worked. The product of oxidation of aluminum scrap is the powder of Al(OH)3. Then it can be preliminary granulated or directly subjected to thermal treatment deleting the impurities from the product (aluminum oxide). It was shown the possibility to produce the high-purity aluminum oxide of 5N grade (99.999 %). Aluminum oxide, synthesized by means of the proposed method, meets the requirements of industrial manufacturers of synthetic sapphire (aluminum oxide monocrystals). Obtained high pure aluminum oxide can be also used for the manufacture of implants, artificial joints, microscalpels, high-purity ceramics and other refractory shapes for manufacture of ultra-pure products.

Comparative analysis of protocols for DNA extraction from soybean caterpillars.

PubMed

Palma, J; Valmorbida, I; da Costa, I F D; Guedes, J V C

2016-04-07

Genomic DNA extraction is crucial for molecular research, including diagnostic and genome characterization of different organisms. The aim of this study was to comparatively analyze protocols of DNA extraction based on cell lysis by sarcosyl, cetyltrimethylammonium bromide, and sodium dodecyl sulfate, and to determine the most efficient method applicable to soybean caterpillars. DNA was extracted from specimens of Chrysodeixis includens and Spodoptera eridania using the aforementioned three methods. DNA quantification was performed using spectrophotometry and high molecular weight DNA ladders. The purity of the extracted DNA was determined by calculating the A260/A280 ratio. Cost and time for each DNA extraction method were estimated and analyzed statistically. The amount of DNA extracted by these three methods was sufficient for PCR amplification. The sarcosyl method yielded DNA of higher purity, because it generated a clearer pellet without viscosity, and yielded high quality amplification products of the COI gene I. The sarcosyl method showed lower cost per extraction and did not differ from the other methods with respect to preparation times. Cell lysis by sarcosyl represents the best method for DNA extraction in terms of yield, quality, and cost effectiveness.

Analysis of optical purity and impurity of synthetic D-phenylalanine products using sulfated beta-cyclodextrin as chiral selector by reversed-polarity capillary electrophoresis.

PubMed

Zhao, Yan; Yang, Xing-Bin; Jiang, Ru; Sun, Xiao-Li; Li, Xiao-Ye; Liu, Wen-Min; Zhang, Sheng-Yong

2006-02-01

A new capillary electrophoresis (CE) method has been achieved for simultaneous separation and quantification of phenylalanine, N-acetylphenylalanine enantiomers, and prochiral N-acetylaminocinnamic acid, possibly co-existent in reaction systems or synthesized products of D-phenylalanine. The separation was carried out in an uncoated capillary under reversed-electrophoretic mode. Among the diverse charged cyclodextrins (CDs) examined, highly sulfated (HS)-beta-CD as the chiral selector exhibited the best enantioselectivity. The complete separation of the analytes was obtained under the optimum conditions of pH 2.5, 35 mM Tris buffer containing 4% HS-beta-CD, applied voltage -15 kV, and capillary temperature 25 degrees C. Furthermore, the proposed method was applied to the determination of optical purity and trace impurities in three batches of the asymmetric synthetic samples of D-phenylalanine, and satisfactory results were obtained. The determination recoveries of the samples were in the range of 97.8-103.8%, and precisions fell within 2.3-5.0% (RSD). The results demonstrate that this CE method is a useful, simple technique and is applicable to purity assays of D-phenylalanine. (c) 2005 Wiley-Liss, Inc.

One-step isolation of γ-oryzanol from rice bran oil by non-aqueous hydrostatic countercurrent chromatography.

PubMed

Angelis, Apostolis; Urbain, Aurélie; Halabalaki, Maria; Aligiannis, Nektarios; Skaltsounis, Alexios-Leandros

2011-09-01

The value-added γ-oryzanol was purified in one step from crude rice bran oil (RBO) using a preparative hydrostatic countercurrent chromatography (hydrostatic CCC) method, operating in the dual mode. The fractionation was performed using a non-aqueous biphasic solvent system consisting of heptane-acetonitrile-butanol (1.8:1.4:0.7, v/v/v), leading rapidly to the target compounds. Transfer of the analytical CCC method to large-scale isolation was also carried out yielding a high quantity-high purity fraction of γ-oryzanol. In addition, a fraction of hydroxylated triterpene alcohol ferulates (polar γ-oryzanol) was clearly separated and obtained. Furthermore, a fast HPLC-APCI(±)-HRMS method was developed and applied for the identification of γ-oryzanol as well as the polar γ-oryzanol in RBO and the resulting fractions. The purity of γ-oryzanol fraction was estimated as 97% based on HPLC-APCI-HRMS analysis. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Purification of lignans from Fructus Arctii using off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography.

PubMed

Yang, Bichao; Xin, Huaxia; Wang, Feier; Cai, Jianfeng; Liu, Yanfang; Fu, Qing; Jin, Yu; Liang, Xinmiao

2017-08-01

As a common traditional Chinese medicine, Fructus Arctii has important clinical medical values. Its main components are lignans, which are difficult to separate and analyze because of the complex composition, similar chemical structures, and close properties. In this study, an off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method, as well as an effective sample pretreatment method based on hydrophilic interaction chromatography material, was developed to enrich the minor lignan fractions and obtain high-purity compounds. In total, 12 high-purity compounds were isolated from Fructus Arctii. Their structures were identified by using high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy, which showed that all were lignans and that most of them were isomers. The results demonstrated the effective off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method for the purification of lignans from Fructus Arctii. The separation protocol established here will be beneficial for the separation of complex samples from other kinds of natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel electroless method to prepare a platinum electrocatalyst on diamond for fuel cell applications

NASA Astrophysics Data System (ADS)

Lyu, Xiao; Hu, Jingping; Foord, John S.; Wang, Qiang

2013-11-01

A novel electroless deposition method was demonstrated to prepare a platinum electrocatalyst on boron doped diamond (BDD) substrates without the need for pre-activation. This green method addresses the uniformity and particle size issues associated with electrodeposition and circumvents the pre-activation procedure which is necessary for conventional electroless deposition. The inert BDD substrate formed a galvanic couple with an iron wire, to overcome the activation barrier associated with conventional electroless deposition on diamond, leading to the formation of Pt nanoparticles on the electrode surface in a galvanic process coupled to a chemical process. When sodium hypophosphite was employed as the reducing agent to drive the electroless reaction Pt deposits which were contaminated with iron and phosphorus resulted. In contrast, the reducing agent ascorbic acid gave rise to high purity Pt nanoparticles. Optimal deposition conditions with respect to bath temperature, pH value and stabilizing additives are identified. Using this approach, high purity and uniformly distributed platinum nanoparticles are obtained on the diamond electrode surface, which demonstrate a high electrochemical activity towards methanol oxidation.

High-Purity Semiconducting Single-Walled Carbon Nanotubes: A Key Enabling Material in Emerging Electronics.

PubMed

Lefebvre, Jacques; Ding, Jianfu; Li, Zhao; Finnie, Paul; Lopinski, Gregory; Malenfant, Patrick R L

2017-10-17

Semiconducting single-walled carbon nanotubes (sc-SWCNTs) are emerging as a promising material for high-performance, high-density devices as well as low-cost, large-area macroelectronics produced via additive manufacturing methods such as roll-to-roll printing. Proof-of-concept demonstrations have indicated the potential of sc-SWCNTs for digital electronics, radiofrequency circuits, radiation hard memory, improved sensors, and flexible, stretchable, conformable electronics. Advances toward commercial applications bring numerous opportunities in SWCNT materials development and characterization as well as fabrication processes and printing technologies. Commercialization in electronics will require large quantities of sc-SWCNTs, and the challenge for materials science is the development of scalable synthesis, purification, and enrichment methods. While a few synthesis routes have shown promising results in making near-monochiral SWCNTs, gram quantities are available only for small-diameter sc-SWCNTs, which underperform in transistors. Most synthesis routes yield mixtures of SWCNTs, typically 30% metallic and 70% semiconducting, necessitating the extraction of sc-SWCNTs from their metallic counterparts in high purity using scalable postsynthetic methods. Numerous routes to obtain high-purity sc-SWCNTs from raw soot have been developed, including density-gradient ultracentrifugation, chromatography, aqueous two-phase extraction, and selective DNA or polymer wrapping. By these methods (termed sorting or enrichment), >99% sc-SWCNT content can be achieved. Currently, all of these approaches have drawbacks and limitations with respect to electronics applications, such as excessive dilution, expensive consumables, and high ionic impurity content. Excess amount of dispersant is a common challenge that hinders direct inclusion of sc-SWCNTs into electronic devices. At present, conjugated polymer extraction may represent the most practical route to sc-SWCNTs. By the use of polymers with a π-conjugated backbone, sc-SWCNTs with >99.9% purity can be dispersed in organic solvents via a simple sonication and centrifugation process. With 1000 times less excipient and the flexibility to accommodate a broad range of solvents via diverse polymer constructs, inks are readily deployable in solution-based fabrication processes such as aerosol spray, inkjet, and gravure. Further gains in sc-SWCNT purity, among other attributes, are possible with a better understanding of the structure-property relationships that govern conjugated polymer extraction. This Account covers three interlinked topics in SWCNT electronics: metrology, enrichment, and SWCNT transistors fabricated via solution processes. First, we describe how spectroscopic techniques such as optical absorption, fluorescence, and Raman spectroscopy are applied for sc-SWCNT purity assessment. Stringent requirements for sc-SWCNTs in electronics are pushing the techniques to new levels while serving as an important driver toward the development of quantitative metrology. Next, we highlight recent progress in understanding the sc-SWCNT enrichment process using conjugated polymers, with special consideration given to the effect of doping on the mechanism. Finally, developments in sc-SWCNT-based electronics are described, with emphasis on the performance of transistors utilizing random networks of sc-SWCNTs as the semiconducting channel material. Challenges and advances associated with using polymer-based dielectrics in the unique context of sc-SWCNT transistors are presented. Such transistor packages have enabled the realization of fully printed transistors as well as transparent and even stretchable transistors as a result of the unique and excellent electrical and mechanical properties of sc-SWCNTs.

Separation and purification of astaxanthin from Phaffia rhodozyma by preparative high-speed counter-current chromatography.

PubMed

Du, Xiping; Dong, Congcong; Wang, Kai; Jiang, Zedong; Chen, Yanhong; Yang, Yuanfan; Chen, Feng; Ni, Hui

2016-09-01

An effective high-speed counter-current chromatography (HSCCC) method was established for the preparative isolation and purification of astaxanthin from Phaffia rhodozyma. With a two-phase solvent system composed of n-hexane-acetone-ethanol-water (1:1:1:1, v/v/v/v), 100mg crude extract of P. rhodozyma was separated to yield 20.6mg of astaxanthin at 92.0% purity. By further one step silica gel column chromatography, the purity reached 99.0%. The chemical structure of astaxanthin was confirmed by thin layer chromatography (TLC), UV spectroscopy scanning, high performance liquid chromatography with a ZORBAX SB-C18 column and a Waters Nova-pak C18 column, and ESI/MS/MS. Copyright © 2016 Elsevier B.V. All rights reserved.

The Chemistry of Ultra-Radiopure Materials

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

Miley, Harry S.; Aalseth, Craig E.; Day, Anthony R.

Ultra-pure materials are needed for the construction of the next generation of ultra-low level radiation detectors. These detectors are used for environmental research as well as rare nuclear decay experiments, e.g. probing the effective mass and character of the neutrino. Unfortunately, radioactive isotopes are found in most construction materials, either primordial isotopes, activation/spallation products from cosmic-ray exposure, or surface deposition of dust or radon progeny. Copper is an ideal candidate material for these applications. High-purity copper is commercially available and, when even greater radiopurity is needed, additional electrochemical purification can be combined with the final construction step, resulting in “electroformed”more » copper of extreme purity. Copper also offers desirable thermal, mechanical, and electrical properties. To bridge the gap between commercially-available high purity copper and the most stringent requirements of next-generation low-background experiments, a method of additional chemical purification is being developed based on well-known copper electrochemistry. This method is complemented with the co-development of surface cleaning techniques and more sensitive assay for both surface and bulk contamination. Developments in the electroplating of copper, surface cleaning, assay of U and Th in the bulk copper, and residual surface contamination will be discussed relative to goals of less than 1 microBq/kg Th.« less

Simultaneous Separation of Actinium and Radium Isotopes from a Proton Irradiated Thorium Matrix

DOE PAGES

Mastren, Tara; Radchenko, Valery; Owens, Allison; ...

2017-08-15

A new method has been developed for the isolation of 223,224,225Ra, in high yield and purity, from a proton irradiated 232Th matrix. We report an all-aqueous process using multiple solid-supported adsorption steps including a citrate chelation method developed to remove >99.9% of the barium contaminants by activity from the final radium product. Moreover, we developed a procedure involving the use of three columns in succession, and the separation of 223,224,225Ra from the thorium matrix was obtained with an overall recovery yield of 91 ± 3%, average radiochemical purity of 99.9%, and production yields that correspond to physical yields based onmore » previously measured excitation functions.« less

Isolation of Chromoplasts and Suborganellar Compartments from Tomato and Bell Pepper Fruit.

PubMed

Barsan, Cristina; Kuntz, Marcel; Pech, Jean-Claude

2017-01-01

Tomato is a model for fruit development and ripening. The isolation of intact plastids from this organism is therefore important for metabolic and proteomic analyses. Pepper, a species from the same family, is also of interest since it allows isolation of intact chromoplasts in large amounts. Here, we provide a detailed protocol for the isolation of tomato plastids at three fruit developmental stages, namely, nascent chromoplasts from the mature green stage, chromoplasts from an intermediate stage, and fully differentiated red chromoplasts. The method relies on sucrose density gradient centrifugations. It yields high purity organelles suitable for proteome analyses. Enzymatic and microscopy assays are summarized to assess purity and intactness. A method is also described for subfractionation of pepper chromoplast lipoprotein structures.

Improving the efficiency of quantitative (1)H NMR: an innovative external standard-internal reference approach.

PubMed

Huang, Yande; Su, Bao-Ning; Ye, Qingmei; Palaniswamy, Venkatapuram A; Bolgar, Mark S; Raglione, Thomas V

2014-01-01

The classical internal standard quantitative NMR (qNMR) method determines the purity of an analyte by the determination of a solution containing the analyte and a standard. Therefore, the standard must meet the requirements of chemical compatibility and lack of resonance interference with the analyte as well as a known purity. The identification of such a standard can be time consuming and must be repeated for each analyte. In contrast, the external standard qNMR method utilizes a standard with a known purity to calibrate the NMR instrument. The external standard and the analyte are measured separately, thereby eliminating the matter of chemical compatibility and resonance interference between the standard and the analyte. However, the instrumental factors, including the quality of NMR tubes, must be kept the same. Any deviations will compromise the accuracy of the results. An innovative qNMR method reported herein utilizes an internal reference substance along with an external standard to assume the role of the standard used in the traditional internal standard qNMR method. In this new method, the internal reference substance must only be chemically compatible and be free of resonance-interference with the analyte or external standard whereas the external standard must only be of a known purity. The exact purity or concentration of the internal reference substance is not required as long as the same quantity is added to the external standard and the analyte. The new method reduces the burden of searching for an appropriate standard for each analyte significantly. Therefore the efficiency of the qNMR purity assay increases while the precision of the internal standard method is retained. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis and morphological examination of high-purity Ca(OH)2 nanoparticles suitable to consolidate porous surfaces

NASA Astrophysics Data System (ADS)

Madrid, Juan Antonio; Lanzón, Marcos

2017-12-01

Adequate synthetic methods to obtain pure Ca(OH)2 nanoparticles are scarcely documented in the literature. This paper presents a complete methodology to obtain highly-pure Ca(OH)2 nanoparticles that are appropriate for strengthening heritage materials. The precipitation synthesis was operated in controlled atmosphere to avoid carbonation by atmospheric CO2. A complete purification method was developed to eliminate the sodium chloride generated in the reaction. Several analytical techniques, such as electrical conductivity, pH, ion chromatography, X-ray diffraction (XRD) and thermogravimetric analysis coupled to mass spectrometry (TGA-MS) were used to analyse both the aqueous medium and solid phase. The amount of material obtained in the synthesis (yield) was quantified throughout the purification procedure. The influence of temperature on the nanoparticles' size and stability was studied by transmission electron microscopy (HRTEM) and sedimentation tests (light scattering). It was found that the synthesis yielded high-purity nanoparticles, whose morphological features were greatly affected by the reaction temperature.

The study on the extraction method of indirubin from Indigo Naturalis.

PubMed

Cheng, Li-hui

2007-01-01

To discuss how to extract the indirubin of the higher purity from Indigo Naturalis. After extracting the indirubin from Indigo Naturalis by acetic ether, compare the separation effect of the extract in Si gel column with that in alumina column. The indirubin in Indigo Naturalis by Si gel column chromatography is chosen. The purity of indirubin is 98.3% after Si gel column chromatography. The indiruhbin of the higher purity was attained by the simple experimental method.

Determination of chemical purity and isotopic composition of natural and carbon-13-labeled arsenobetaine bromide standards by quantitative(1)H-NMR.

PubMed

Le, Phuong-Mai; Ding, Jianfu; Leek, Donald M; Mester, Zoltan; Robertson, Gilles; Windust, Anthony; Meija, Juris

2016-10-01

In this study, we report the characterization of three arsenobetaine-certified reference materials by quantitative NMR. We have synthesized an arsenobetaine bromide high-purity standard of natural isotopic composition (ABET-1) and two carbon-13-labeled isotopic standards (BBET-1 and CBET-1). Assignments of the chemical purity and isotopic composition are not trivial in the case of arsenobetaine, and in this study we utilized quantitative(1)H-NMR techniques for the determination of the mass fractions (chemical purity). The isotopic purity of all three standards was also assessed by NMR from the carbon-13 satellite signals. The standards are non-hygroscopic, high-purity (ca. 0.99 g/g), and the carbon-13 enrichment for both isotopic standards is x((13)C)≈0.99. These standards are designed for use as primary calibrators for mass spectrometric determination of arsenobetaine in environmental samples.

Delta Doping High Purity CCDs and CMOS for LSST

NASA Technical Reports Server (NTRS)

Blacksberg, Jordana; Nikzad, Shouleh; Hoenk, Michael; Elliott, S. Tom; Bebek, Chris; Holland, Steve; Kolbe, Bill

2006-01-01

A viewgraph presentation describing delta doping high purity CCD's and CMOS for LSST is shown. The topics include: 1) Overview of JPL s versatile back-surface process for CCDs and CMOS; 2) Application to SNAP and ORION missions; 3) Delta doping as a back-surface electrode for fully depleted LBNL CCDs; 4) Delta doping high purity CCDs for SNAP and ORION; 5) JPL CMP thinning process development; and 6) Antireflection coating process development.

Purity of Vector Vortex Beams through a Birefringent Amplifier

NASA Astrophysics Data System (ADS)

Sroor, Hend; Lisa, Nyameko; Naidoo, Darryl; Litvin, Igor; Forbes, Andrew

2018-04-01

Creating high-quality vector vortex (VV) beams is possible with a myriad of techniques at low power, and while a few studies have produced such beams at high power, none have considered the impact of amplification on the vector purity. Here we employ tools to study the amplification of VV beams and, in particular, the purity of such modes. We outline a versatile toolbox for such investigations and demonstrate its use in the general case of VV beams through a birefringent gain medium. Intriguingly, we show that it is possible to enhance the purity of such beams during amplification, paving the way for high-brightness VV beams, a requirement for their use in high-power applications such as optical communication and laser-enabled manufacturing.

A method for Removing Surface Contamination on Ultra-pure Copper Spectrometer Components

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

Hoppe, Eric W.; Seifert, Allen; Aalseth, Craig E.

Spectrometers for the lowest-level radiometric measurements require materials of extreme radiopurity. Measurements of rare nuclear decays, e.g. neutrinoless double-beta decay, can require construction and shielding materials with bulk radiopurity reaching one micro-Becquerel per kilogram or less. When such extreme material purity is achieved, surface contamination, particularly solid daughters in the natural radon decay chains, can become the limiting background. High-purity copper is an important material for ultra-low-background spectrometers and thus is the focus of this work. A method for removing surface contamination at very low levels without attacking the bulk material is described. An assay method using a low-background proportionalmore » counter made of the material under examination is employed, and the resulting preliminary result of achievable surface contamination levels is presented.« less

Histamine monolith versatility to purify supercoiled plasmid deoxyribonucleic acid from Escherichia coli lysate.

PubMed

Sousa, A; Almeida, A M; Černigoj, U; Sousa, F; Queiroz, J A

2014-08-15

Preparation of high quantities of supercoiled plasmid DNA of pharmaceutical grade purity is a research area where intensive investigation is being performed. From this standpoint, several downstream methods have been proposed, among them the monolithic chromatographic strategies owing to excellent mass transfer properties of monolithic supports and their high binding capacity for large biomolecules. The present study explores the physicochemical properties of histamine ligand in a supercoiled plasmid DNA purification process from an Escherichia coli clarified lysate, where the emphasis is given to the elution strategy that allows higher selectivity and efficient removal of other impurities besides the open circular isoform. The combination of high NaCl concentration and acidic pH allowed the elimination of 89% of RNA during the preparative loading of the lysate sample. The results of the purification strategy with ascending sodium chloride gradient revealed that 97% of supercoiled plasmid DNA was recovered with a purity degree of 99%. In addition, using a combined purification strategy with ascending sodium chloride (capture step) and then descending ammonium sulfate (polishing step) gradient, it was achieved a lower supercoiled plasmid DNA recovery yield of 79% with a purity degree of 92%, although the dynamic binding capacity under these conditions was higher than in the previous strategy. A significant reduction of host contents, such as proteins, RNA and genomic DNA, was obtained in both purification strategies. Accordingly, histamine is a useful and versatile ligand that allows the desirable supercoiled plasmid purification with high yield and purity level. Copyright © 2014. Published by Elsevier B.V.

Zero- and two-dimensional hybrid carbon phosphors for high colorimetric purity white light-emission.

PubMed

Ding, Yamei; Chang, Qing; Xiu, Fei; Chen, Yingying; Liu, Zhengdong; Ban, Chaoyi; Cheng, Shuai; Liu, Juqing; Huang, Wei

2018-03-01

Carbon nanomaterials are promising phosphors for white light emission. A facile single-step synthesis method has been developed to prepare zero- and two-dimensional hybrid carbon phosphors for the first time. Zero-dimensional carbon dots (C-dots) emit bright blue luminescence under 365 nm UV light and two-dimensional nanoplates improve the dispersity and film forming ability of C-dots. As a proof-of-concept application, the as-prepared hybrid carbon phosphors emit bright white luminescence in the solid state, and the phosphor-coated blue LEDs exhibit high colorimetric purity white light-emission with a color coordinate of (0.3308, 0.3312), potentially enabling the successful application of white emitting phosphors in the LED field.

Catalytic dehydrogenation of amine borane complexes

NASA Technical Reports Server (NTRS)

Mohajeri, Nahid (Inventor); Tabatabaie-Raissi, Ali (Inventor)

2007-01-01

A method of generating hydrogen includes the steps of providing an amine borane (AB) complex, at least one hydrogen generation catalyst, and a solvent, and mixing these components. Hydrogen is generated. The hydrogen produced is high purity hydrogen suitable for PEM fuel cells. A hydrolytic in-situ hydrogen generator includes a first compartment that contains an amine borane (AB) complex, a second container including at least one hydrogen generation catalyst, wherein the first or second compartment includes water or other hydroxyl group containing solvent. A connecting network permits mixing contents in the first compartment with contents in the second compartment, wherein high purity hydrogen is generated upon mixing. At least one flow controller is provided for controlling a flow rate of the catalyst or AB complex.

Catalytic dehydrogenation of amine borane complexes

NASA Technical Reports Server (NTRS)

Tabatabaie-Raissi, Ali (Inventor); Mohajeri, Nahid (Inventor); Bokerman, Gary (Inventor)

2009-01-01

A method of generating hydrogen includes the steps of providing an amine borane (AB) complex, at least one hydrogen generation catalyst, and a solvent, and mixing these components Hydrogen is generated. The hydrogen produced is high purity hydrogen suitable for PEM fuel cells. A hydrolytic in-situ hydrogen generator includes a first compartment that contains an amine borane (AB) complex, a second container including at least one hydrogen generation catalyst, wherein the first or second compartment includes water or other hydroxyl group containing solvent. A connecting network permits mixing contents in the first compartment with contents in the second compartment, wherein high purity hydrogen is generated upon mixing. At least one flow controller is provided for controlling a flow rate of the catalyst or AB complex.

Preparative separation of capsaicin and dihydrocapsaicin from Capsicum frutescens by high-speed counter-current chromatography.

PubMed

Peng, Aihua; Ye, Haoyu; Li, Xia; Chen, Lijuan

2009-09-01

Capsaicin and dihydrocapsaicin are two main bioactive components of Capsicum frutescens and are widely used as food additives and drugs in China and India. Due to their similarity in structures, isolation of capsaicin and dihydrocapsaicin with traditional methods such as silica gel column chromatography, normal-phase thin-layer chromatography (TLC) becomes difficult. This study involves separating capsaicin and dihydrocapsaicin with sufficient purity and recovery using high-speed counter-current chromatography (HSCCC) with a solvent system composed of n-hexane-ethyl acetate-methanol-water-acetic acid (20:20:20:20:2, v/v/v/v/v). Separation parameters such as sample volume, and sample concentration were first optimized on analytical HSCCC, and then scaled up to preparative HSCCC. 0.65 g capsaicin and 0.28 g dihydrocapsaicin were obtained from 1.2 g crude extract and their purities were 98.5 and 97.8%, respectively. The recoveries of the two compounds were 86.3 and 85.4%, respectively. The purity of the isolated compounds was analyzed by high-performance liquid chromatography (HPLC) and their structures were identified by (1)H nuclear magnetic resonance (NMR) and (13)C NMR analysis.

APPARATUS FOR HIGH PURITY METAL RECOVERY

DOEpatents

Magel, T.T.

1959-02-10

An apparatus is described for preparing high purity metal such as uranium, plutonium and the like from an impure mass of the same metal. The apparatus is arranged so that the impure metal is heated and swept by a stream of hydrogen gas bearing a halogen such as iodine. The volatiie metal halide formed is carried on to a hot filament where the metal halide is decomposed and the molten high purity metal is collected in a rceeiver below

Measurements and modeling of charge carrier lifetime in compressed xenon

NASA Astrophysics Data System (ADS)

Pudov, A. O.; Abyzov, A. S.; Sokolov, S. A.; Davydov, L. N.; Rybka, A. V.; Kutny, V. E.; Melnikov, S. I.; Kholomyeyev, G. A.; Leonov, S. A.; Turchin, A. A.

2018-06-01

Gamma-spectrometers based on high-pressure xenon gas (HPXe) are proving themselves as a great potential alternative to the spectrometers based on high-purity germanium crystals and scintillators. The working medium for the high-resolution HPXe detectors, that is, xenon gas compressed up to pressure ∼50 bar and sometimes doped with hydrogen, methane or others gases, needs to be of very high purity. The gas purity level can be determined by direct measurements or, alternatively, its usability in gamma-spectrometers can be evaluated indirectly through the charge carrier (electron) lifetime measurements. Different approaches and specific setups have been used for the lifetime determination, most of those methods involve the measurement and analyses of individual pulses from ionizing particles registered in an ionization chamber filled with Xe. In the present paper, we report on the HPXe electron lifetime study carried out by using measurements in a cylindrical ionization chamber and the respective analytical charge transport model. Our results support the possibility of carrier lifetime determination in the cylindrical configuration. In addition, the voltage regimes for the use of the chamber in the spectroscopic mode were determined. The measurements were conducted in a two-electrode configuration for a range of pressure values (5 to 50 bar) for the Xe+0.25%H2 gas mixture of ∼6N purity. It is shown that in gases with relatively high values of the electron drift velocity and the electron lifetime, for example low-density gases, the charge collection time measurements can give significantly underestimated lifetime assessment. On the other hand, for the low drift velocity gases, they give much more accurate results. With the use of the analytical model, the electron lifetime was determined more precisely.

Superconducting radio-frequency cavities made from medium and low-purity niobium ingots

DOE PAGES

Ciovati, Gianluigi; Dhakal, Pashupati; Myneni, Ganapati R.

2016-04-07

Superconducting radio-frequency cavities made of ingot niobium with residual resistivity ratio (RRR) greater than 250 have proven to have similar or better performance than fine-grain Nb cavities of the same purity, after standard processing. The high purity requirement contributes to the high cost of the material. As superconducting accelerators operating in continuous-wave typically require cavities to operate at moderate accelerating gradients, using lower purity material could be advantageous not only to reduce cost but also to achieve higher Q 0-values. In this contribution we present the results from cryogenic RF tests of 1.3–1.5 GHz single-cell cavities made of ingot Nbmore » of medium (RRR = 100–150) and low (RRR = 60) purity from different suppliers. Cavities made of medium-purity ingots routinely achieved peak surface magnetic field values greater than 70 mT with an average Q 0-value of 2 × 10 10 at 2 K after standard processing treatments. As a result, the performances of cavities made of low-purity ingots were affected by significant pitting of the surface after chemical etching.« less

High Color-Purity Green, Orange, and Red Light-Emitting Didoes Based on Chemically Functionalized Graphene Quantum Dots

NASA Astrophysics Data System (ADS)

Kwon, Woosung; Kim, Young-Hoon; Kim, Ji-Hee; Lee, Taehyung; Do, Sungan; Park, Yoonsang; Jeong, Mun Seok; Lee, Tae-Woo; Rhee, Shi-Woo

2016-04-01

Chemically derived graphene quantum dots (GQDs) to date have showed very broad emission linewidth due to many kinds of chemical bondings with different energy levels, which significantly degrades the color purity and color tunability. Here, we show that use of aniline derivatives to chemically functionalize GQDs generates new extrinsic energy levels that lead to photoluminescence of very narrow linewidths. We use transient absorption and time-resolved photoluminescence spectroscopies to study the electronic structures and related electronic transitions of our GQDs, which reveals that their underlying carrier dynamics is strongly related to the chemical properties of aniline derivatives. Using these functionalized GQDs as lumophores, we fabricate light-emitting didoes (LEDs) that exhibit green, orange, and red electroluminescence that has high color purity. The maximum current efficiency of 3.47 cd A-1 and external quantum efficiency of 1.28% are recorded with our LEDs; these are the highest values ever reported for LEDs based on carbon-nanoparticle phosphors. This functionalization of GQDs with aniline derivatives represents a new method to fabricate LEDs that produce natural color.

METHOD FOR PREPARATION OF SINTERABLE BERYLLIUM OXIDE

DOEpatents

Sturm, B.J.

1963-08-13

High-purity beryllium oxide for nuclear reactor applications can be prepared by precipitation of beryllium oxalate monohydrate from aqueous solution at a temperature above 50 deg C and subsequent calcination of the precipitate. Improved purification with respect to metallic impurities is obtained, and the product beryllium oxide sinters reproducibly to a high density. (AEC)

Process for producing organic products containing silicon, hydrogen, nitrogen, and carbon by the direct reaction between elemental silicon and organic amines and products formed thereby

DOEpatents

Pugar, E.A.; Morgan, P.E.D.

1988-04-04

A process is disclosed for producing, at a low temperature, a high purity organic reaction product consisting essentially of silicon, hydrogen, nitrogen, and carbon. The process comprises reacting together a particulate elemental high purity silicon with a high purity reactive amine reactant in a liquid state at a temperature of from about O/degree/C up to about 300/degree/C. A high purity silicon carbide/silicon nitride ceramic product can be formed from this intermediate product, if desired, by heating the intermediate product at a temperature of from about 1200-1700/degree/C for a period from about 15 minutes up to about 2 hours or the organic reaction product may be employed in other chemical uses.

Process for producing organic products containing silicon, hydrogen, nitrogen, and carbon by the direct reaction between elemental silicon and organic amines

DOEpatents

Pugar, Eloise A.; Morgan, Peter E. D.

1990-04-03

A process is disclosed for producing, at a low temperature, a high purity organic reaction product consisting essentially of silicon, hydrogen, nitrogen, and carbon. The process comprises reacting together a particulate elemental high purity silicon with a high purity reactive amine reactant in a liquid state at a temperature of from about 0.degree. C. up to about 300.degree. C. A high purity silicon carbide/silicon nitride ceramic product can be formed from this intermediate product, if desired, by heating the intermediate product at a temperature of from about 1200.degree.-1700.degree. C. for a period from about 15 minutes up to about 2 hours or the organic reaction product may be employed in other chemical uses.

Alternative polymer separation technology by centrifugal force in a melted state

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

Dobrovszky, Károly; Ronkay, Ferenc, E-mail: ronkay@pt.bme.hu

2014-11-15

Highlights: • Waste separation should take place at high purity. • Developed a novel, alternative separation method, where the separation occurred in a melted state by centrifugal forces. • Possibility of separation two different plastics into neat fractions. • High purity fractions were established at granulates and also at prefabricated blend. • Results were verified by DSC, optical microscopy and Raman spectroscopy. - Abstract: In order to upgrade polymer waste during recycling, separation should take place at high purity. The present research was aimed to develop a novel, alternative separation opportunity, where the polymer fractions were separated by centrifugal forcemore » in melted state. The efficiency of the constructed separation equipment was verified by two immiscible plastics (polyethylene terephthalate, PET; low density polyethylene, LDPE), which have a high difference of density, and of which large quantities can also be found in the municipal solid waste. The results show that the developed equipment is suitable not only for separating dry blended mixtures of PET/LDPE into pure components again, but also for separating prefabricated polymer blends. By this process it becomes possible to recover pure polymer substances from multi-component products during the recycling process. The adequacy of results was verified by differential scanning calorimetry (DSC) measurement as well as optical microscopy and Raman spectroscopy.« less

A Cabin Air Separator for EVA Oxygen

NASA Technical Reports Server (NTRS)

Graf, John C.

2011-01-01

Presently, the Extra-Vehicular Activities (EVAs) conducted from the Quest Joint Airlock on the International Space Station use high pressure, high purity oxygen that is delivered to the Space Station by the Space Shuttle. When the Space Shuttle retires, a new method of delivering high pressure, high purity oxygen to the High Pressure Gas Tanks (HPGTs) is needed. One method is to use a cabin air separator to sweep oxygen from the cabin air, generate a low pressure/high purity oxygen stream, and compress the oxygen with a multistage mechanical compressor. A main advantage to this type of system is that the existing low pressure oxygen supply infrastructure can be used as the source of cabin oxygen. ISS has two water electrolysis systems that deliver low pressure oxygen to the cabin, as well as chlorate candles and compressed gas tanks on cargo vehicles. Each of these systems can feed low pressure oxygen into the cabin, and any low pressure oxygen source can be used as an on-board source of oxygen. Three different oxygen separator systems were evaluated, and a two stage Pressure Swing Adsorption system was selected for reasons of technical maturity. Two different compressor designs were subjected to long term testing, and the compressor with better life performance and more favorable oxygen safety characteristics was selected. These technologies have been used as the basis of a design for a flight system located in Equipment Lock, and taken to Preliminary Design Review level of maturity. This paper describes the Cabin Air Separator for EVA Oxygen (CASEO) concept, describes the separator and compressor technology trades, highlights key technology risks, and describes the flight hardware concept as presented at Preliminary Design Review (PDR)

Extinction coefficients and purity of single-walled carbon nanotubes.

PubMed

Zhao, B; Itkis, M E; Niyogi, S; Hu, H; Perea, D E; Haddon, R C

2004-11-01

Single-walled carbon nanotubes (SWNTs) hold great promise for advanced applications in aerospace, electronics and medicine, yet these industries require materials with rigorous quality control. There are currently no accepted standards for quality assurance or quality control among the commercial suppliers of SWNTs. We briefly discuss the applicability of various techniques to measure SWNT purity and review, in detail, the advantages of near infrared (NIR) spectroscopy for the quantitative assessment of the bulk carbonaceous purity of SWNTs. We review the use of solution phase NIR spectroscopy for the analysis and characterization of a variety of carbon materials, emphasizing SWNTs produced by the electric arc (EA), laser oven (LO) and HiPco (HC) methods. We consider the applicability of Beer's law to carbon materials dispersed in dimethylformamide (DMF) and the effective extinction coefficients that are obtained from such dispersions. Analysis of the areal absorptivities of the second interband transition of semiconducting EA-produced SWNTs for a number of samples of differing purities has lead to an absolute molar extinction coefficient for the carbonaceous impurities in EA-produced SWNT samples. We conclude that NIR spectroscopy is the clear method of choice for the assessment of the bulk carbonaceous purity of EA-produced SWNTs, and we suggest that an absolute determination of the purity of SWNTs is within reach. Continued work in this area is expected to lead to a universal method for the assessment of the absolute bulk purity of SWNTs from all sources--such a development will be of great importance for nanotube science and for future customers for this product.

Rare Cell Capture in Microfluidic Devices

PubMed Central

Pratt, Erica D.; Huang, Chao; Hawkins, Benjamin G.; Gleghorn, Jason P.; Kirby, Brian J.

2010-01-01

This article reviews existing methods for the isolation, fractionation, or capture of rare cells in microfluidic devices. Rare cell capture devices face the challenge of maintaining the efficiency standard of traditional bulk separation methods such as flow cytometers and immunomagnetic separators while requiring very high purity of the target cell population, which is typically already at very low starting concentrations. Two major classifications of rare cell capture approaches are covered: (1) non-electrokinetic methods (e.g., immobilization via antibody or aptamer chemistry, size-based sorting, and sheath flow and streamline sorting) are discussed for applications using blood cells, cancer cells, and other mammalian cells, and (2) electrokinetic (primarily dielectrophoretic) methods using both electrode-based and insulative geometries are presented with a view towards pathogen detection, blood fractionation, and cancer cell isolation. The included methods were evaluated based on performance criteria including cell type modeled and used, number of steps/stages, cell viability, and enrichment, efficiency, and/or purity. Major areas for improvement are increasing viability and capture efficiency/purity of directly processed biological samples, as a majority of current studies only process spiked cell lines or pre-diluted/lysed samples. Despite these current challenges, multiple advances have been made in the development of devices for rare cell capture and the subsequent elucidation of new biological phenomena; this article serves to highlight this progress as well as the electrokinetic and non-electrokinetic methods that can potentially be combined to improve performance in future studies. PMID:21532971

Solution-Processable High-Purity Semiconducting SWCNTs for Large-Area Fabrication of High-Performance Thin-Film Transistors.

PubMed

Gu, Jianting; Han, Jie; Liu, Dan; Yu, Xiaoqin; Kang, Lixing; Qiu, Song; Jin, Hehua; Li, Hongbo; Li, Qingwen; Zhang, Jin

2016-09-01

For the large-area fabrication of thin-film transistors (TFTs), a new conjugated polymer poly[9-(1-octylonoyl)-9H-carbazole-2,7-diyl] is developed to harvest ultrahigh-purity semiconducting single-walled carbon nanotubes. Combined with spectral and nanodevice characterization, the purity is estimated up to 99.9%. High density and uniform network formed by dip-coating process is liable to fabricate high-performance TFTs on a wafer-scale and the as-fabricated TFTs exhibit a high degree of uniformity. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Production of recombinant protein G through high-density fermentation of engineered bacteria as well as purification.

PubMed

Zhang, Hu-Cheng; Yang, Jun; Yang, Guo-Wei; Wang, Xiao-Jie; Fan, Hai-Tao

2015-08-01

Recombinant Streptococcus Protein G (PG) is a cell wall protein, which, when combined with mammal immunoglobulin, is used in separating antibody technology. High-density fermentation technologies using an engineered recombinant PG-producing bacteria as well as PG separation and purification technologies have a direct impact on the availability and application of PG. Through primary and secondary seed cultivation, a recombinant E. coli strain was subjected to high-density fermentation with controlled feed supplement concentration under stimulation with isopropyl β-D-1-thiogalactopyranoside. The present study investigated the effect of factors including inoculum size, oxygen levels, pH and the cultivating method on the fermentation process, as well as the effect of the separation and purification technologies, including ultrasonication, nickel column affinity chromatography, Sephadex G-25 gel filtration chromatography and diethylaminoethanol-sepharose fast flow ion exchange chromatography on the yield and purity of PG. The efficiency of extraction was detected using SDS-PAGE. High-density fermentation yielded 80-150 g/l of bacteria and 1 g PG was obtained from one liter broth. The present study delivered a highly efficient novel method via which PG can be obtained at a high concentration and a purity >95%.

High surface area calcite

NASA Astrophysics Data System (ADS)

Schultz, L. N.; Andersson, M. P.; Dalby, K. N.; Müter, D.; Okhrimenko, D. V.; Fordsmand, H.; Stipp, S. L. S.

2013-05-01

Calcite (CaCO3) is important in many fields—in nature, because it is a component of aquifers, oil reservoirs and prospective CO2 storage sites, and in industry, where it is used in products as diverse as paper, toothpaste, paint, plastic and aspirin. It is difficult to obtain high purity calcite with a high surface area but such material is necessary for industrial applications and for fundamental calcite research. Commercial powder is nearly always contaminated with growth inhibitors such as sugars, citrate or pectin and most laboratory synthesis methods deliver large precipitates, often containing vaterite or aragonite. To address this problem, we (i) adapted the method of carbonating a Ca(OH)2 slurry with CO2 gas to develop the first simple, cheap, safe and reproducible procedure using common laboratory equipment, to obtain calcite that reproducibly had a surface area of 14-17 m2/g and (ii) conducted a thorough characterization of the product. Scanning electron microscopy (SEM) revealed nanometer scale, rhombohedral crystals. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (IR) confirmed highly crystalline, pure calcite that more closely resembles the dimensions of the biogenic calcite produced by algae in coccoliths than other methods for synthesizing calcite. We suggest that this calcite is useful when purity and high surface area are important.

Trace elements study of high purity nanocrystalline silicon carbide (3C-SiC) using k0-INAA method

NASA Astrophysics Data System (ADS)

Huseynov, Elchin; Jazbec, Anze

2017-07-01

Silicon carbide (3C-SiC) nanoparticles have been irradiated by neutron flux (2×1013 n·cm-2·s-1) at TRIGA Mark II type research reactor. After neutron irradiation, the radioisotopes of trace elements in the nanocrystalline 3C-SiC were studied as time functions. The identification of isotopes which significantly increased the activity of the samples as a result of neutron radiation was carried out. Nanocrystalline 3C-SiC are synthesized by standard laser technique and the purity of samples was determined by the k0-based Instrumental Neutron Activation Analysis (k0-INAA) method. Trace elements concentration in the 3C-SiC nanoparticles were determined by the radionuclides of appropriate elements. The trace element isotopes concentration have been calculated in percentage according to k0-INAA method.

3D pulsed laser-triggered high-speed microfluidic fluorescence-activated cell sorter

PubMed Central

Chen, Yue; Wu, Ting-Hsiang; Kung, Yu-Chun; Teitell, Michael A.; Chiou, Pei-Yu

2014-01-01

We report a 3D microfluidic pulsed laser-triggered fluorescence-activated cell sorter capable of sorting at a throughput of 23,000 cells sec−1 with 90% purity in high-purity mode and at a throughput of 45,000 cells sec−1 with 45% purity in enrichment mode in one stage and in a single channel. This performance is realized by exciting laser-induced cavitation bubbles in a 3D PDMS microfluidic channel to generate high-speed liquid jets that deflect detected fluorescent cells and particles focused by 3D sheath flows. The ultrafast switching mechanism (20 μsec complete on-off cycle), small liquid jet perturbation volume, and three-dimensional sheath flow focusing for accurate timing control of fast (1.5 m sec−1) passing cells and particles are three critical factors enabling high-purity sorting at high-throughput in this sorter. PMID:23844418

Proportion estimation using prior cluster purities

NASA Technical Reports Server (NTRS)

Terrell, G. R. (Principal Investigator)

1980-01-01

The prior distribution of CLASSY component purities is studied, and this information incorporated into maximum likelihood crop proportion estimators. The method is tested on Transition Year spring small grain segments.

High-purity circular RNA isolation method (RPAD) reveals vast collection of intronic circRNAs.

PubMed

Panda, Amaresh C; De, Supriyo; Grammatikakis, Ioannis; Munk, Rachel; Yang, Xiaoling; Piao, Yulan; Dudekula, Dawood B; Abdelmohsen, Kotb; Gorospe, Myriam

2017-07-07

High-throughput RNA sequencing methods coupled with specialized bioinformatic analyses have recently uncovered tens of thousands of unique circular (circ)RNAs, but their complete sequences, genes of origin and functions are largely unknown. Given that circRNAs lack free ends and are thus relatively stable, their association with microRNAs (miRNAs) and RNA-binding proteins (RBPs) can influence gene expression programs. While exoribonuclease treatment is widely used to degrade linear RNAs and enrich circRNAs in RNA samples, it does not efficiently eliminate all linear RNAs. Here, we describe a novel method for the isolation of highly pure circRNA populations involving RNase R treatment followed by Polyadenylation and poly(A)+ RNA Depletion (RPAD), which removes linear RNA to near completion. High-throughput sequencing of RNA prepared using RPAD from human cervical carcinoma HeLa cells and mouse C2C12 myoblasts led to two surprising discoveries: (i) many exonic circRNA (EcircRNA) isoforms share an identical backsplice sequence but have different body sizes and sequences, and (ii) thousands of novel intronic circular RNAs (IcircRNAs) are expressed in cells. In sum, isolating high-purity circRNAs using the RPAD method can enable quantitative and qualitative analyses of circRNA types and sequence composition, paving the way for the elucidation of circRNA functions. Published by Oxford University Press on behalf of Nucleic Acids Research 2017.

High-purity circular RNA isolation method (RPAD) reveals vast collection of intronic circRNAs

PubMed Central

De, Supriyo; Grammatikakis, Ioannis; Munk, Rachel; Yang, Xiaoling; Piao, Yulan; Dudekula, Dawood B.; Gorospe, Myriam

2017-01-01

Abstract High-throughput RNA sequencing methods coupled with specialized bioinformatic analyses have recently uncovered tens of thousands of unique circular (circ)RNAs, but their complete sequences, genes of origin and functions are largely unknown. Given that circRNAs lack free ends and are thus relatively stable, their association with microRNAs (miRNAs) and RNA-binding proteins (RBPs) can influence gene expression programs. While exoribonuclease treatment is widely used to degrade linear RNAs and enrich circRNAs in RNA samples, it does not efficiently eliminate all linear RNAs. Here, we describe a novel method for the isolation of highly pure circRNA populations involving RNase R treatment followed by Polyadenylation and poly(A)+ RNA Depletion (RPAD), which removes linear RNA to near completion. High-throughput sequencing of RNA prepared using RPAD from human cervical carcinoma HeLa cells and mouse C2C12 myoblasts led to two surprising discoveries: (i) many exonic circRNA (EcircRNA) isoforms share an identical backsplice sequence but have different body sizes and sequences, and (ii) thousands of novel intronic circular RNAs (IcircRNAs) are expressed in cells. In sum, isolating high-purity circRNAs using the RPAD method can enable quantitative and qualitative analyses of circRNA types and sequence composition, paving the way for the elucidation of circRNA functions. PMID:28444238

Monte Carlo simulation of gamma-ray interactions in an over-square high-purity germanium detector for in-vivo measurements

NASA Astrophysics Data System (ADS)

Saizu, Mirela Angela

2016-09-01

The developments of high-purity germanium detectors match very well the requirements of the in-vivo human body measurements regarding the gamma energy ranges of the radionuclides intended to be measured, the shape of the extended radioactive sources, and the measurement geometries. The Whole Body Counter (WBC) from IFIN-HH is based on an “over-square” high-purity germanium detector (HPGe) to perform accurate measurements of the incorporated radionuclides emitting X and gamma rays in the energy range of 10 keV-1500 keV, under conditions of good shielding, suitable collimation, and calibration. As an alternative to the experimental efficiency calibration method consisting of using reference calibration sources with gamma energy lines that cover all the considered energy range, it is proposed to use the Monte Carlo method for the efficiency calibration of the WBC using the radiation transport code MCNP5. The HPGe detector was modelled and the gamma energy lines of 241Am, 57Co, 133Ba, 137Cs, 60Co, and 152Eu were simulated in order to obtain the virtual efficiency calibration curve of the WBC. The Monte Carlo method was validated by comparing the simulated results with the experimental measurements using point-like sources. For their optimum matching, the impact of the variation of the front dead layer thickness and of the detector photon absorbing layers materials on the HPGe detector efficiency was studied, and the detector’s model was refined. In order to perform the WBC efficiency calibration for realistic people monitoring, more numerical calculations were generated simulating extended sources of specific shape according to the standard man characteristics.

6. LOOKING WEST IN LOW PURITY BULK OXYGEN BUILDING AT ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

6. LOOKING WEST IN LOW PURITY BULK OXYGEN BUILDING AT STEAM TURBINE END OF TWO ALLIS-CHALMERS AXIAL AIR COMPRESSORS FOR 1000 TON PER DAY HIGH PURITY OXYGEN MAKING PLANT. - U.S. Steel Duquesne Works, Fuel & Utilities Plant, Along Monongahela River, Duquesne, Allegheny County, PA

5. LOOKING WEST IN LOW PURITY BULK OXYGEN BUILDING AT ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

5. LOOKING WEST IN LOW PURITY BULK OXYGEN BUILDING AT STEAM TURBINE END OF TWO ALLIS-CHALMER AXIAL AIR COMPRESSORS FOR 1000 TON PER DAY HIGH PURITY OXYGEN MAKING PLANT. - U.S. Steel Duquesne Works, Fuel & Utilities Plant, Along Monongahela River, Duquesne, Allegheny County, PA

Characteristics of signals originating near the lithium-diffused N+ contact of high purity germanium p-type point contact detectors

DOE PAGES

Aguayo, E.; Amman, M.; Avignone, F. T.; ...

2012-11-09

A study of signals originating near the lithium-diffused n+ contact of p-type point contact (PPC) high purity germanium detectors (HPGe) is presented. The transition region between the active germanium and the fully dead layer of the n+ contact is examined. Energy depositions in this transition region are shown to result in partial charge collection. This provides a mechanism for events with a well defined energy to contribute to the continuum of the energy spectrum at lower energies. A novel technique to quantify the contribution from this source of background is introduced. Furthermore, experiments that operate germanium detectors with a verymore » low energy threshold may benefit from the methods presented herein.« less

Solid-state curved focal plane arrays

NASA Technical Reports Server (NTRS)

Jones, Todd (Inventor); Nikzad, Shouleh (Inventor); Hoenk, Michael (Inventor)

2010-01-01

The present invention relates to curved focal plane arrays. More specifically, the present invention relates to a system and method for making solid-state curved focal plane arrays from standard and high-purity devices that may be matched to a given optical system. There are two ways to make a curved focal plane arrays starting with the fully fabricated device. One way, is to thin the device and conform it to a curvature. A second way, is to back-illuminate a thick device without making a thinned membrane. The thick device is a special class of devices; for example devices fabricated with high purity silicon. One surface of the device (the non VLSI fabricated surface, also referred to as the back surface) can be polished to form a curved surface.

High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

2017-03-01

In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

In-Situ Analysis of the Chemical Vapor Synthesis of Nanocrystalline Silicon Carbide by Aerosol Mass Spectrometry

DTIC Science & Technology

2001-11-01

ultrafine particles with a narrow size distribution and high purity. Chemical Vapor Synthesis (CVS) is a method to generate particles in the size range...high temperatures due to strong covalent bonds. Ultrafine particles of SiC are promising for the production of dense bulk solids due to the small grain

Flow cytometry sorting of nuclei enables the first global characterization of Paramecium germline DNA and transposable elements.

PubMed

Guérin, Frédéric; Arnaiz, Olivier; Boggetto, Nicole; Denby Wilkes, Cyril; Meyer, Eric; Sperling, Linda; Duharcourt, Sandra

2017-04-26

DNA elimination is developmentally programmed in a wide variety of eukaryotes, including unicellular ciliates, and leads to the generation of distinct germline and somatic genomes. The ciliate Paramecium tetraurelia harbors two types of nuclei with different functions and genome structures. The transcriptionally inactive micronucleus contains the complete germline genome, while the somatic macronucleus contains a reduced genome streamlined for gene expression. During development of the somatic macronucleus, the germline genome undergoes massive and reproducible DNA elimination events. Availability of both the somatic and germline genomes is essential to examine the genome changes that occur during programmed DNA elimination and ultimately decipher the mechanisms underlying the specific removal of germline-limited sequences. We developed a novel experimental approach that uses flow cell imaging and flow cytometry to sort subpopulations of nuclei to high purity. We sorted vegetative micronuclei and macronuclei during development of P. tetraurelia. We validated the method by flow cell imaging and by high throughput DNA sequencing. Our work establishes the proof of principle that developing somatic macronuclei can be sorted from a complex biological sample to high purity based on their size, shape and DNA content. This method enabled us to sequence, for the first time, the germline DNA from pure micronuclei and to identify novel transposable elements. Sequencing the germline DNA confirms that the Pgm domesticated transposase is required for the excision of all ~45,000 Internal Eliminated Sequences. Comparison of the germline DNA and unrearranged DNA obtained from PGM-silenced cells reveals that the latter does not provide a faithful representation of the germline genome. We developed a flow cytometry-based method to purify P. tetraurelia nuclei to high purity and provided quality control with flow cell imaging and high throughput DNA sequencing. We identified 61 germline transposable elements including the first Paramecium retrotransposons. This approach paves the way to sequence the germline genomes of P. aurelia sibling species for future comparative genomic studies.

Method for efficient recovery of high-purity polycarbonates from electronic waste.

PubMed

Weeden, George S; Soepriatna, Nicholas H; Wang, Nien-Hwa Linda

2015-02-17

More than one million tons of polycarbonates from waste electrical and electronic equipment are consigned to landfills at an increasing rate of 3-5% per year. Recycling the polymer waste should have a major environmental impact. Pure solvents cannot be used to selectively extract polycarbonates from mixtures of polymers with similar properties. In this study, selective mixed solvents are found using guidelines from Hansen solubility parameters, gradient polymer elution chromatography, and solubility tests. A room-temperature sequential extraction process using two mixed solvents is developed to recover polycarbonates with high yield (>95%) and a similar purity and molecular weight distribution as virgin polycarbonates. The estimated cost of recovery is less than 30% of the cost of producing virgin polycarbonates from petroleum. This method would potentially reduce raw materials from petroleum, use 84% less energy, reduce emission by 1-6 tons of CO2 per ton of polycarbonates, and reduce polymer accumulation in landfills and associated environmental hazards.

A Comparison of Methods for Computing the Residual Resistivity Ratio of High-Purity Niobium

PubMed Central

Splett, J. D.; Vecchia, D. F.; Goodrich, L. F.

2011-01-01

We compare methods for estimating the residual resistivity ratio (RRR) of high-purity niobium and investigate the effects of using different functional models. RRR is typically defined as the ratio of the electrical resistances measured at 273 K (the ice point) and 4.2 K (the boiling point of helium at standard atmospheric pressure). However, pure niobium is superconducting below about 9.3 K, so the low-temperature resistance is defined as the normal-state (i.e., non-superconducting state) resistance extrapolated to 4.2 K and zero magnetic field. Thus, the estimated value of RRR depends significantly on the model used for extrapolation. We examine three models for extrapolation based on temperature versus resistance, two models for extrapolation based on magnetic field versus resistance, and a new model based on the Kohler relationship that can be applied to combined temperature and field data. We also investigate the possibility of re-defining RRR so that the quantity is not dependent on extrapolation. PMID:26989580

Measurements of gamma (γ)-emitting radionuclides with a high-purity germanium detector: the methods and reliability of our environmental assessments on the Fukushima 1 Nuclear Power Plant accident.

PubMed

Mimura, Tetsuro; Mimura, Mari; Komiyama, Chiyo; Miyamoto, Masaaki; Kitamura, Akira

2014-01-01

The severe accident of Fukushima 1 Nuclear Power Plant due to the Tohoku Region Pacific Coast Earthquake in 11 March 2011 caused wide contamination and pollution by radionuclides in Fukushima and surrounding prefectures. In the current JPR symposium, a group of plant scientists attempted to examine the impact of the radioactive contamination on wild and cultivated plants. Measurements of gamma (γ) radiation from radionuclides in "Fukushima samples", which we called and collected from natural and agricultural areas in Fukushima prefecture were mostly done with a high-purity Ge detector in the Graduate School of Maritime Sciences, Kobe University. In this technical note, we describe the methods of sample preparation and measurements of radioactivity of the samples and discuss the reliability of our data in regards to the International Atomic Energy Agency (IAEA) Interlaboratory comparisons and proficiency test (IAEA proficiency test).

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

Meyer, Jeremy, E-mail: jeremy.meyer@hcuge.ch; Unit of Surgical Research, University of Geneva, Rue Michel-Servet 1, 1206 Genève; Lacotte, Stéphanie, E-mail: stephanie.lacotte@unige.ch

The objective of the present study was to develop an accurate and reproducible method for liver sinusoidal endothelial cell (LSEC) isolation in mice. Non-parenchymal cells were isolated using a modified two-step collagenase digestion combined with Optiprep density gradient centrifugation. LSEC were further purified using two prevalent methods, short-term selective adherence and CD146+ magnetic-activated cell sorting (MACS), and compared in terms of cell yield, viability and purity to our purification technique using CD11b cell depletion combined with long-term selective adherence. LSEC purification using our technique allowed to obtain 7.07±3.80 million LSEC per liver, while CD146+ MACS and short-term selective adherence yieldedmore » 2.94±1.28 and 0.99±0.66 million LSEC, respectively. Purity of the final cell preparation reached 95.10±2.58% when using our method. In contrast, CD146+ MACS and short-term selective adherence gave purities of 86.75±3.26% and 47.95±9.82%, respectively. Similarly, contamination by non-LSEC was the lowest when purification was performed using our technique, with a proportion of contaminating macrophages of only 1.87±0.77%. Further, isolated cells analysed by scanning electron microscopy presented typical LSEC fenestrations organized in sieve plates, demonstrating that the technique allowed to isolate bona fide LSEC. In conclusion, we described a reliable and reproducible technique for the isolation of high yields of pure LSEC in mice. This protocol provides an efficient method to prepare LSEC for studying their biological functions. - Highlights: • This protocol provides an efficient method to prepare primary mouse LSEC for studying their biological functions. • The liver cell dispersion step was improved by performing a retrograde cannulation of the liver. • The cell yield and the purity obtained were higher than comparative techniques in mice. • Contaminating macrophages were removed by introducing a CD11b- magnetic –activated cell sorting step.« less

Opioid Agonist Treatments and Heroin Overdose Deaths in Baltimore, Maryland, 1995–2009

PubMed Central

Gryczynski, Jan; O’Grady, Kevin E.; Sharfstein, Joshua M.; Warren, Gregory; Olsen, Yngvild; Mitchell, Shannon G.; Jaffe, Jerome H.

2013-01-01

Objectives. We examined the association between the expansion of methadone and buprenorphine treatment and the prevalence of heroin overdose deaths in Baltimore, Maryland from 1995 to 2009. Methods. We conducted a longitudinal time series analysis of archival data using linear regression with the Newey–West method to correct SEs for heteroscedasticity and autocorrelation, adjusting for average heroin purity. Results. Overdose deaths attributed to heroin ranged from a high of 312 in 1999 to a low of 106 in 2008. While mean heroin purity rose sharply (1995–1999), the increasing number of patients treated with methadone was not associated with a change in the number of overdose deaths, but starting in 2000 expansion of opioid agonist treatment was associated with a decline in overdose deaths. Adjusting for heroin purity and the number of methadone patients, there was a statistically significant inverse relationship between heroin overdose deaths and patients treated with buprenorphine (P = .002). Conclusions. Increased access to opioid agonist treatment was associated with a reduction in heroin overdose deaths. Implementing policies that support evidence-based medication treatment of opiate dependence may decrease heroin overdose deaths. PMID:23488511

Different Technical Applications of Carbon Nanotubes.

PubMed

Abdalla, S; Al-Marzouki, F; Al-Ghamdi, Ahmed A; Abdel-Daiem, A

2015-12-01

Carbon nanotubes have been of great interest because of their simplicity and ease of synthesis. The novel properties of nanostructured carbon nanotubes such as high surface area, good stiffness, and resilience have been explored in many engineering applications. Research on carbon nanotubes have shown the application in the field of energy storage, hydrogen storage, electrochemical supercapacitor, field-emitting devices, transistors, nanoprobes and sensors, composite material, templates, etc. For commercial applications, large quantities and high purity of carbon nanotubes are needed. Different types of carbon nanotubes can be synthesized in various ways. The most common techniques currently practiced are arc discharge, laser ablation, and chemical vapor deposition and flame synthesis. The purification of CNTs is carried out using various techniques mainly oxidation, acid treatment, annealing, sonication, filtering chemical functionalization, etc. However, high-purity purification techniques still have to be developed. Real applications are still under development. This paper addresses the current research on the challenges that are associated with synthesis methods, purification methods, and dispersion and toxicity of CNTs within the scope of different engineering applications, energy, and environmental impact.

High-yield production of pure tagatose from fructose by a three-step enzymatic cascade reaction.

PubMed

Lee, Seon-Hwa; Hong, Seung-Hye; Kim, Kyoung-Rok; Oh, Deok-Kun

2017-08-01

To produce tagatose from fructose with a high conversion rate and to establish a high-yield purification method of tagatose from the reaction mixture. Fructose at 1 M (180 g l -1 ) was converted to 0.8 M (144 g l -1 ) tagatose by a three-step enzymatic cascade reaction, involving hexokinase, plus ATP, fructose-1,6-biphosphate aldolase, phytase, over 16 h with a productivity of 9 g l -1 h -1 . No byproducts were detected. Tagatose was recrystallized from ethanol to a purity of 99.9% and a yield of 96.3%. Overall, tagatose at 99.9% purity was obtained from fructose with a yield of 77%. This is the first biotechnological production of tagatose from fructose and the first application of solvent recrystallization for the purification of rare sugars.

High purity silane and silicon production

NASA Technical Reports Server (NTRS)

Breneman, William C. (Inventor)

1987-01-01

Silicon tetrachloride, hydrogen and metallurgical silicon are reacted at about 400.degree.-600.degree. C. and at pressures in excess of 100 psi, and specifically from about 300 up to about 600 psi to form di- and trichlorosilane that is subjected to disproportionation in the presence of an anion exchange resin to form high purity silane. By-product and unreacted materials are recycled, with metallurgical silicon and hydrogen being essentially the only consumed feed materials. The silane product may be further purified, as by means of activated carbon or cryogenic distillation, and decomposed in a fluid bed or free space reactor to form high purity polycrystalline silicon and by-product hydrogen which can be recycled for further use. The process results in simplified waste disposal operations and enhances the overall conversion of metallurgical grade silicon to silane and high purity silicon for solar cell and semiconductor silicon applications.

Method of preparing silicon from sodium fluosilicate

DOEpatents

Schmidt, Frederick A.; Rehbein, David; Chiotti, Premo

1984-01-01

A process for preparing high purity silicon metal from Na.sub.2 SiF.sub.6 (sodium fluosilicate). The sodium fluosilicate is heated to decomposition temperature to form NaF, which retains most of the impurities, and gaseous SiF.sub.4. The SiF.sub.4 is then reduced by the bomb reduction method using a reductant having a low packing density.

Purity assessment of organic calibration standards using a combination of quantitative NMR and mass balance.

PubMed

Davies, Stephen R; Jones, Kai; Goldys, Anna; Alamgir, Mahuiddin; Chan, Benjamin K H; Elgindy, Cecile; Mitchell, Peter S R; Tarrant, Gregory J; Krishnaswami, Maya R; Luo, Yawen; Moawad, Michael; Lawes, Douglas; Hook, James M

2015-04-01

Quantitative NMR spectroscopy (qNMR) has been examined for purity assessment using a range of organic calibration standards of varying structural complexities, certified using the traditional mass balance approach. Demonstrated equivalence between the two independent purity values confirmed the accuracy of qNMR and highlighted the benefit of using both methods in tandem to minimise the potential for hidden bias, thereby conferring greater confidence in the overall purity assessment. A comprehensive approach to purity assessment is detailed, utilising, where appropriate, multiple peaks in the qNMR spectrum, chosen on the basis of scientific reason and statistical analysis. Two examples are presented in which differences between the purity assignment by qNMR and mass balance are addressed in different ways depending on the requirement of the end user, affording fit-for-purpose calibration standards in a cost-effective manner.

Method of purifying metallurgical grade silicon employing reduced pressure atmospheric control

NASA Technical Reports Server (NTRS)

Ingle, W. M.; Thompson, S. W.; Chaney, R. E. (Inventor)

1979-01-01

A method in which a quartz tube is charged with chunks of metallurgical grade silicon and/or a mixture of such chunks and high purity quartz sand, and impurities from a class including aluminum, boron, as well as certain transition metals including nickel, iron, and manganese is described. The tube is then evacuated and heated to a temperature within a range of 800 C to 1400 C. A stream of gas comprising a reactant, such as silicon tetrafluoride, is continuously delivered at low pressures through the charge for causing a metathetical reaction of impurities of the silicon and the reactant to occur for forming a volatile halide and leaving a residue of silicon of an improved purity. The reactant which included carbon monoxide gas and impurities such as iron and nickel react to form volatile carbonyls.

High-voltage lateral double-implanted MOSFETs implemented on high-purity semi-insulating 4H-SiC substrates with gate field plates

NASA Astrophysics Data System (ADS)

Seok, Ogyun; Kim, Hyoung Woo; Moon, Jeong Hyun; Lee, Hyun-Su; Bahng, Wook

2018-06-01

Lateral double-implanted MOSFETs (LDIMOSFETs) fabricated on on-axis high-purity semi-insulating (HPSI) 4H-SiC substrates with gate field plates have been demonstrated for the enhancement of reverse blocking capability. The effects of gate field plate on LDIMOSFET were analyzed by simulation and experimental methods. The electric field concentration at the gate edge was successfully suppressed by a gate field plate. A high breakdown voltage of 934 V and a figure of merit of 14.6 MW/cm2 were achieved at L FP of 2 µm and L drift of 15 µm, while those of the conventional device without a gate field plate were 744 V and 13.3 MW/cm2, respectively. Also, the fabricated device shows stable blocking characteristics at a high temperature of 250 °C. The drain leakage was increased by only 22% at 250 °C compared with that at room temperature.

A High-Purity Alumina for Use in Studies of Shock Loaded Samples

NASA Astrophysics Data System (ADS)

Lacina, David; Neel, Christopher

2017-06-01

We report the results of plate impact experiments on a potential new ``standard'' material, Coorstek Plasmapure-UC (99.9% purity) polycrystalline alumina, for use in non-conduction, impact environment, shock loading studies. This work was motivated by a desire to find a 99.9% purity alumina to replace the now unavailable Coors Vistal (99.9%) alumina, as it was hoped the Hugoniot elastic limit (HEL) of the new standard would match the 9-11 GPa value of Vistal. Shock response data, including the HEL, Hugoniot particle velocities, Hugoniot shock velocities, stress vs volume, and release wave speeds, was obtained up to 14 GPa. This data will be compared with Hugoniot curve data for other high purity alumina to contrast differences in the shock response, and is intended to be useful in impedance matching calculations. We will show that the HEL of Plasmapure-UC alumina is 5.5 GPa and speculate on causes for this lower than expected value. We will also explore why the elastic-plastic response for Plasmapure-UC alumina differs from what has been observed from other high purity alumina. The final result of this work is to recommend a well-characterized, lower purity alumina (Coorstek AD-995) as a potential new ``standard'' material.

Reverse-engineering flow-cytometry gating strategies for phenotypic labelling and high-performance cell sorting.

PubMed

Becht, Etienne; Simoni, Yannick; Coustan-Smith, Elaine; Maximilien, Evrard; Cheng, Yang; Ng, Lai Guan; Campana, Dario; Newell, Evan

2018-06-21

Recent flow and mass cytometers generate datasets of dimensions 20 to 40 and a million single cells. From these, many tools facilitate the discovery of new cell populations associated with diseases or physiology. These new cell populations require the identification of new gating strategies, but gating strategies become exponentially more difficult to optimize when dimensionality increases. To facilitate this step, we developed Hypergate, an algorithm which given a cell population of interest identifies a gating strategy optimized for high yield and purity. Hypergate achieves higher yield and purity than human experts, Support Vector Machines and Random-Forests on public datasets. We use it to revisit some established gating strategies for the identification of innate lymphoid cells, which identifies concise and efficient strategies that allow gating these cells with fewer parameters but higher yield and purity than the current standards. For phenotypic description, Hypergate's outputs are consistent with fields' knowledge and sparser than those from a competing method. Hypergate is implemented in R and available on CRAN. The source code is published at http://github.com/ebecht/hypergate under an Open Source Initiative-compliant licence. Supplementary data are available at Bioinformatics online.

Nearly Blinking-Free, High-Purity Single-Photon Emission by Colloidal InP/ZnSe Quantum Dots.

PubMed

Chandrasekaran, Vigneshwaran; Tessier, Mickaël D; Dupont, Dorian; Geiregat, Pieter; Hens, Zeger; Brainis, Edouard

2017-10-11

Colloidal core/shell InP/ZnSe quantum dots (QDs), recently produced using an improved synthesis method, have a great potential in life-science applications as well as in integrated quantum photonics and quantum information processing as single-photon emitters. Single-particle spectroscopy of 10 nm QDs with 3.2 nm cores reveals strong photon antibunching attributed to fast (70 ps) Auger recombination of multiple excitons. The QDs exhibit very good photostability under strong optical excitation. We demonstrate that the antibunching is preserved when the QDs are excited above the saturation intensity of the fundamental-exciton transition. This result paves the way toward their usage as high-purity on-demand single-photon emitters at room temperature. Unconventionally, despite the strong Auger blockade mechanism, InP/ZnSe QDs also display very little luminescence intermittency ("blinking"), with a simple on/off blinking pattern. The analysis of single-particle luminescence statistics places these InP/ZnSe QDs in the class of nearly blinking-free QDs, with emission stability comparable to state-of-the-art thick-shell and alloyed-interface CdSe/CdS, but with improved single-photon purity.

Supply-side response to declining heroin purity: fentanyl overdose episode in New Jersey.

PubMed

Hempstead, Katherine; Yildirim, Emel O

2014-06-01

The inelastic price demand observations characteristic of illegal drug markets have led to the conclusion that the burden of a negative supply shock would be completely reflected to consumers. This paper argues that the increasing availability of prescription opioids may threaten heroin sellers' profit margin and force them to find alternative methods to compensate buyers in the event of a supply shock. We investigate the 2006 fentanyl overdose episode in New Jersey and argue that the introduction of non-pharmaceutical fentanyl, its spatial distribution, and the timing of overdose deaths may have been related to trends in heroin purity. Using medical examiner data, as well as data from the Drug Enforcement Administration, Office of Diversion Control on retail sales of prescription opioids in a negative binomial specification, we show that month-to-month fluctuations in heroin purity have a significant effect on fentanyl-related overdoses, particularly in those areas where prescription opioids are highly available. Copyright © 2013 John Wiley & Sons, Ltd.

Extraction of Polysaccharide from Spirulina and Evaluation of Its Activities.

PubMed

Wang, Bingyue; Liu, Qian; Huang, Yinghong; Yuan, Yueling; Ma, Qianqian; Du, Manling; Cai, Tiange; Cai, Yu

2018-01-01

Polysaccharide of Spirulina platensis (PSP) is a kind of water-soluble polysaccharide extracted from Spirulina platensis . It has been proved to have antitumor, antioxidation, antiaging, and antivirus properties. And it has a promising prospect for wide application. This study aims to identify an extraction process for high-purity polysaccharide in Spirulina (PSP) through a series of optimization methods and then evaluates its initial antiaging activities. Four kinds of extraction methods-hot-water extraction, alkali extraction, ultrasonic-assisted extraction, and freeze-thaw extraction-were compared to find the optimal one, which was further optimized by response surface methodology. PSP was obtained after the crude PSP was deproteinized and depigmented. The antiaging effects of PSP were preliminarily evaluated through in vitro cell experiments. The alkali extraction method was determined as the optimal method, with the optimized extraction process consisting of a solid-liquid ratio of 1 : 50, a pH value of 10.25, a temperature of 89.24°C, and a time of 9.99 h. The final PSP contained 71.65% of polysaccharide and 8.54% of protein. At a concentration of 50  μ g/mL, PSP exerted a significant promoting effect on the proliferation and traumatic fusion of human immortalized epidermal cells HaCaT. An extraction method for high-purity PSP with a high extraction rate was established, and in vitro results suggest antioxidation and antiaging activities.

High purity tungsten targets

NASA Technical Reports Server (NTRS)

1975-01-01

High purity tungsten, which is used for targets in X-ray tubes was considered for space processing. The demand for X-ray tubes was calculated using the growth rates for dental and medical X-ray machines. It is concluded that the cost benefits are uncertain.

Spectral properties of molecular iodine in absorption cells filled to specified saturation pressure.

PubMed

Hrabina, Jan; Šarbort, Martin; Acef, Ouali; Burck, Frédéric Du; Chiodo, Nicola; Holá, Miroslava; Číp, Ondřej; Lazar, Josef

2014-11-01

We present the results of measurement and evaluation of spectral properties of iodine absorption cells filled at certain saturation pressure. A set of cells made of borosilicate glass instead of common fused silica was tested for their spectral properties in greater detail with special care for the long-term development of the absorption media purity. The results were compared with standard fused silica cells and the high quality of iodine was verified. A measurement method based on an approach relying on measurement of linewidth of the hyperfine transitions is proposed as a novel technique for iodine cell absorption media purity evaluation. A potential application in laser metrology of length is also discussed.

Pentatwinned Cu Nanowires with Ultrathin Diameters below 20 nm and Their Use as Templates for the Synthesis of Au-Based Nanotubes

DOE PAGES

Luo, Ming; Zhou, Ming; Rosa da Silva, Robson; ...

2017-01-24

Here, we report a one-pot method for the facile synthesis of Cu nanowires in high purity, together with ultrathin diameters well below 20 nm. Selected area electron diffraction and high-resolution transmission electron microscopy studies confirm that the Cu nanowires are grown along the <110> direction to give pentatwinned, one-dimensional nanostructures, enclosed by five {100} facets on the side surface. A systematic study further indicates that it is critical to conduct the synthesis under an argon atmosphere in order to improve the purity and uniformity of the nanowires while keeping their diameters thinner than 20 nm. Finally, we demonstrate the usemore » of these nanowires as sacrificial templates for the synthesis of Au-based nanotubes through a galvanic replacement process.« less

Pentatwinned Cu Nanowires with Ultrathin Diameters below 20 nm and Their Use as Templates for the Synthesis of Au-Based Nanotubes

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

Luo, Ming; Zhou, Ming; Rosa da Silva, Robson

Here, we report a one-pot method for the facile synthesis of Cu nanowires in high purity, together with ultrathin diameters well below 20 nm. Selected area electron diffraction and high-resolution transmission electron microscopy studies confirm that the Cu nanowires are grown along the <110> direction to give pentatwinned, one-dimensional nanostructures, enclosed by five {100} facets on the side surface. A systematic study further indicates that it is critical to conduct the synthesis under an argon atmosphere in order to improve the purity and uniformity of the nanowires while keeping their diameters thinner than 20 nm. Finally, we demonstrate the usemore » of these nanowires as sacrificial templates for the synthesis of Au-based nanotubes through a galvanic replacement process.« less

Active noise canceling system for mechanically cooled germanium radiation detectors

DOEpatents

Nelson, Karl Einar; Burks, Morgan T

2014-04-22

A microphonics noise cancellation system and method for improving the energy resolution for mechanically cooled high-purity Germanium (HPGe) detector systems. A classical adaptive noise canceling digital processing system using an adaptive predictor is used in an MCA to attenuate the microphonics noise source making the system more deployable.

20171130_Ind Ergo Report_631 DI Water Movement Process.

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

Rivera, Cynthia R.

Perform an industrial ergonomic assessment to evaluate the new procedures for filling, lifting, and delivering high purity de-ionized water to building 9925. The goal was to improve on the previous method by minimizing/eliminating as much lifting and bending as possible to reduce the potential for overexertion-related injuries.

Iodine Absorption Cells Purity Testing.

PubMed

Hrabina, Jan; Zucco, Massimo; Philippe, Charles; Pham, Tuan Minh; Holá, Miroslava; Acef, Ouali; Lazar, Josef; Číp, Ondřej

2017-01-06

This article deals with the evaluation of the chemical purity of iodine-filled absorption cells and the optical frequency references used for the frequency locking of laser standards. We summarize the recent trends and progress in absorption cell technology and we focus on methods for iodine cell purity testing. We compare two independent experimental systems based on the laser-induced fluorescence method, showing an improvement of measurement uncertainty by introducing a compensation system reducing unwanted influences. We show the advantages of this technique, which is relatively simple and does not require extensive hardware equipment. As an alternative to the traditionally used methods we propose an approach of hyperfine transitions' spectral linewidth measurement. The key characteristic of this method is demonstrated on a set of testing iodine cells. The relationship between laser-induced fluorescence and transition linewidth methods will be presented as well as a summary of the advantages and disadvantages of the proposed technique (in comparison with traditional measurement approaches).

Iodine Absorption Cells Purity Testing

PubMed Central

Hrabina, Jan; Zucco, Massimo; Philippe, Charles; Pham, Tuan Minh; Holá, Miroslava; Acef, Ouali; Lazar, Josef; Číp, Ondřej

2017-01-01

This article deals with the evaluation of the chemical purity of iodine-filled absorption cells and the optical frequency references used for the frequency locking of laser standards. We summarize the recent trends and progress in absorption cell technology and we focus on methods for iodine cell purity testing. We compare two independent experimental systems based on the laser-induced fluorescence method, showing an improvement of measurement uncertainty by introducing a compensation system reducing unwanted influences. We show the advantages of this technique, which is relatively simple and does not require extensive hardware equipment. As an alternative to the traditionally used methods we propose an approach of hyperfine transitions’ spectral linewidth measurement. The key characteristic of this method is demonstrated on a set of testing iodine cells. The relationship between laser-induced fluorescence and transition linewidth methods will be presented as well as a summary of the advantages and disadvantages of the proposed technique (in comparison with traditional measurement approaches). PMID:28067834

High temperature support apparatus and method of use for casting materials

DOEpatents

Clark, Roger F; Cliber, James A; Stoddard, Nathan G; Gerber, Jesse I; Roberts, Raymond J; Wilmerton, Mark A

2015-02-10

This invention relates to a system and a method of use for large ceramic member support and manipulation at elevated temperatures in non-oxidizing atmospheres, such as using carbon-carbon composite materials for producing high purity silicon in the manufacture of solar modules. The high temperature apparatus of this invention includes one or more support ribs, one or more cross braces in combination with the one or more support ribs, and a shaped support liner positionable upon the one or more support ribs and the one or more cross braces.

Comparison of different particles and methods for magnetic isolation of circulating tumor cells

NASA Astrophysics Data System (ADS)

Sieben, S.; Bergemann, C.; Lübbe, A.; Brockmann, B.; Rescheleit, D.

2001-01-01

A more effective method for tumor cell separation from peripheral blood was established. The results of optimized magnetic particles verified by analyzing yield, purity and viability of isolated epithelial tumor cells were compared with a commercial kit for immunomagnetic cell separation. Porous silica particles of 230 nm were found to give best recovery rates and high viability of extracted cells.

Efficient generation and characterization of spectrally factorable biphotons.

PubMed

Chen, Changchen; Bo, Cao; Niu, Murphy Yuezhen; Xu, Feihu; Zhang, Zheshen; Shapiro, Jeffrey H; Wong, Franco N C

2017-04-03

Spectrally unentangled biphotons with high single-spatiotemporal-mode purity are highly desirable for many quantum information processing tasks. We generate biphotons with an inferred heralded-state spectral purity of 99%, the highest to date without any spectral filtering, by pulsed spontaneous parametric downconversion in a custom-fabricated periodically-poled KTiOPO₄ crystal under extended Gaussian phase-matching conditions. To efficiently characterize the joint spectral intensity of the generated biphotons at high spectral resolution, we employ a commercially available dispersion compensation module (DCM) with a dispersion equivalent to 100 km of standard optical fiber and with an insertion loss of only 2.8 dB. Compared with the typical method of using two temperature-stabilized equal-length fibers that incurs an insertion loss of 20 dB per fiber, the DCM approach achieves high spectral resolution in a much shorter measurement time. Because the dispersion amount and center wavelengths of DCMs can be easily customized, spectral characterization in a wide range of quantum photonic applications should benefit significantly from this technique.

Comparison of DNA extraction protocols for microbial communities from soil treated with biochar

PubMed Central

Leite, D.C.A.; Balieiro, F.C.; Pires, C.A.; Madari, B.E.; Rosado, A.S.; Coutinho, H.L.C.; Peixoto, R.S.

2014-01-01

Many studies have evaluated the effects of biochar application on soil structure and plant growth. However, there are very few studies describing the effect of biochar on native soil microbial communities. Microbial analysis of environmental samples requires accurate and reproducible methods for the extraction of DNA from samples. Because of the variety among microbial species and the strong adsorption of the phosphate backbone of the DNA molecule to biochar, extracting and purifying high quality microbial DNA from biochar-amended soil is not a trivial process and can be considerably more difficult than the extraction of DNA from other environmental samples. The aim of this study was to compare the relative efficacies of three commercial DNA extraction kits, the FastDNA® SPIN Kit for Soil (FD kit), the PowerSoil® DNA Isolation Kit (PS kit) and the ZR Soil Microbe DNA Kit Miniprep™ (ZR kit), for extracting microbial genomic DNA from sand treated with different types of biochar. The methods were evaluated by comparing the DNA yields and purity and by analysing the bacterial and fungal community profiles generated by PCR-DGGE. Our results showed that the PCR-DGGE profiles for bacterial and fungal communities were highly affected by the purity and yield of the different DNA extracts. Among the tested kits, the PS kit was the most efficient with respect to the amount and purity of recovered DNA and considering the complexity of the generated DGGE microbial fingerprint from the sand-biochar samples. PMID:24948928

Comparison of DNA extraction protocols for microbial communities from soil treated with biochar.

PubMed

Leite, D C A; Balieiro, F C; Pires, C A; Madari, B E; Rosado, A S; Coutinho, H L C; Peixoto, R S

2014-01-01

Many studies have evaluated the effects of biochar application on soil structure and plant growth. However, there are very few studies describing the effect of biochar on native soil microbial communities. Microbial analysis of environmental samples requires accurate and reproducible methods for the extraction of DNA from samples. Because of the variety among microbial species and the strong adsorption of the phosphate backbone of the DNA molecule to biochar, extracting and purifying high quality microbial DNA from biochar-amended soil is not a trivial process and can be considerably more difficult than the extraction of DNA from other environmental samples. The aim of this study was to compare the relative efficacies of three commercial DNA extraction kits, the FastDNA® SPIN Kit for Soil (FD kit), the PowerSoil® DNA Isolation Kit (PS kit) and the ZR Soil Microbe DNA Kit Miniprep™ (ZR kit), for extracting microbial genomic DNA from sand treated with different types of biochar. The methods were evaluated by comparing the DNA yields and purity and by analysing the bacterial and fungal community profiles generated by PCR-DGGE. Our results showed that the PCR-DGGE profiles for bacterial and fungal communities were highly affected by the purity and yield of the different DNA extracts. Among the tested kits, the PS kit was the most efficient with respect to the amount and purity of recovered DNA and considering the complexity of the generated DGGE microbial fingerprint from the sand-biochar samples.

High temperature thermocouple development program, part A and part B

NASA Technical Reports Server (NTRS)

Toenshoff, D. A.; Zysk, E. D.; Fleischner, P. L.

1972-01-01

The problem of extending the useful life of thermocouples intended for in-core and out-of-core thermionic applications in a vacuum environment at temperatures up to 2273 K for periods of time up to 10,000 hours was investigated. Many factors that may influence this useful life were examined, and a basic probe design was developed. With a few modifications, twenty-three thermocouple assemblies were fabricated. Generally the finished thermocouple consisted of solid doped W-3% Re and W-25% Re wires and high purity and high density BeO insulators, and was sheathed in a high purity tantalum tube. In a few probes, stranded thermocouple wires were substituted; commercial grade BeO was used; and in two cases, CVD W-22% Re tubing was used. Each of the components was made of the highest purity materials available; was subjected to special cleaning steps, and was assembled in a class 10,000 clean room. Pertinent physical and chemical properties were determined on each of the components. Special processing techniques were used in the fabrication of the high purity (99.95%), high density (over 95% of theoretical) BeO.

Recent advancements in transparent ceramics and crystal fibers for high power lasers

NASA Astrophysics Data System (ADS)

Kim, W.; Baker, C.; Villalobos, G.; Florea, C.; Gibson, D.; Shaw, L. B.; Bowman, S.; Bayya, S.; Sadowski, B.; Hunt, M.; Askins, C.; Peele, J.; Aggarwal, I. D.; Sanghera, J. S.

2013-05-01

In this paper, we present our recent progress in the development of rare-earth (Yb3+ or Ho3+) doped Lu2O3 and Y2O3 sesquioxides for high power solid state lasers. We have fabricated high quality transparent ceramics using nano-powders synthesized by a co-precipitation method. This was accomplished by developments in high purity powder synthesis and low temperature scalable sintering technology developed at NRL. The optical, spectral and morphological properties as well as the lasing performance from our highly transparent ceramics are presented. In the second part of the paper, we discuss our recent research effort in developing cladded-single crystal fibers for high power single frequency fiber lasers has the potential to significantly exceed the capabilities of existing silica fiber based lasers. Single crystal fiber cores with diameters as small as 35μm have been drawn using high purity rare earth doped ceramic or single crystal feed rods by the Laser Heated Pedestal Growth (LHPG) process. Our recent results on the development of suitable claddings on the crystal fiber core are discussed.

Green and scalable production of colloidal perovskite nanocrystals and transparent sols by a controlled self-collection process

NASA Astrophysics Data System (ADS)

Liu, Shuangyi; Huang, Limin; Li, Wanlu; Liu, Xiaohua; Jing, Shui; Li, Jackie; O'Brien, Stephen

2015-07-01

Colloidal perovskite oxide nanocrystals have attracted a great deal of interest owing to the ability to tune physical properties by virtue of the nanoscale, and generate thin film structures under mild chemical conditions, relying on self-assembly or heterogeneous mixing. This is particularly true for ferroelectric/dielectric perovskite oxide materials, for which device applications cover piezoelectrics, MEMs, memory, gate dielectrics and energy storage. The synthesis of complex oxide nanocrystals, however, continues to present issues pertaining to quality, yield, % crystallinity, purity and may also suffer from tedious separation and purification processes, which are disadvantageous to scaling production. We report a simple, green and scalable ``self-collection'' growth method that produces uniform and aggregate-free colloidal perovskite oxide nanocrystals including BaTiO3 (BT), BaxSr1-xTiO3 (BST) and quaternary oxide BaSrTiHfO3 (BSTH) in high crystallinity and high purity. The synthesis approach is solution processed, based on the sol-gel transformation of metal alkoxides in alcohol solvents with controlled or stoichiometric amounts of water and in the stark absence of surfactants and stabilizers, providing pure colloidal nanocrystals in a remarkably low temperature range (15 °C-55 °C). Under a static condition, the nanoscale hydrolysis of the metal alkoxides accomplishes a complete transformation to fully crystallized single domain perovskite nanocrystals with a passivated surface layer of hydroxyl/alkyl groups, such that the as-synthesized nanocrystals can exist in the form of super-stable and transparent sol, or self-accumulate to form a highly crystalline solid gel monolith of nearly 100% yield for easy separation/purification. The process produces high purity ligand-free nanocrystals excellent dispersibility in polar solvents, with no impurity remaining in the mother solution other than trace alcohol byproducts (such as isopropanol). The afforded stable and transparent suspension/solution can be treated as inks, suitable for printing or spin/spray coating, demonstrating great capabilities of this process for fabrication of high performance dielectric thin films. The simple ``self-collection'' strategy can be described as green and scalable due to the simplified procedure from synthesis to separation/purification, minimum waste generation, and near room temperature crystallization of nanocrystal products with tunable sizes in extremely high yield and high purity.Colloidal perovskite oxide nanocrystals have attracted a great deal of interest owing to the ability to tune physical properties by virtue of the nanoscale, and generate thin film structures under mild chemical conditions, relying on self-assembly or heterogeneous mixing. This is particularly true for ferroelectric/dielectric perovskite oxide materials, for which device applications cover piezoelectrics, MEMs, memory, gate dielectrics and energy storage. The synthesis of complex oxide nanocrystals, however, continues to present issues pertaining to quality, yield, % crystallinity, purity and may also suffer from tedious separation and purification processes, which are disadvantageous to scaling production. We report a simple, green and scalable ``self-collection'' growth method that produces uniform and aggregate-free colloidal perovskite oxide nanocrystals including BaTiO3 (BT), BaxSr1-xTiO3 (BST) and quaternary oxide BaSrTiHfO3 (BSTH) in high crystallinity and high purity. The synthesis approach is solution processed, based on the sol-gel transformation of metal alkoxides in alcohol solvents with controlled or stoichiometric amounts of water and in the stark absence of surfactants and stabilizers, providing pure colloidal nanocrystals in a remarkably low temperature range (15 °C-55 °C). Under a static condition, the nanoscale hydrolysis of the metal alkoxides accomplishes a complete transformation to fully crystallized single domain perovskite nanocrystals with a passivated surface layer of hydroxyl/alkyl groups, such that the as-synthesized nanocrystals can exist in the form of super-stable and transparent sol, or self-accumulate to form a highly crystalline solid gel monolith of nearly 100% yield for easy separation/purification. The process produces high purity ligand-free nanocrystals excellent dispersibility in polar solvents, with no impurity remaining in the mother solution other than trace alcohol byproducts (such as isopropanol). The afforded stable and transparent suspension/solution can be treated as inks, suitable for printing or spin/spray coating, demonstrating great capabilities of this process for fabrication of high performance dielectric thin films. The simple ``self-collection'' strategy can be described as green and scalable due to the simplified procedure from synthesis to separation/purification, minimum waste generation, and near room temperature crystallization of nanocrystal products with tunable sizes in extremely high yield and high purity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr02351c

Hybrid method for building extraction in vegetation-rich urban areas from very high-resolution satellite imagery

NASA Astrophysics Data System (ADS)

Jayasekare, Ajith S.; Wickramasuriya, Rohan; Namazi-Rad, Mohammad-Reza; Perez, Pascal; Singh, Gaurav

2017-07-01

A continuous update of building information is necessary in today's urban planning. Digital images acquired by remote sensing platforms at appropriate spatial and temporal resolutions provide an excellent data source to achieve this. In particular, high-resolution satellite images are often used to retrieve objects such as rooftops using feature extraction. However, high-resolution images acquired over built-up areas are associated with noises such as shadows that reduce the accuracy of feature extraction. Feature extraction heavily relies on the reflectance purity of objects, which is difficult to perfect in complex urban landscapes. An attempt was made to increase the reflectance purity of building rooftops affected by shadows. In addition to the multispectral (MS) image, derivatives thereof namely, normalized difference vegetation index and principle component (PC) images were incorporated in generating the probability image. This hybrid probability image generation ensured that the effect of shadows on rooftop extraction, particularly on light-colored roofs, is largely eliminated. The PC image was also used for image segmentation, which further increased the accuracy compared to segmentation performed on an MS image. Results show that the presented method can achieve higher rooftop extraction accuracy (70.4%) in vegetation-rich urban areas compared to traditional methods.

Effect of the microstructure on electrical properties of high-purity germanium

NASA Astrophysics Data System (ADS)

Podkopaev, O. I.; Shimanskii, A. F.; Molotkovskaya, N. O.; Kulakovskaya, T. V.

2013-05-01

The interrelation between the electrical properties and the microstructure of high-purity germanium crystals has been revealed. The electrical conductivity of polycrystalline samples increases and the life-time of nonequilibrium charge carriers in them decreases with a decrease in the crystallite sizes.

Qualification and initial characterization of a high-purity 233U spike for use in uranium analyses

DOE PAGES

Mathew, K. J.; Canaan, R. D.; Hexel, C.; ...

2015-08-20

Several high-purity 233U items potentially useful as isotope dilution mass spectrometry standards for safeguards, non-proliferation, and nuclear forensics measurements are identified and rescued from downblending. By preserving the supply of 233U materials of different pedigree for use as source materials for certified reference materials (CRMs), it is ensured that the safeguards community has high quality uranium isotopic standards required for calibration of the analytical instruments. One of the items identified as a source material for a high-purity CRM is characterized for the uranium isotope-amount ratios using thermal ionization mass spectrometry (TIMS). Additional verification measurements on this material using quadrupole inductivelymore » coupled plasma mass spectrometry (ICPMS) are also performed. As a result, the comparison of the ICPMS uranium isotope-amount ratios with the TIMS data, with much smaller uncertainties, validated the ICPMS measurement practices. ICPMS is proposed for the initial screening of the purity of items in the rescue campaign.« less

Synthesis and evaluation of L-cystathionine as a standard for amino acid analysis.

PubMed

Amino, Yusuke; Suzuki, Yumiko

2017-01-01

L-Cystathionine is a key nonprotein amino acid related to metabolic conditions. The quantitative determination of L-cystathionine in physiological fluids by amino acid analysis is important for clinical diagnosis; however, certified reference material for L-cystathionine with satisfactory purity, content, and quantity has been unavailable until recently. Consequently, a practical and simple method for the preparation of L-cystathionine was examined, which involves thioalkylation of N-tert-butoxycarbonyl-L-cysteine tert-butyl ester, derived from L-cystine, with (2S)-2-(tert-butoxycarbonyl)amino-4-iodobutanoic acid tert-butyl ester, derived from L-aspartic acid, to obtain L-cystathionine with protecting groups, followed by single-step deprotection under mild conditions. This method produces L-cystathionine in high purity (99.4%) and having sufficient percentage content according to amino acid analysis, which could be used as a standard for the amino acid analysis of physiological fluids.

Method and apparatus for hydrogen production from water

NASA Technical Reports Server (NTRS)

Muradov, Nazim Z. (Inventor)

2012-01-01

A method, apparatuses and chemical compositions are provided for producing high purity hydrogen from water. Metals or alloys capable of reacting with water and producing hydrogen in aqueous solutions at ambient conditions are reacted with one or more inorganic hydrides capable of releasing hydrogen in aqueous solutions at ambient conditions, one or more transition metal compounds are used to catalyze the reaction and, optionally, one or more alkali metal-based compounds. The metal or alloy is preferably aluminum. The inorganic hydride is from a family of complex inorganic hydrides; most preferably, NaBH.sub.4. The transition metal catalyst is from the groups VIII and IB; preferably, Cu and Fe. The alkali metal-based compounds are preferably NaOH, KOH, and the like. Hydrogen generated has a purity of at least 99.99 vol. % (dry basis), and is used without further purification in all types of fuel cells, including the polymer electrolyte membrane (PEM) fuel cell.

Large scale extraction of poly(3-hydroxybutyrate) from Ralstonia eutropha H16 using sodium hypochlorite

PubMed Central

2012-01-01

Isolation of polyhydroxyalkanoates (PHAs) from bacterial cell matter is a critical step in order to achieve a profitable production of the polymer. Therefore, an extraction method must lead to a high recovery of a pure product at low costs. This study presents a simplified method for large scale poly(3-hydroxybutyrate), poly(3HB), extraction using sodium hypochlorite. Poly(3HB) was extracted from cells of Ralstonia eutropha H16 at almost 96% purity. At different extraction volumes, a maximum recovery rate of 91.32% was obtained. At the largest extraction volume of 50 L, poly(3HB) with an average purity of 93.32% ± 4.62% was extracted with a maximum recovery of 87.03% of the initial poly(3HB) content. This process is easy to handle and requires less efforts than previously described processes. PMID:23164136

CONTINUOUS PROCESS FOR THE CONVERSION OF UF$sub 6$ TO UF$sub 4$

DOEpatents

Smiley, S.H.; Brater, D.C.; Nimmo, R.H.

1959-10-01

A method is presented for reducing UF/sub 6/ to UF/sub 6/ with hydrogen. A preheated mixture of UF/sub 6/ and fluorine is contacted with a stoichiometric excess of preheated hydrogen in a reaction chamber thereby producing UF/sub 6/. The UF/sub 6/ reacts quantitatively and the UF/sub 6/ produced is of high purity and high density.

Penetration Resistance of Armor Ceramics: Dimensional Analysis and Property Correlations

DTIC Science & Technology

2015-08-01

been reported in experimental studies. Particular ceramics analyzed here are low- and high-purity alumina, aluminum nitride, boron carbide, silicon...analyzed here are low- and high-purity alumina, aluminum nitride, boron carbide, silicon carbide, and titanium diboride. Data for penetration depth...include high hardness, high elastic stiffness, high strengths (static/dynamic compressive, shear, and bending), and low density relative to armor steels

Identification and accurate quantification of structurally related peptide impurities in synthetic human C-peptide by liquid chromatography-high resolution mass spectrometry.

PubMed

Li, Ming; Josephs, Ralf D; Daireaux, Adeline; Choteau, Tiphaine; Westwood, Steven; Wielgosz, Robert I; Li, Hongmei

2018-06-04

Peptides are an increasingly important group of biomarkers and pharmaceuticals. The accurate purity characterization of peptide calibrators is critical for the development of reference measurement systems for laboratory medicine and quality control of pharmaceuticals. The peptides used for these purposes are increasingly produced through peptide synthesis. Various approaches (for example mass balance, amino acid analysis, qNMR, and nitrogen determination) can be applied to accurately value assign the purity of peptide calibrators. However, all purity assessment approaches require a correction for structurally related peptide impurities in order to avoid biases. Liquid chromatography coupled to high resolution mass spectrometry (LC-hrMS) has become the key technique for the identification and accurate quantification of structurally related peptide impurities in intact peptide calibrator materials. In this study, LC-hrMS-based methods were developed and validated in-house for the identification and quantification of structurally related peptide impurities in a synthetic human C-peptide (hCP) material, which served as a study material for an international comparison looking at the competencies of laboratories to perform peptide purity mass fraction assignments. More than 65 impurities were identified, confirmed, and accurately quantified by using LC-hrMS. The total mass fraction of all structurally related peptide impurities in the hCP study material was estimated to be 83.3 mg/g with an associated expanded uncertainty of 3.0 mg/g (k = 2). The calibration hierarchy concept used for the quantification of individual impurities is described in detail. Graphical abstract ᅟ.

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

Boussaa, S. Anas, E-mail: sabiha.anas@gmail.com; Kheloufi, A.; Kefaifi, A.

Raw materials are essential for the functioning of modern societies, and access to these raw materials is vital to the world economy. Sustainable development, both globally level, raises important new challenges associated with access and efficient use of raw materials. High purity quartz, is consider as a critical raw material and it is a rare commodity that only forms under geological conditions where a narrow set of chemical and physical parameters is fulfilled. When identified and following special beneficiation techniques, high purity quartz obtains very attractive prices and is applied in high technology sectors that currently are under rapid expansionmore » such as photovoltaic solar cells, silicon metal - oxide wafers in the semiconductor industry and long distance optical fibers that are used in communication networks. Crystalline silicon remains the principal material for photovoltaic technology. Metallurgical silicon is produced industrially by the reduction of silica with carbon in an electric arc furnace at temperatures higher than 2000 °C in the hottest parts, by a reaction that can be written ideally as: SiO{sub 2} + 2C = Si + 2CO. The aim of this study has been to test experimental methods for investigating the various physical and chemical proprieties of Hoggar quartz with different techniques: X Ray Fluorescence, infra-red spectroscopy, Scanning Electron Microscopy, Optic Microscopy, Carbon Analyzer and Vickers Hardness. The results show finally that the quartz has got good result in purity but need enrichment for the photovoltaic application.« less

Use of low-cost aluminum in electric energy production

NASA Astrophysics Data System (ADS)

Zhuk, Andrey Z.; Sheindlin, Alexander E.; Kleymenov, Boris V.; Shkolnikov, Eugene I.; Lopatin, Marat Yu.

Suppression of the parasitic corrosion while maintaining the electrochemical activity of the anode metal is one of the serious problems that affects the energy efficiency of aluminum-air batteries. The need to use high-purity aluminum or special aluminum-based alloys results in a significant increase in the cost of the anode, and thus an increase in the total cost of energy generated by the aluminum-air battery, which narrows the range of possible applications for this type of power source. This study considers the process of parasitic corrosion as a method for hydrogen production. Hydrogen produced in an aluminum-air battery by this way may be further employed in a hydrogen-air fuel cell (Hy-air FC) or in a heat engine, or it may be burnt to generate heat. Therefore, anode materials may be provided by commercially pure aluminum, commercially produced aluminum alloys, and secondary aluminum. These materials are much cheaper and more readily available than special anode alloys of aluminum and high-purity aluminum. The aim of present study is to obtain experimental data for comparison of energy and cost parameters of some commercially produced aluminum alloys, of high-purity aluminum, and of a special Al-ln anode alloy in the context of using these materials as anodes for an Al-air battery and for combined production of electrical power and hydrogen.

Hydrogen recovery from the thermal plasma gasification of solid waste.

PubMed

Byun, Youngchul; Cho, Moohyun; Chung, Jae Woo; Namkung, Won; Lee, Hyeon Don; Jang, Sung Duk; Kim, Young-Suk; Lee, Jin-Ho; Lee, Carg-Ro; Hwang, Soon-Mo

2011-06-15

Thermal plasma gasification has been demonstrated as one of the most effective and environmentally friendly methods for solid waste treatment and energy utilization in many of studies. Therefore, the thermal plasma process of solid waste gasification (paper mill waste, 1.2 ton/day) was applied for the recovery of high purity H(2) (>99.99%). Gases emitted from a gasification furnace equipped with a nontransferred thermal plasma torch were purified using a bag-filter and wet scrubber. Thereafter, the gases, which contained syngas (CO+H(2)), were introduced into a H(2) recovery system, consisting largely of a water gas shift (WGS) unit for the conversion of CO to H(2) and a pressure swing adsorption (PSA) unit for the separation and purification of H(2). It was successfully demonstrated that the thermal plasma process of solid waste gasification, combined with the WGS and PSA, produced high purity H(2) (20 N m(3)/h (400 H(2)-Nm(3)/PMW-ton), up to 99.99%) using a plasma torch with 1.6 MWh/PMW-ton of electricity. The results presented here suggest that the thermal plasma process of solid waste gasification for the production of high purity H(2) may provide a new approach as a future energy infrastructure based on H(2). Copyright © 2011 Elsevier B.V. All rights reserved.

NIST-Traceable NMR Method to Determine Quantitative Weight Percentage Purity of Mustard (HD) Feedstock Samples

DTIC Science & Technology

2018-01-01

ECBC-TR-1506 NIST-TRACEABLE NMR METHOD TO DETERMINE QUANTITATIVE WEIGHT PERCENTAGE PURITY OF MUSTARD (HD) FEEDSTOCK SAMPLES David J...McGarvey RESEARCH AND TECHNOLOGY DIRECTORATE William R. Creasy LEIDOS, INC. Abingdon, MD 21009-1261 Theresa R. Connell EXCET, INC...be construed as an official Department of the Army position unless so designated by other authorizing documents. REPORT DOCUMENTATION PAGE

Measurement scheme for purity based on two two-body gates

NASA Astrophysics Data System (ADS)

Nakazato, H.; Tanaka, T.; Yuasa, K.; Florio, G.; Pascazio, S.

2012-04-01

A scheme for measuring the purity of a quantum system with a finite number of levels is presented. The method makes use of two swap gates and hinges only on measurements performed on a reference system, prepared in a certain pure state and coupled with the target system. Neither tomographic methods, with the complete reconstruction of the state, nor interferometric setups are needed.

Analysis and Characterization of High-Purity Talc for Use in Propellants; Determination of Talc in Propellants

DTIC Science & Technology

1975-12-01

is determined by combustion in an induction furnace with iron as a flux. The methods for moisture, loss in ignition, water-soluble matter, acid... determination of talc in nitro- cellulose-base propellants. The first method (which is the method recom- mended for the usual nitrocellulose -base...In the present report an improved scheme is proposed for the analysis of talc. The silica and magnesium oxide are determined by fusion with sodium

Preparative isolation and purification of capsaicin and dihydrocapsaicin from Capsici Fructus using supercritical fluid extraction combined with high speed countercurrent chromatography.

PubMed

Yan, Rongwei; Zhao, Leilei; Tao, Junfei; Zou, Yong; Xu, Xinjun

2018-05-01

Supercritical fluid extraction with CO 2 (SFE-CO 2 ) was utilized for extraction of capsaicin (CA) and dihydrocapsaicin (DHCA) from Capsici Fructus, and then a two-step enrichment method for separating capsaicinoids from SFE-CO 2 extracts was developed. The process involved extraction with aqueous methanol and crystallization by alkali extraction and acid precipitation. Finally, a consecutive high-speed countercurrent chromatography (HSCCC) separation method was successfully applied in the purification of CA and DHCA from capsaicinoid crystal. The extraction pressure, extraction temperature and volume of co-solvent were optimized at 33 MPa, 41 °C and 75 mL, respectively, using response surface methodology; the extraction rates of CA and DHCA were about 93.18% and 93.49%, respectively. 407.43 mg capsaicinoid crystal was isolated from the SFE-CO 2 extracts obtained from 100 g capsicum powder by the two-step enrichment method. About 506 mg and 184 mg CA and DHCA with purities up to 98.31% and 96.68%, respectively, were obtained from 1 g capsaicinoid crystal in one HSCCC of three consecutive sample loadings without exchanging any solvent system. This method comprising SFE-CO 2 , a two-step enrichment and HSCCC was efficient, powerful and practical for the large-scale preparation of CA and DHCA from Capsici Fructus with high purity and high yield. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Optimization of Ultrasonic-Microwave Synergistic Extraction of Ricinine from Castor Cake by Response Surface Methodology.

PubMed

Xu, Wei; Yan, Xiuhua; Shao, Rong; Chen, Ligen; Ke, Zengguang

Castor cake is the residue in castor oil production in which many active components exist and the major one among them is ricinine. In this study, optimization of extraction of ricinine from castor cake using ultrasonic-microwave synergistic extraction (UMSE) was investigated to obtain high yield and purity by Box-Behnken design (BBD) response surface design. The optimal conditions of extraction were: ultrasound power 342 W, extracting time 5 min, microwave power 395 W, and non-significant factor of liquid/solid ratio 1:10. The crude extraction was recrystallized from ethanol. As a result, the maximum yield of ricinine was approximately 67.52%. The purity of ricinine was 99.39% which was determined by high performance liquid chromatography (HPLC). Additionally, the structure of purified ricinine was identified by fourier transforms infrared (FTIR) and liquid chromatography-mass spectrometry (LC-MS). Scanning electron microscope (SEM) was used to characterize the prismatic crystals morphology of ricinine. Results demonstrated that the present method combined the advantages of ultrasonic extraction and microwave extraction, which is time-saving with high extraction yield. Our results offer a suitable method for large-scale isolation of ricinine.

[Isolation, purification and primary culture of adult mouse cardiac fibroblasts].

PubMed

Li, Rujun; Gong, Kaizheng; Zhang, Zhengang

2017-01-01

Objective To establish a method for primary culture of adult mouse cardiac fibroblasts. Methods Myocardial tissues from adult mice were digested with 1 g/L trypsin and 0.8 g/L collagenase IV by oscillating water bath for a short time repeatedly. Cardiac fibroblasts and myocardial cells were isolated with differential adhesion method. Immunofluorescence staining was used to assess the purity of cardiac fibroblasts. The cell morphology was observed under an inverted phase contrast microscope. The proliferation of cardiac fibroblasts was analyzed by growth curve and CCK-8 assay. The Smad2/3 phosphorylation induced by TGF-β1 was detected by Western blotting. Results After 90 minutes of differential adhesion, adherent fibroblasts formed spherical cell mass and after 3 days, cells were spindle-shaped and proliferated rapidly. Cells were confluent after 5 days and the growth curve presented nearly "S" shape. The positive expression rate of vimentin was 95%. CCK-8 assay showed that the optimal cell proliferating activity was found from day 3 to day 5. The level of phosphorylated Smad2/3 obviously increased at the second passage induced by TGF-β1. Conclusion This method is economical and stable to isolate cardiac fibroblasts with high activity and high purity from adult mice.

Preparative separation and identification of novel subsidiary colors of the color additive D&C Red No. 33 (Acid Red 33) using spiral high-speed counter-current chromatography☆

PubMed Central

Weisz, Adrian; Ridge, Clark D.; Mazzola, Eugene P.; Ito, Yoichiro

2015-01-01

Three low-level subsidiary color impurities (A, B, and C) often present in batches of the color additive D&C Red No. 33 (R33, Acid Red 33, Colour Index No. 17200) were separated from a portion of R33 by spiral high-speed counter-current chromatography (HSCCC). The separation involved use of a very polar solvent system, 1-BuOH/5 mM aq. (NH4)2SO4. Addition of ammonium sulfate to the lower phase forced partition of the components into the upper phase, thereby eliminating the need to add a hydrophobic counterion as was previously required for separations of components from sulfonated dyes. The very polar solvent system used would not have been retained in a conventional multi-layer coil HSCCC instrument, but the spiral configuration enabled retention of the stationary phase, and thus, the separation was possible. A 1 g portion of R33 enriched in A, B, and C was separated using the upper phase of the solvent system as the mobile phase. The retention of the stationary phase was 38.1%, and the separation resulted in 4.8 mg of A of >90% purity, 18.3 mg of B of >85% purity, and 91 mg of C of 65–72% purity. A second separation of a portion of the C mixture resulted in 7 mg of C of >94% purity. The separated impurities were identified by high-resolution mass spectrometry and NMR spectroscopic techniques as follows: 5-amino-3-biphenyl-3-ylazo-4-hydroxy-naphthalene-2,7-disulfonic acid, A; 5-amino-4-hydroxy-6-phenyl-3-phenylazo-naphthalene-2,7-disulfonic acid, B; and 5-amino-4-hydroxy-3,6-bis-phenylazo-naphthalene-2,7-disulfonic acid, C. The isomers A and B are compounds reported for the first time. Application of the spiral HSCCC method resulted in the additional benefit of yielding 930 mg of the main component of R33, 5-amino-4-hydroxy-3-phenylazo-naphthalene-2,7-disulfonic acid, of >97% purity. PMID:25591404

Preparative separation and identification of novel subsidiary colors of the color additive D&C Red No. 33 (Acid Red 33) using spiral high-speed counter-current chromatography.

PubMed

Weisz, Adrian; Ridge, Clark D; Mazzola, Eugene P; Ito, Yoichiro

2015-02-06

Three low-level subsidiary color impurities (A, B, and C) often present in batches of the color additive D&C Red No. 33 (R33, Acid Red 33, Colour Index No. 17200) were separated from a portion of R33 by spiral high-speed counter-current chromatography (HSCCC). The separation involved use of a very polar solvent system, 1-BuOH/5mM aq. (NH4)2SO4. Addition of ammonium sulfate to the lower phase forced partition of the components into the upper phase, thereby eliminating the need to add a hydrophobic counterion as was previously required for separations of components from sulfonated dyes. The very polar solvent system used would not have been retained in a conventional multi-layer coil HSCCC instrument, but the spiral configuration enabled retention of the stationary phase, and thus, the separation was possible. A 1g portion of R33 enriched in A, B, and C was separated using the upper phase of the solvent system as the mobile phase. The retention of the stationary phase was 38.1%, and the separation resulted in 4.8 mg of A of >90% purity, 18.3mg of B of >85% purity, and 91 mg of C of 65-72% purity. A second separation of a portion of the C mixture resulted in 7 mg of C of >94% purity. The separated impurities were identified by high-resolution mass spectrometry and NMR spectroscopic techniques as follows: 5-amino-3-biphenyl-3-ylazo-4-hydroxy-naphthalene-2,7-disulfonic acid, A; 5-amino-4-hydroxy-6-phenyl-3-phenylazo-naphthalene-2,7-disulfonic acid, B; and 5-amino-4-hydroxy-3,6-bis-phenylazo-naphthalene-2,7-disulfonic acid, C. The isomers A and B are compounds reported for the first time. Application of the spiral HSCCC method resulted in the additional benefit of yielding 930 mg of the main component of R33, 5-amino-4-hydroxy-3-phenylazo-naphthalene-2,7-disulfonic acid, of >97% purity. Published by Elsevier B.V.

Measurement of energy transitions for the decay radiations of 75Ge and 69Ge in a high purity germanium detector

NASA Astrophysics Data System (ADS)

Aydın, Güral; Usta, Metin; Oktay, Adem

2018-06-01

Photoactivation experiments have a wide range of application areas in nuclear, particle physics, and medical physics such as measuring energy levels and half-lifes of nuclei, experiments for understanding imaging methods in medicine, isotope production for patient treatment, radiation security and transportation, radiation therapy, and astrophysics processes. In this study, some energy transition values of the decay radiations of 75Ge and 69Ge, which are the products of photonuclear reactions (γ, n) with germanium isotopes (75Ge and 69Ge), were measured. The gamma spectrum as a result of atomic transitions were analysed by using a high purity semiconductor germanium detector and the energy transition values which are presented here were compared with the ones which are the best in literature. It was observed that the results presented are in agreement with literature in error range and some results have better precisions.

Isolation and Purification of Two Isoflavones from Hericium erinaceum Mycelium by High-Speed Counter-Current Chromatography.

PubMed

He, Jinzhe; Fan, Peng; Feng, Simin; Shao, Ping; Sun, Peilong

2018-03-02

High-speed counter-current chromatography (HSCCC) was used to separate and purify two isoflavones for the first time from Hericium erinaceum ( H. erinaceum ) mycelium using a two-phase solvent system composed of chloroform-dichloromethane-methanol-water (4:2:3:2, v / v / v / v ). These two isoflavones were identified as genistein (4',5,7-trihydroxyisoflavone, C 15 H 10 O₅) and daidzein (4',7-dihydroxyisoflavone, C 15 H 10 O₄), using infrared spectroscopy (IR), electro-spary ionisation mass (ESI-MS), ¹H-nuclear magnetic resonance (NMR) and 13 C-NMR spectra. About 23 mg genistein with 95.7% purity and 18 mg daidzein with 97.3% purity were isolated from 150 mg ethanolic extract of H. erinaceum mycelium. The results demonstrated that HSCCC was a feasible method to separate and purify genistein and daidzein from H. erinaceum mycelium.

Electrochemical study of aluminum corrosion in boiling high purity water

NASA Technical Reports Server (NTRS)

Draley, J. E.; Legault, R. A.

1969-01-01

Electrochemical study of aluminum corrosion in boiling high-purity water includes an equation relating current and electrochemical potential derived on the basis of a physical model of the corrosion process. The work involved an examination of the cathodic polarization behavior of 1100 aluminum during aqueous oxidation.

URANIUM COMPOSITIONS

DOEpatents

Allen, N.P.; Grogan, J.D.

1959-05-12

This patent relates to high purity uranium alloys characterized by improved stability to thermal cycling and low thermal neutron absorption. The high purity uranium alloy contains less than 0.1 per cent by weight in total amount of any ore or more of the elements such as aluminum, silicon, phosphorous, tin, lead, bismuth, niobium, and zinc.

Proximity to the US-Mexico border: a key to explaining geographic variation in US methamphetamine, cocaine and heroin purity.

PubMed

Cunningham, James K; Maxwell, Jane Carlisle; Campollo, Octavio; Cunningham, Kathryn I; Liu, Lon-Mu; Lin, Hui-Lin

2010-10-01

Although illicit drug purity is a widely discussed health risk, research explaining its geographic variation within a country is rare. This study examines whether proximity to the US-Mexico border, the United States' primary drug import portal, is associated with geographic variation in US methamphetamine, heroin and cocaine purity. Distances (proximity) between the US-Mexico border and locations of methamphetamine, cocaine and heroin seizures/acquisitions (n = 239,070) recorded in STRIDE (System to Retrieve Information from Drug Evidence) were calculated for the period of 1990-2004. The association of drug purity with these distances and other variables, including time and seizure/acquisition size, was examined using hierarchical multivariate linear modeling (HMLM). Coterminous United States. Methamphetamine, cocaine and heroin purity generally decreased with distance from the US-Mexico border. Heroin purity, however, after initially declining with distance, turned upwards-a U-shaped association. During 2000-04, methamphetamine purity also had a U-shaped association with distance. For each of the three drugs, temporal changes in the purity of small acquisitions (<10 g) were typically more dynamic in areas closer to the US-Mexico border. Geographic variance in methamphetamine, cocaine and heroin purity throughout the coterminous United States was associated with US-Mexico border proximity. The U-shaped associations between border-distance and purity for heroin and methamphetamine may be due to imports of those drugs via the eastern United States and southeast Canada, respectively. That said, areas closer to the US-Mexico border generally had relatively high illicit drug purity, as well as more dynamic change in the purity of small ('retail level') drug amounts. © 2010 The Authors, Addiction © 2010 Society for the Study of Addiction.

Flow cytometric sorting of fresh and frozen-thawed spermatozoa in the western lowland gorilla (Gorilla gorilla gorilla).

PubMed

O'Brien, J K; Stojanov, T; Crichton, E G; Evans, K M; Leigh, D; Maxwell, W M C; Evans, G; Loskutoff, N M

2005-08-01

We adapted flow cytometry technology for high-purity sorting of X chromosome-bearing spermatozoa in the western lowland gorilla (Gorilla gorilla gorilla). Our objectives were to develop methodologies for liquid storage of semen prior to sorting, sorting of liquid-stored and frozen-thawed spermatozoa, and assessment of sorting accuracy. In study 1, the in vitro sperm characteristics of gorilla ejaculates from one male were unchanged (P > 0.05) after 8 hr of liquid storage at 15 degrees C in a non-egg yolk diluent (HEPES-buffered modified Tyrode's medium). In study 2, we examined the efficacy of sorting fresh and frozen-thawed spermatozoa using human spermatozoa as a model for gorilla spermatozoa. Ejaculates from one male were split into fresh and frozen aliquots. X-enriched samples derived from both fresh and frozen-thawed human semen were of high purity, as determined by fluorescence in situ hybridization (FISH; 90.7%+/-2.3%, overall), and contained a high proportion of morphologically normal spermatozoa (86.0%+/-1.0%, overall). In study 3, we processed liquid-stored semen from two gorillas for sorting using a modification of methods for human spermatozoa. The sort rate for enrichment of X-bearing spermatozoa was 7.3+/-2.5 spermatozoa per second. The X-enriched samples were of high purity (single-sperm PCR: 83.7%) and normal morphology (79.0%+/-3.9%). In study 4 we examined frozen-thawed gorilla semen, and the sort rate (8.3+/-2.9 X-bearing sperm/sec), purity (89.7%), and normal morphology (81.4%+/-3.4%) were comparable to those of liquid-stored semen. Depending on the male and the type of sample used (fresh or frozen-thawed), 0.8-2.2% of gorilla spermatozoa in the processed ejaculate were present in the X-enriched sample. These results demonstrate that fresh or frozen-thawed gorilla spermatozoa can be flow cytometrically sorted into samples enriched for X-bearing spermatozoa. Copyright 2005 Wiley-Liss, Inc.

The radioisotope complex project “RIC-80” at the Petersburg Nuclear Physics Institute

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

Panteleev, V. N., E-mail: vnp@pnpi.spb.ru; Barzakh, A. E.; Batist, L. Kh.

2015-12-15

The high current cyclotron C-80 capable of producing 40-80 MeV proton beams with a current of up to 200 μA has been constructed at Petersburg Nuclear Physics Institute. One of the main goals of the C-80 is the production of a wide spectrum of medical radionuclides for diagnostics and therapy. The project development of the radioisotope complex RIC-80 (radioisotopes at the cyclotron C-80) at the beam of C-80 has been completed. The RIC-80 complex is briefly discussed in this paper. The combination of the mass-separator with the target-ion source device, available at one of the new target stations for on-linemore » or semi on-line production of a high purity separated radioisotopes, is explored in greater detail. The results of target and ion source tests for a mass-separator method for the production of high purity radioisotopes {sup 82}Sr and {sup 223,224}Ra are also presented.« less

Industrial-scale separation of high-purity single-chirality single-wall carbon nanotubes for biological imaging

PubMed Central

Yomogida, Yohei; Tanaka, Takeshi; Zhang, Minfang; Yudasaka, Masako; Wei, Xiaojun; Kataura, Hiromichi

2016-01-01

Single-chirality, single-wall carbon nanotubes are desired due to their inherent physical properties and performance characteristics. Here, we demonstrate a chromatographic separation method based on a newly discovered chirality-selective affinity between carbon nanotubes and a gel containing a mixture of the surfactants. In this system, two different selectivities are found: chiral-angle selectivity and diameter selectivity. Since the chirality of nanotubes is determined by the chiral angle and diameter, combining these independent selectivities leads to high-resolution single-chirality separation with milligram-scale throughput and high purity. Furthermore, we present efficient vascular imaging of mice using separated single-chirality (9,4) nanotubes. Due to efficient absorption and emission, blood vessels can be recognized even with the use of ∼100-fold lower injected dose than the reported value for pristine nanotubes. Thus, 1 day of separation provides material for up to 15,000 imaging experiments, which is acceptable for industrial use. PMID:27350127

The radioisotope complex project "RIC-80" at the Petersburg Nuclear Physics Institute.

PubMed

Panteleev, V N; Barzakh, A E; Batist, L Kh; Fedorov, D V; Ivanov, V S; Moroz, F V; Molkanov, P L; Orlov, S Yu; Volkov, Yu M

2015-12-01

The high current cyclotron C-80 capable of producing 40-80 MeV proton beams with a current of up to 200 μA has been constructed at Petersburg Nuclear Physics Institute. One of the main goals of the C-80 is the production of a wide spectrum of medical radionuclides for diagnostics and therapy. The project development of the radioisotope complex RIC-80 (radioisotopes at the cyclotron C-80) at the beam of C-80 has been completed. The RIC-80 complex is briefly discussed in this paper. The combination of the mass-separator with the target-ion source device, available at one of the new target stations for on-line or semi on-line production of a high purity separated radioisotopes, is explored in greater detail. The results of target and ion source tests for a mass-separator method for the production of high purity radioisotopes (82)Sr and (223,224)Ra are also presented.

Target materials for exotic ISOL beams

NASA Astrophysics Data System (ADS)

Gottberg, A.

2016-06-01

The demand for intensity, purity, reliability and availability of short-lived isotopes far from stability is steadily high, and considerably exceeding the supply. In many cases the ISOL (Isotope Separation On-Line) method can provide beams of high intensity and purity. Limitations in terms of accessible chemical species and minimum half-life are driven mainly by chemical reactions and physical processes inside of the thick target. A wide range of materials are in use, ranging from thin metallic foils and liquids to refractory ceramics, while poly-phasic mixed uranium carbides have become the reference target material for most ISOL facilities world-wide. Target material research and development is often complex and especially important post-irradiation analyses are hindered by the high intrinsic radiotoxicity of these materials. However, recent achievements have proven that these investigations are possible if the effort of different facilities is combined, leading to the development of new material matrices that can supply new beams of unprecedented intensity and beam current stability.

Absolute sulfur isotope amount ratios in two batches of high purity SO2 gas: sulfur isotope reference materials IRMM-2012 and IRMM-2013

NASA Astrophysics Data System (ADS)

Valkiers, S.; Ding, T.; Ruße, K.; de Bièvre, P.; Taylor, P. D. P.

2005-04-01

SI-traceable ("absolute") values have been obtained for sulfur isotope amount ratios n(33S)/n(32S) and n(34S)/n(32S), in two batches of high purity SO2 gas (IRMM-2012 and IRMM-2013). The SO2 gas was converted at IMR-Beijing to Ag2S, then fluorinated to SF6 gas both at IMR-Beijing and at IRMM-Geel. Yields of different conversion methods exceeded 99%. The sulfur amount-of-substance measurements were performed by gas mass spectrometry on SF5+ ions using "IRMM's amount comparator II". These isotope amount ratios were calibrated by means of gravimetrically prepared synthetic mixtures of highly enriched sulfur isotopes (32S, 33S and 34S) in Ag2S form. The ratio values in the SO2 Secondary Measurement Standard are traceable to the SI system. They can be used in the calibration of field sulfur isotope measurements thus making these metrologically traceable to the SI.

[Study of purity tests for silicone resins].

PubMed

Sato, Kyoko; Otsuki, Noriko; Ohori, Akio; Chinda, Mitsuru; Furusho, Noriko; Osako, Tsutomu; Akiyama, Hiroshi; Kawamura, Yoko

2012-01-01

In the 8th edition of Japan's Specifications and Standards for Food Additives, the purity test for silicone resins requires the determination of the refractive index and kinetic viscosity of the extracted silicone oil, and allows for only a limited amount of silicon dioxide. In the purity test, carbon tetrachloride is used to separate the silicone oil and silicon dioxide. To exclude carbon tetrachloride, methods were developed for separating the silicone oil and silicon dioxide from silicone resin, which use hexane and 10% n-dodecylbenzenesulfonic acid in hexane. For silicone oil, the measured refractive index and kinetic viscosity of the silicone oil obtained from the hexane extract were shown to be equivalent to those of the intact silicone oil. In regard to silicon dioxide, it was confirmed that, following the separation with 10% n-dodecylbenzenesulfonic acid in hexane, the level of silicon dioxide in silicone resin can be accurately determined. Therefore, in this study, we developed a method for testing the purity of silicone resins without the use of carbon tetrachloride, which is a harmful reagent.

Synthesis and Primary Characterization of Self-Assembled Peptide-Based Hydrogels

PubMed Central

Nagarkar, Radhika P.; Schneider, Joel P.

2009-01-01

Summary Hydrogels based on peptide self-assembly form an important class of biomaterials that find application in tissue engineering and drug delivery. It is essential to prepare peptides with high purity to achieve batch-to-batch consistency affording hydrogels with reproducible properties. Automated solid-phase peptide synthesis coupled with optimized Fmoc (9-fluorenylmethoxycarbonyl) chemistry to obtain peptides in high yield and purity is discussed. Details of isolating a desired peptide from crude synthetic mixtures and assessment of the peptide’s final purity by high-performance liquid chromatography and mass spectrometry are provided. Beyond the practical importance of synthesis and primary characterization, techniques used to investigate the properties of hydrogels are briefly discussed. PMID:19031061

Purification and crystal growth of NPB via imidazolium based ionic liquids

NASA Astrophysics Data System (ADS)

Oh, Yong-Taeg; Shin, Dong-Chan

2018-04-01

Here we report the production of high purity and crystallinity organic electronic material of NPB (N,N‧-Di-[(1-naphthyl)-N,N‧-diphenyl]-1,1‧-biphenyl-4,4‧-diamine (C44H32N2) through solution recrystallization within imidazolium based ionic liquids. When low purity NPB was recrystallized at 170 °C within C8MIM[TFSI], its purity was drastically improved from 82% to 99.92%. These recrystallized NPB crystals showed 0.040° FWHM (Full Width Half Maximum) of X-ray (1 1 1) diffraction peak. Such small FWHM angle indicates single-crystal like crystallinity. Initial NPB powder was dissolved at 100 °C and recrystallized at temperature above 110 °C. At higher temperature of 170 °C, a small number of bigger crystals were formed compared to those at 110 °C. This can be well explained by the classical nucleation and growth theory. Therefore, solution recrystallization process using ionic liquid might be promising for mass production of organic electronic materials by replacing the widely-used sublimation purification method.

Optimal quality (131)I-monoclonal antibodies on high-dose labeling in a large reaction volume and temporarily coating the antibody with IODO-GEN.

PubMed

Visser, G W; Klok, R P; Gebbinck, J W; ter Linden, T; van Dongen, G A; Molthoff, C F

2001-03-01

A novel, facile procedure for efficient coupling of high doses of (131)I to monoclonal antibodies (MAbs) was developed with minimal chemical and radiation damage. To diminish the radiation and chemical burden during labeling, iodination was performed in a large reaction volume and by temporarily coating the MAb with a minimal amount of IODO-GEN. The MAb was coated by injection of IODO-GEN (dissolved in acetonitrile [MeCN]) into the aqueous MAb solution, and the coating was subsequently removed by addition of ascorbic acid. For chemoprotection before, during, and after PD-10 purification of the (131)I-MAbs, ascorbic acid and human serum albumin were used. The effects of autoradiolysis in the starting (131)I solution were countered by treatment with NaOH and ascorbic acid. For this so-called IODO-GEN-coated MAb method, the sensitive chimeric MAb MOv18 (c-MOv18) and the more robust murine MAbs K928 and E48 were used. The high-dose (131)I-labeled MAbs were characterized for radiochemical purity and MAb integrity by thin-layer chromatography, high-performance liquid chromatography, and sodium dodecyl sulfate polyacrylamide gel electrophoresis followed by phosphor imager quantification. The high-dose (131)I-labeled MAbs were also characterized for immunoreactivity. The radiopharmacokinetics and biodistribution of (131)I-c-MOv18 were analyzed in human tumor-bearing nude mice. For comparison, (131)I-c-MOv18 batches were made using the conventional chloramine-T or IODO-GEN-coated vial method. Conventional high-dose labeling of 5 mg c-MOv18 with 4.4 GBq (131)I resulted in a labeling yield of 60%, a radiochemical purity of 90%, an immunoreactive fraction of 25% (72% being the maximum in the assay used), and the presence of aggregation and degradation products. Using similar amounts of (131)I and MAb in the IODO-GEN-coated MAb method, 85%-89% overall radiochemical yield, at least 99.7% radiochemical purity, and full preservation of MAb integrity and immunoreactivity were achieved. For this labeling, 5 mg MAb were coated with 35 microg IODO-GEN during 3 min in a reaction volume of 6 mL. Also, biodistribution was optimal, and tumor accumulation was superior to that of coinjected (125)I-c-MOv18 labeled according to the conventional IODO-GEN-coated vial method. A new, facile, high-dose (131)I-labeling method was developed for production of (131)I-labeled MAbs with optimal quality for use in clinical radioimmunotherapy.

Dynamic Exergy Method for Evaluating the Control and Operation of Oxy-Combustion Boiler Island Systems.

PubMed

Jin, Bo; Zhao, Haibo; Zheng, Chuguang; Liang, Zhiwu

2017-01-03

Exergy-based methods are widely applied to assess the performance of energy conversion systems; however, these methods mainly focus on a certain steady-state and have limited applications for evaluating the control impacts on system operation. To dynamically obtain the thermodynamic behavior and reveal the influences of control structures, layers and loops, on system energy performance, a dynamic exergy method is developed, improved, and applied to a complex oxy-combustion boiler island system for the first time. The three most common operating scenarios are studied, and the results show that the flow rate change process leads to less energy consumption than oxygen purity and air in-leakage change processes. The variation of oxygen purity produces the largest impact on system operation, and the operating parameter sensitivity is not affected by the presence of process control. The control system saves energy during flow rate and oxygen purity change processes, while it consumes energy during the air in-leakage change process. More attention should be paid to the oxygen purity change because it requires the largest control cost. In the control system, the supervisory control layer requires the greatest energy consumption and the largest control cost to maintain operating targets, while the steam control loops cause the main energy consumption.

Development of Advanced Materials for Electro-Ceramic Application Final Report CRADA No. TC-1331-96

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

Caplan, M.; Olstad, R.; McMillan, L.

The goal of this project was to further develop and characterize the electrochemical methods originating in Russia for producing ultra high purity organometallic compounds utilized as precursors in the production of high quality electro-ceramic materials. Symetrix planned to use electro-ceramic materials with high dielectric constant for microelectronic memory circuit applications. General Atomics planned to use the barium titanate type ceramics with low loss tangent for producing a high power ferroelectric tuner used to match radio frequency power into their Dill-D fusion machine. Phase I of the project was scheduled to have a large number of organometallic (alkoxides) chemical samples producedmore » using various methods. These would be analyzed by LLNL, Soliton and Symetrix independently to determine the level of chemical impurities thus verifying each other's analysis. The goal was to demonstrate a cost-effective production method, which could be implemented in a large commercial facility to produce high purity organometallic compounds. In addition, various compositions of barium-strontium-titanate ceramics were to be produced and analyzed in order to develop an electroceramic capacitor material having the desired characteristics with respect to dielectric constant, loss tangent, temperature characteristics and non-linear behavior under applied voltage. Upon optimizing the barium titanate material, 50 capacitor preforms would be produced from this material demonstrating the ability to produce, in quantity, the pills ultimately required for the ferroelectric tuner (approx 2000-3000 ceramic pills).« less

Mechanical Properties of a High Lead Glass Used in the Mars Organic Molecule Analyzer

NASA Technical Reports Server (NTRS)

Salem, Jonathan A.; Smith, Nathan A.; Ersahin, Akif

2015-01-01

The elastic constants, strength, fracture toughness, slow crack growth parameters, and mirror constant of a high lead glass supplied as tubes and funnels were measured using ASTM International (formerly ASTM, American Society for Testing and Materials) methods and modifications thereof. The material exhibits lower Young's modulus and slow crack growth exponent as compared to soda-lime silica glass. Highly modified glasses exhibit lower fracture toughness and slow crack growth exponent than high purity glasses such as fused silica.

Synthesis of Silane and Silicon in a Non-equilibrium Plasma Jet

NASA Technical Reports Server (NTRS)

Calcote, H. F.

1978-01-01

The original objective of this program was to determine the feasibility of high volume, low-cost production of high purity silane or solar cell grade silicon using a non equilibrium plasma jet. The emphasis was changed near the end of the program to determine the feasibility of preparing photovoltaic amorphous silicon films directly using this method. The non equilibrium plasma jet should be further evaluated as a technique for producing high efficiency photovoltaic amorphous silicon films.

Low-cost high purity production

NASA Technical Reports Server (NTRS)

Kapur, V. K.

1978-01-01

Economical process produces high-purity silicon crystals suitable for use in solar cells. Reaction is strongly exothermic and can be initiated at relatively low temperature, making it potentially suitable for development into low-cost commercial process. Important advantages include exothermic character and comparatively low process temperatures. These could lead to significant savings in equipment and energy costs.

Heat capacity of high-purity lanthanum

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

Pan, P.H.; Finnemore, D.K.; Bevolo, A.J.

1980-04-01

A study of the specific heat of high-purity single-phase dhcp La shows that this material is an intrinsic type-II superconductor with a kappa of about 2.4. The temperature dependence of the free energy is characteristic of an intermediate coupling superconductor with 2..delta../k/sub B/T/sub c/ approx. = 3.7.

METHOD OF MAKING REFRACTORY BODIES

DOEpatents

Andersen, J.C.

1960-05-31

A method is given for the manufacture of silicon carbide bodies that are characterized by high density, high purity, and superior resistance to oxidative deterioration. Dense silicon bodies are obtained by a process in which granular silicon carbide, a carbonizable material, and a carbonaceous material are mixed together, the mixture is shaped as desired, and then the shape is fired in the presence of more than the stoichiometric amount of silicon. The carbonizable material preferably includes a temporary binder that is set before the firing step to hold the mix in shape for firing.

Improved recovery of functionally active eosinophils and neutrophils using novel immunomagnetic technology.

PubMed

Son, Kiho; Mukherjee, Manali; McIntyre, Brendan A S; Eguez, Jose C; Radford, Katherine; LaVigne, Nicola; Ethier, Caroline; Davoine, Francis; Janssen, Luke; Lacy, Paige; Nair, Parameswaran

2017-10-01

Clinically relevant and reliable reports derived from in vitro research are dependent on the choice of cell isolation protocols adopted between different laboratories. Peripheral blood eosinophils are conventionally isolated using density-gradient centrifugation followed by immunomagnetic selection (positive/negative) while neutrophils follow a more simplified dextran-sedimentation methodology. With the increasing sophistication of molecular techniques, methods are now available that promise protocols with reduced user-manipulations, improved efficiency, and better yield without compromising the purity of enriched cell populations. These recent techniques utilize immunomagnetic particles with multiple specificities against differential cell surface markers to negatively select non-target cells from whole blood, greatly reducing the cost/time taken to isolate granulocytes. Herein, we compare the yield efficiencies, purity and baseline activation states of eosinophils/neutrophils isolated using one of these newer protocols that use immunomagnetic beads (MACSxpress isolation) vs. the standard isolation procedures. The study shows that the MACSxpress method consistently allowed higher yields per mL of peripheral blood compared to conventional methods (P<0.001, n=8, Wilcoxon paired test), with high isolation purities for both eosinophils (95.0±1.7%) and neutrophils (94.2±10.1%) assessed by two methods: Wright's staining and flow cytometry. In addition, enumeration of CD63 + (marker for eosinophil activation) and CD66b + (marker for neutrophil activation) cells within freshly isolated granulocytes, respectively, confirmed that conventional protocols using density-gradient centrifugation caused cellular activation of the granulocytes at baseline compared to the MACSxpress method. In conclusion, MACSxpress isolation kits were found to be superior to conventional techniques for consistent purifications of eosinophils and neutrophils that were suitable for activation assays involving degranulation markers. Copyright © 2017 Elsevier B.V. All rights reserved.

Low threshold field emission from high-quality cubic boron nitride films

NASA Astrophysics Data System (ADS)

Teii, Kungen; Matsumoto, Seiichiro

2012-05-01

Field emission performance of materials with mixed sp2/sp3 phases often depends upon the phase composition at the surface. In this study, the emission performance of high-quality cubic boron nitride (cBN) films is studied in terms of phase purity. Thick cBN films consisting of micron-sized grains are prepared from boron trifluoride gas by chemical vapor deposition in a plasma jet and an inductively coupled plasma. Both the bulk and surface phase purities as well as crystallinities of cBN evaluated by visible and ultraviolet Raman spectroscopy, glancing-angle x-ray diffraction, and x-ray photoelectron spectroscopy are the highest when the film is deposited in a plasma jet under an optimized condition. The emission turn-on field decreases with increasing the phase purity, down to around 5 V/μm for the highest cBN purity, due to the larger field enhancement, while it is higher than 14 V/μm without cBN (sp2-bonded hexagonal BN only). The results indicate that the total field enhancement for the high phase purity film is governed by the internal field amplification related to the surface coverage of more conductive cBN, rather than the external one related to the surface topology or roughness.

Nano-particulate Aluminium Nitride/Al: An Efficient and Versatile Heterogeneous Catalyst for the Synthesis of Biginelli Scaffolds

NASA Astrophysics Data System (ADS)

Tekale, S. U.; Tekale, A. B.; Kanhe, N. S.; Bhoraskar, S. V.; Pawar, R. P.

2011-12-01

Nano-particulate aluminium nitride/Al (7:1) is reported as a new heterogeneous solid acid catalyst for the synthesis of 3, 4-dihydroxypyrimidi-2-(1H)-ones and their sulphur analogues using the Biginelli reaction. This method involves short reaction time, easy separation, high yields and purity of products.

Powder X-ray diffraction method for the quantification of cocrystals in the crystallization mixture.

PubMed

Padrela, Luis; de Azevedo, Edmundo Gomes; Velaga, Sitaram P

2012-08-01

The solid state purity of cocrystals critically affects their performance. Thus, it is important to accurately quantify the purity of cocrystals in the final crystallization product. The aim of this study was to develop a powder X-ray diffraction (PXRD) quantification method for investigating the purity of cocrystals. The method developed was employed to study the formation of indomethacin-saccharin (IND-SAC) cocrystals by mechanochemical methods. Pure IND-SAC cocrystals were geometrically mixed with 1:1 w/w mixture of indomethacin/saccharin in various proportions. An accurately measured amount (550 mg) of the mixture was used for the PXRD measurements. The most intense, non-overlapping, characteristic diffraction peak of IND-SAC was used to construct the calibration curve in the range 0-100% (w/w). This calibration model was validated and used to monitor the formation of IND-SAC cocrystals by liquid-assisted grinding (LAG). The IND-SAC cocrystal calibration curve showed excellent linearity (R(2) = 0.9996) over the entire concentration range, displaying limit of detection (LOD) and limit of quantification (LOQ) values of 1.23% (w/w) and 3.74% (w/w), respectively. Validation results showed excellent correlations between actual and predicted concentrations of IND-SAC cocrystals (R(2) = 0.9981). The accuracy and reliability of the PXRD quantification method depend on the methods of sample preparation and handling. The crystallinity of the IND-SAC cocrystals was higher when larger amounts of methanol were used in the LAG method. The PXRD quantification method is suitable and reliable for verifying the purity of cocrystals in the final crystallization product.

Understanding Single-Stranded Telomere End Binding by an Essential Protein

DTIC Science & Technology

2000-08-01

BioPharma Inc., 1885 33rd Street, Boulder, CO 80301 Traditional sequential medicinal chemistry methods have been augmented by combinatorial synthesis...on the same wells that were being analyzed in parallel by RP-HPLC/UV for purity. The sampling protocol for purity determination at Array BioPharma is

Evaluation of measurement uncertainty for purity of a monoterpenic acid by small-scale coulometry

NASA Astrophysics Data System (ADS)

Norte, L. C.; de Carvalho, E. M.; Tappin, M. R. R.; Borges, P. P.

2018-03-01

Purity of the perylic acid (HPe) which is a monoterpenic acid from natural product (NP) with anti-inflammatory and anticancer properties was analyzed by small-scale coulometry (SSC), due to the low availability of HPe on the pharmaceutic market and its high cost. This work aims to present the evaluation of the measurements uncertainty from the purity of HPe by using SSC. Coulometric mean of purity obtained from 5 replicates resulted in 94.23% ± 0.88% (k = 2.06, for an approximately 95% confidence level). These studies aim in the future to develop the production of certified reference materials from NPs.

GTA welding and heat treating of high purity aluminum. [-452/sup 0/F

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

Voigt, R.C.; Loper, C.R. Jr.

1979-01-01

Gas tungsten arc welding is a suitable way to join high purity aluminum with only small increases in the electrical resistivity at 4.2 K (i.e., -269 C or -452 F) if proper welding procedures are used. High purity aluminum weld zone properties, useful for the design of cryogenic superconducting devices, are now available. The additional electrical resistivity caused by welding is independent of original base metal resistivity and can be decreased significantly by heat treatments as low as 260 C (500 F) for 30 minutes. Tungsten contamination caused from welding is small (on the order of 0.2 ppM) but itmore » is a significant contribution to weld zone resistivity. This suggests that other welding techniques such as laser welding or electron beam welding may be successful alternatives. Additional GTA welding tests for various welding conditions and welding procedures would lead to a greater understanding of the tungsten emission levels during welding. Perturbations during GTA welding such as electrode spitting or electrode contact with the weld metal must be eliminated to successfully weld high purity aluminum. Improper welding techniques causing arc instabilities, for any reason, cause highly resistive welds that must be properly repaired.« less

In vitro evaluation of the mutagenic and carcinogenic power of high purity zirconia ceramic.

PubMed

Covacci, V; Bruzzese, N; Maccauro, G; Andreassi, C; Ricci, G A; Piconi, C; Marmo, E; Burger, W; Cittadini, A

1999-02-01

Tetragonal zirconia polycrystal (TZP) is a new interesting ceramic for the manufacture of medical devices. Its wide use in orthopedic and odontoiatric implants was limited till now by the high chemical and radiochemical impurities of the raw materials. Purification processes now available allow to obtain high purity ceramic grade powders suitable for TZP ceramics manufacture, even if their possible mutagenic and transforming effects are still unclear. The aim of this work is to study in vitro the mutagenic and oncogenic effects of a new zirconia ceramic stabilized by yttria (Y-TZP). This ceramic was sintered from high purity powders obtained by a process developed under a project carried out within the Brite EuRam programme. For comparison, ceramics made from unpurified zirconia powder were also tested. Fibroblasts irradiated by a linear accelerator were used as positive control. The results obtained show that Y-TZP ceramic does not elicit either mutagenic or transforming effect on C3H/10T(1/2) (10T(1/2)) cells and demonstrate that ceramic from high purity powders can be considered suitable for biomedical applications from the point of view of the effects of its radioactive impurity content.

Super high-rate fabrication of high-purity carbon nanotube aerogels from floating catalyst method for oil spill cleaning

NASA Astrophysics Data System (ADS)

Khoshnevis, Hamed; Mint, Sandar Myo; Yedinak, Emily; Tran, Thang Q.; Zadhoush, Ali; Youssefi, Mostafa; Pasquali, Matteo; Duong, Hai M.

2018-02-01

In this study, we apply an advanced floating catalyst method to fabricate carbon nanotube (CNT) aerogels at super high deposition rate for oil spill cleaning. The aerogels consist of 3D porous network of stacking double-walled CNT bundles with low catalyst impurity (9%) and high thermal stability (650 °C). With high porosity, surface areas, and water contact angles, the CNT aerogels exhibit a high oil adsorption of up to 107 g/g and good reusability of up to four adsorption-burning cycles. This work suggests that the lightweight, porous, and super hydrophobic CNT aerogels can be promising sorbent materials for environmental applications.

Human plasma-derived immunoglobulin G fractionated by an aqueous two-phase system, caprylic acid precipitation, and membrane chromatography has a high purity level and is free of detectable in vitro thrombogenic activity.

PubMed

Vargas, M; Segura, Á; Wu, Y-W; Herrera, M; Chou, M-L; Villalta, M; León, G; Burnouf, T

2015-02-01

Instituto Clodomiro Picado has developed an immunoglobulin G (IgG) plasma fractionation process combining a polyethylene glycol/phosphate aqueous two-phase system (ATPS), caprylic acid precipitation and anion-exchange membrane chromatography. We evaluated the purity and in vitro thrombogenicity of such IgG, in line with current international requirements. Contributions of the different production steps to reduce thrombogenicity were assessed at 0·2 l-scale, and then the methodology was scaled-up to a 10 l-scale and final products (n = 3) were analysed. Purity, immunoglobulin composition, and subclass distribution were determined by electrophoretic and immunochemical methods. The in vitro thrombogenic potential was determined by a thrombin generation assay (TGA) using a Technothrombin fluorogenic substrate. Prekallikrein activator (PKA), plasmin, factor Xa, thrombin and thrombin-like activities were assessed using S-2302, S-2251, S-2222, S-2238 and S-2288 chromogenic substrates, respectively, and FXI by an ELISA. The thrombogenicity markers were reduced mostly during the ATPS step and were found to segregate mostly into the discarded liquid upper phase. The caprylic acid precipitation eliminated the residual procoagulant activity. The IgG preparations made from the 10 l-batches contained 100% gamma proteins, low residual IgA and undetectable IgM. The IgG subclass distribution was not substantially affected by the process. TGA and amidolytic activities revealed an undetectable in vitro thrombogenic risk and the absence of proteolytic enzymes in the final product. Fractionating human plasma by an ATPS combined with caprylic acid and membrane chromatography resulted in an IgG preparation of high purity and free of a detectable in vitro thrombogenic risk. © 2014 International Society of Blood Transfusion.

Analysis of high-purity germanium dioxide by ETV-ICP-AES with preliminary concentration of trace elements.

PubMed

Medvedev, Nickolay S; Shaverina, Anastasiya V; Tsygankova, Alphiya R; Saprykin, Anatoly I

2016-08-01

The paper presents a combined technique of germanium dioxide analysis by inductively coupled plasma atomic emission spectrometry (ICP-AES) with preconcentration of trace elements by distilling off matrix and electrothermal (ETV) introduction of the trace elements concentrate into the ICP. Evaluation of metrological characteristics of the developed technique of high-purity germanium dioxide analysis was performed. The limits of detection (LODs) for 25 trace elements ranged from 0.05 to 20ng/g. The accuracy of proposed technique is confirmed by "added-found" («or spiking») experiment and comparing the results of ETV-ICP-AES and ICP-AES analysis of high purity germanium dioxide samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Sub-atmospheric pressure gas sources for bulk storage and delivery of arsine and phosphine to MOCVD tools

NASA Astrophysics Data System (ADS)

Raynor, M. W.; Houlding, V. H.; Funke, H. H.; Frye, R.; Dietz, J. A.

2003-02-01

A sub-atmospheric (SA) pressure gas source, based on the reversible adsorption of hydride gas onto a high surface area substrate within a cylinder, has been developed for the safe storage and delivery of high-purity arsine and phosphine for MOCVD processes. SA pressure and high-pressure sources are compared with respect to gas delivery and purity, risk reduction, and cost benefits. Gas analysis and performance of epi-structures grown with SA pressure cylinders confirm that the hydride gas delivered meets the purity requirements of MOCVD processes. Further, the low gas release rates measured from 2.2 and 49 l SA pressure cylinders indicate that the technology can be scaled up without additional safety risk.

On-Demand Single Photons with High Extraction Efficiency and Near-Unity Indistinguishability from a Resonantly Driven Quantum Dot in a Micropillar.

PubMed

Ding, Xing; He, Yu; Duan, Z-C; Gregersen, Niels; Chen, M-C; Unsleber, S; Maier, S; Schneider, Christian; Kamp, Martin; Höfling, Sven; Lu, Chao-Yang; Pan, Jian-Wei

2016-01-15

Scalable photonic quantum technologies require on-demand single-photon sources with simultaneously high levels of purity, indistinguishability, and efficiency. These key features, however, have only been demonstrated separately in previous experiments. Here, by s-shell pulsed resonant excitation of a Purcell-enhanced quantum dot-micropillar system, we deterministically generate resonance fluorescence single photons which, at π pulse excitation, have an extraction efficiency of 66%, single-photon purity of 99.1%, and photon indistinguishability of 98.5%. Such a single-photon source for the first time combines the features of high efficiency and near-perfect levels of purity and indistinguishabilty, and thus opens the way to multiphoton experiments with semiconductor quantum dots.

Method and apparatus for measuring lung density by Compton backscattering

DOEpatents

Loo, Billy W.; Goulding, Frederick S.

1991-01-01

The density of the lung of a patient suffering from pulmonary edema is monitored by irradiating the lung by a single collimated beam of monochromatic photons and measuring the energies of photons Compton backscattered from the lung by a single high-resolution, high-purity germanium detector. A compact system geometry and a unique data extraction scheme are utilized to monimize systematic errors due to the presence of the chestwall and multiple scattering.

Carbon nanotube materials for hydrogen storage

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

Dillon, A.C.; Parilla, P.A.; Jones, K.M.

1998-08-01

Carbon single-wall nanotubes (SWNTs) are essentially elongated pores of molecular dimensions and are capable of adsorbing hydrogen at relatively high temperatures and low pressures. This behavior is unique to these materials and indicates that SWNTs are the ideal building block for constructing safe, efficient, and high energy density adsorbents for hydrogen storage applications. In past work the authors developed methods for preparing and opening SWNTs, discovered the unique adsorption properties of these new materials, confirmed that hydrogen is stabilized by physical rather than chemical interactions, measured the strength of interaction to be {approximately} 5 times higher than for adsorption onmore » planar graphite, and performed infrared absorption spectroscopy to determine the chemical nature of the surface terminations before, during, and after oxidation. This year the authors have made significant advances in synthesis and characterization of SWNT materials so that they can now prepare gram quantities of high-purity SWNT samples and measure and control the diameter distribution of the tubes by varying key parameters during synthesis. They have also developed methods which purify nanotubes and cut nanotubes into shorter segments. These capabilities provide a means for opening the tubes which were unreactive to the oxidation methods that successfully opened tubes, and offer a path towards organizing nanotube segments to enable high volumetric hydrogen storage densities. They also performed temperature programmed desorption spectroscopy on high purity carbon nanotube material obtained from collaborator Prof. Patrick Bernier and finished construction of a high precision Seivert`s apparatus which will allow the hydrogen pressure-temperature-composition phase diagrams to be evaluated for SWNT materials.« less

A novel multi-wall CNT synthesis technique using conventional CVD with controlled pressure

NASA Astrophysics Data System (ADS)

Kara, M. H. S.; Amir, M. H.; Teh, A. A.; Ahmad, R.; Mahmood, M. R.; Awang, Z.

2012-09-01

In this paper we have demonstrated successfully for the first time, a simple but efficient and reliable approach for the growth of multi walled carbon nanotubes (MWCNTs) with high degree of crystallinity, purity and density under a wide range of growth parameters. Multi-walled carbon nanotubes (MWCNTs) were synthesized at 800 - 950°C by thermal chemical vapor deposition (TCVD) method using a thin nickel film as catalyst and methane gas as carbon source. In this process, two substrates were placed in a long alumina boat inside a double-heater TCVD. One of the substrates was covered with a short upside down alumina boat. The prepared nanotubes were characterized by scanning electron microscopy (SEM) and field emission scanning electron microscopy (FESEM) and it was found that, CNT growth on the covered substrate was improved in terms of quality and density compared to the other uncovered substrate. In addition, the nanotube diameter is reduced more than half. Results also revealed that the temperature gradient played a key factor for growth efficiency and purity of nanotubes. In addition, the diameter of CNT can be influenced by growth temperature too. The catalyst thickness and gas flow rate were found to influence the diameter and density of tubes, whereas the effect of synthesis time was on the CNT length. This growth technique is unique because of its simplicity, high efficiency and its ability to yield CNTs of high purity and density. This finding is supported by Raman spectrometry analysis.

Evolution of Deformation and Recrystallization Textures in High-Purity Ni and the Ni-5 at. pct W Alloy

NASA Astrophysics Data System (ADS)

Bhattacharjee, Pinaki P.; Ray, Ranjit K.; Tsuji, Nobuhiro

2010-11-01

An attempt has been made to study the evolution of texture in high-purity Ni and Ni-5 at. pct W alloy prepared by the powder metallurgy route followed by heavy cold rolling ( 95 pct deformation) and recrystallization. The deformation textures of the two materials are of typical pure metal or Cu-type texture. Cube-oriented ( left\\{ {00 1} right\\}left< { 100} rightrangle ) regions are present in the deformed state as long thin bands, elongated in the rolling direction (RD). These bands are characterized by a high orientation gradient inside, which is a result of the rotation of the cube-oriented cells around the RD toward the RD-rotated cube ( left\\{ {0 1 3} right\\}left< { 100} rightrangle ). Low-temperature annealing produces a weak cube texture along with the left\\{ {0 1 3} right\\}left< { 100} rightrangle component, with the latter being much stronger in high-purity Ni than in the Ni-W alloy. At higher temperatures, the cube texture is strengthened considerably in the Ni-W alloy; however, the cube volume fraction in high-purity Ni is significantly lower because of the retention of the left\\{ {0 1 3} right\\}left< { 100} rightrangle component. The difference in the relative strengths of the cube, and the left\\{ {0 1 3} right\\}left< { 100} rightrangle components in the two materials is evident from the beginning of recrystallization in which more left\\{ {0 1 3} right\\}left< { 100} rightrangle -oriented grains than near cube grains form in high-purity Ni. The preferential nucleation of the near cube and the left\\{ {0 1 3} right\\}left< { 100} rightrangle grains in these materials seems to be a result of the high orientation gradients associated with the cube bands that offer a favorable environment for early nucleation.

Particle separation by phase modulated surface acoustic waves.

PubMed

Simon, Gergely; Andrade, Marco A B; Reboud, Julien; Marques-Hueso, Jose; Desmulliez, Marc P Y; Cooper, Jonathan M; Riehle, Mathis O; Bernassau, Anne L

2017-09-01

High efficiency isolation of cells or particles from a heterogeneous mixture is a critical processing step in lab-on-a-chip devices. Acoustic techniques offer contactless and label-free manipulation, preserve viability of biological cells, and provide versatility as the applied electrical signal can be adapted to various scenarios. Conventional acoustic separation methods use time-of-flight and achieve separation up to distances of quarter wavelength with limited separation power due to slow gradients in the force. The method proposed here allows separation by half of the wavelength and can be extended by repeating the modulation pattern and can ensure maximum force acting on the particles. In this work, we propose an optimised phase modulation scheme for particle separation in a surface acoustic wave microfluidic device. An expression for the acoustic radiation force arising from the interaction between acoustic waves in the fluid was derived. We demonstrated, for the first time, that the expression of the acoustic radiation force differs in surface acoustic wave and bulk devices, due to the presence of a geometric scaling factor. Two phase modulation schemes are investigated theoretically and experimentally. Theoretical findings were experimentally validated for different mixtures of polystyrene particles confirming that the method offers high selectivity. A Monte-Carlo simulation enabled us to assess performance in real situations, including the effects of particle size variation and non-uniform acoustic field on sorting efficiency and purity, validating the ability to separate particles with high purity and high resolution.

Fabrication and characterization of carbon-backed thin 208Pb targets.

PubMed

Thakur, Meenu; Dubey, R; Abhilash, S R; Behera, B R; Mohanty, B P; Kabiraj, D; Ojha, Sunil; Duggal, Heena

2016-01-01

Thin carbon-backed isotopically enriched 208 Pb targets were required for our experiment aimed to study the reaction dynamics for 48 Ti +  208 Pb system, populating the near super-heavy nucleus 256 Rf, through mass-energy correlation of the fission fragments. Purity and thickness of the targets are of utmost importance in such studies as these factors have strong influence on the measurement accuracy of mass and energy distribution of fission fragments. 208 Pb targets with thickness ranging from 60 μg/cm 2 to 250 μg/cm 2 have been fabricated in high vacuum environment using physical vapor deposition method. Important points in the method are as follows: • 208 Pb was deposited using resistive heating method, whereas carbon (backing foil) deposition was performed by using the electron beam bombardment technique.•Different characterization techniques such as Particle Induced X-ray Emission (PIXE), Energy Dispersive X-Ray Fluorescence (EDXRF) and Rutherford Backscattering Spectrometry (RBS) were used to assert the purity and thickness of the targets.•These targets have successfully been used to accomplish our experimental objectives.

Synthesis of Nano Sized Cr2AlC Powders by Molten Salt Method.

PubMed

Xiao, Dan; Zhu, Jianfeng; Wang, Fen; Tang, Yi

2015-09-01

Cr2AlC powders were successfully synthesized by molten salt method using Cr, Al and C as starting materials. The effects of the process parameters and amount of Al addition on the purity of the Cr2AlC powders were also investigated in details. The formation mechanism of Cr2AlC powders was investigated by XRD and DSC. The results indicated that intermediates of Cr7C3 and Cr- Al intermetallics, such as CrAl17, Cr2Al, Cr2Al8, were formed by the reactions among the initial elements, then the intermediates gradually transformed to Cr2AlC. From the fixed composition of Cr:Al:C = 2:1.2:1, high purity Cr2AlC powders could be obtained with an inorganic salt KCl as a solvent at 1250 degrees C for 60 min under argon atmosphere which was lower than that (generally 1450 degrees C) of conventional solid state reaction.

Integrated Method for Purification and Single-Particle Characterization of Lentiviral Vector Systems by Size Exclusion Chromatography and Tunable Resistive Pulse Sensing.

PubMed

Heider, Susanne; Muzard, Julien; Zaruba, Marianne; Metzner, Christoph

2017-07-01

Elements derived from lentiviral particles such as viral vectors or virus-like particles are commonly used for biotechnological and biomedical applications, for example in mammalian protein expression, gene delivery or therapy, and vaccine development. Preparations of high purity are necessary in most cases, especially for clinical applications. For purification, a wide range of methods are available, from density gradient centrifugation to affinity chromatography. In this study we have employed size exclusion columns specifically designed for the easy purification of extracellular vesicles including exosomes. In addition to viral marker protein and total protein analysis, a well-established single-particle characterization technology, termed tunable resistive pulse sensing, was employed to analyze fractions of highest particle load and purity and characterize the preparations by size and surface charge/electrophoretic mobility. With this study, we propose an integrated platform combining size exclusion chromatography and tunable resistive pulse sensing for monitoring production and purification of viral particles.

Compositions and Methods for Inhibiting Gene Expressions

NASA Technical Reports Server (NTRS)

Williams, Loren D. (Inventor); Hsiao, Chiaolong (Inventor); Fang, Po-Yu (Inventor); Williams, Justin (Inventor)

2018-01-01

A combined packing and assembly method that efficiently packs ribonucleic acid (RNA) into virus like particles (VLPs) has been developed. The VLPs can spontaneously assemble and load RNA in vivo, efficiently packaging specifically designed RNAs at high densities and with high purity. In some embodiments the RNA is capable of interference activity, or is a precursor of a RNA capable of causing interference activity. Compositions and methods for the efficient expression, production and purification of VLP-RNAs are provided. VLP-RNAs can be used for the storage of RNA for long periods, and provide the ability to deliver RNA in stable form that is readily taken up by cells.

System and method for liquid silicon containment

DOEpatents

Cliber, James A; Clark, Roger F; Stoddard, Nathan G; Von Dollen, Paul

2013-05-28

This invention relates to a system and a method for liquid silicon containment, such as during the casting of high purity silicon used in solar cells or solar modules. The containment apparatus includes a shielding member adapted to prevent breaching molten silicon from contacting structural elements or cooling elements of a casting device, and a volume adapted to hold a quantity of breaching molten silicon with the volume formed by a bottom and one or more sides.

System and method for liquid silicon containment

DOEpatents

Cliber, James A; Clark, Roger F; Stoddard, Nathan G; Von Dollen, Paul

2014-06-03

This invention relates to a system and a method for liquid silicon containment, such as during the casting of high purity silicon used in solar cells or solar modules. The containment apparatus includes a shielding ember adapted to prevent breaching molten silicon from contacting structural elements or cooling elements of a casting device, and a volume adapted to hold a quantity of breaching molten silicon with the volume formed by a bottom and one or more sides.

Multiphase separation of copper nanowires

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

Qian, Fang; Lan, Pui Ching; Olson, Tammy

Here, this communication reports a new method to purify copper nanowires with nearly 100% yield from undesired copper nanoparticle side-products formed during batch processes of copper nanowire synthesis. Also, this simple separation method can yield large quantities of long, uniform, high-purity copper nanowires to meet the requirements of nanoelectronics applications as well as provide an avenue for purifying copper nanowires in the industrial scale synthesis of copper nanowires, a key step for commercialization and application of nanowires.

Multiphase separation of copper nanowires

DOE PAGES

Qian, Fang; Lan, Pui Ching; Olson, Tammy; ...

2016-09-01

Here, this communication reports a new method to purify copper nanowires with nearly 100% yield from undesired copper nanoparticle side-products formed during batch processes of copper nanowire synthesis. Also, this simple separation method can yield large quantities of long, uniform, high-purity copper nanowires to meet the requirements of nanoelectronics applications as well as provide an avenue for purifying copper nanowires in the industrial scale synthesis of copper nanowires, a key step for commercialization and application of nanowires.

Efficient isolation method for high-quality genomic DNA from cicada exuviae.

PubMed

Nguyen, Hoa Quynh; Kim, Ye Inn; Borzée, Amaël; Jang, Yikweon

2017-10-01

In recent years, animal ethics issues have led researchers to explore nondestructive methods to access materials for genetic studies. Cicada exuviae are among those materials because they are cast skins that individuals left after molt and are easily collected. In this study, we aim to identify the most efficient extraction method to obtain high quantity and quality of DNA from cicada exuviae. We compared relative DNA yield and purity of six extraction protocols, including both manual protocols and available commercial kits, extracting from four different exoskeleton parts. Furthermore, amplification and sequencing of genomic DNA were evaluated in terms of availability of sequencing sequence at the expected genomic size. Both the choice of protocol and exuvia part significantly affected DNA yield and purity. Only samples that were extracted using the PowerSoil DNA Isolation kit generated gel bands of expected size as well as successful sequencing results. The failed attempts to extract DNA using other protocols could be partially explained by a low DNA yield from cicada exuviae and partly by contamination with humic acids that exist in the soil where cicada nymphs reside before emergence, as shown by spectroscopic measurements. Genomic DNA extracted from cicada exuviae could provide valuable information for species identification, allowing the investigation of genetic diversity across consecutive broods, or spatiotemporal variation among various populations. Consequently, we hope to provide a simple method to acquire pure genomic DNA applicable for multiple research purposes.

High Purity Americium-241 for Fuel Cycle R&D Program

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

Dr. Paul A. Lessing

2011-07-01

Previously the U.S. Department of Energy released Am-241 for various applications such as smoke detectors and Am-Be neutron sources for oil wells. At this date there is a shortage of usable, higher purity Am-241 in metal and oxide form available in the United States. Recently, the limited source of Am-241 has been from Russia with production being contracted to existing customers. The shortage has resulted in the price per gram rising dramatically over the last few years. DOE-NE currently has need for high purity Am-241 metal and oxide to fabricate fuel pellets for reactor testing in the Fuel Cycle R&Dmore » program. All the available high purity americium has been gathered from within the DOE system of laboratories. However, this is only a fraction of the projected needs of FCRD over the next 10 years. Therefore, FCR&D has proposed extraction and purification concepts to extract Am-241 from a mixed AmO2-PuO2 feedstock stored at the Savannah River Site. The most simple extraction system is based upon high temperature reduction using lanthanum metal with concurrent evaporation and condensation to produce high purity Am metal. Metallic americium has over a four order of magnitude higher vapor pressure than plutonium. Results from small-scale reduction experiments are presented. These results confirm thermodynamic predictions that at 1000 deg C metallic lanthanum reduces both PuO2 and AmO2. Faster kinetics are expected for temperatures up to about 1500 deg C.« less

Purity assessment of commercial zein products after purification

USDA-ARS?s Scientific Manuscript database

Successful utilization of commercial zein products for certain food, pharmaceutical, cosmetic and medical applications requires a decolorized/deodorized zein of high purity. A zein protein product with those qualifications can be achieved by column filtration of commercial yellow zein solutions thro...

EUV tools: hydrogen gas purification and recovery strategies

NASA Astrophysics Data System (ADS)

Landoni, Cristian; Succi, Marco; Applegarth, Chuck; Riddle Vogt, Sarah

2015-03-01

The technological challenges that have been overcome to make extreme ultraviolet lithography (EUV) a reality have been enormous1. This vacuum driven technology poses significant purity challenges for the gases employed for purging and cleaning the scanner EUV chamber and source. Hydrogen, nitrogen, argon and ultra-high purity compressed dry air (UHPCDA) are the most common gases utilized at the scanner and source level. Purity requirements are tighter than for previous technology node tools. In addition, specifically for hydrogen, EUV tool users are facing not only gas purity challenges but also the need for safe disposal of the hydrogen at the tool outlet. Recovery, reuse or recycling strategies could mitigate the disposal process and reduce the overall tool cost of operation. This paper will review the types of purification technologies that are currently available to generate high purity hydrogen suitable for EUV applications. Advantages and disadvantages of each purification technology will be presented. Guidelines on how to select the most appropriate technology for each application and experimental conditions will be presented. A discussion of the most common approaches utilized at the facility level to operate EUV tools along with possible hydrogen recovery strategies will also be reported.

Low temperature recombination and trapping analysis in high purity gallium arsenide by microwave photodielectric techniques

NASA Technical Reports Server (NTRS)

Khambaty, M. B.; Hartwig, W. H.

1972-01-01

Some physical theories pertinent to the measurement properties of gallium arsenide are presented and experimental data are analyzed. A model for explaining recombination and trapping high purity gallium arsenide, valid below 77 K is assembled from points made at various places and an appraisal is given of photodielectric techniques for material property studies.

Tannase-mediated biotransformation assisted separation and purification of theaflavin and epigallocatechin by high speed counter current chromatography and preparative high performance liquid chromatography: A comparative study.

PubMed

Xia, Guobin; Lin, Chunfang; Liu, Songbai

2016-09-01

A large scale isolation and purification of theaflavin (TF) and epigallocatechin (EGC) has been successfully developed by tannase-mediated biotransformation combining high-speed countercurrent chromatography. After tannase hydrolysis of a commercially available theaflavins extract (TE), the content of TF and EGC in tannase-mediated biotransformation product (TBP) achieved approximately 3 times enrichment. SEM studies revealed smooth tannase biotransformation and the possibility of recovery of the tannase. A single 1.5 hours' HSCCC separation for TF and EGC employing a two-phase solvent system could simultaneously produce 180.8 mg of 97.3% purity TF and 87.5 mg of 97.3% purity EGC. However, a preparative HPLC separation of maximum injection volume containing 120 mg TBP prepared 11.2 mg TF of 94.9% purity and 7.7 mg EGC of 89.9% purity. HSCCC separation demonstrated significant advantages over Prep HPLC in terms of sample loading size, separation time, environmental friendly solvent systems, and the production. © 2016 Wiley Periodicals, Inc.

Multi-Physics Modeling of Molten Salt Transport in Solid Oxide Membrane (SOM) Electrolysis and Recycling of Magnesium

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

Powell, Adam; Pati, Soobhankar

2012-03-11

Solid Oxide Membrane (SOM) Electrolysis is a new energy-efficient zero-emissions process for producing high-purity magnesium and high-purity oxygen directly from industrial-grade MgO. SOM Recycling combines SOM electrolysis with electrorefining, continuously and efficiently producing high-purity magnesium from low-purity partially oxidized scrap. In both processes, electrolysis and/or electrorefining take place in the crucible, where raw material is continuously fed into the molten salt electrolyte, producing magnesium vapor at the cathode and oxygen at the inert anode inside the SOM. This paper describes a three-dimensional multi-physics finite-element model of ionic current, fluid flow driven by argon bubbling and thermal buoyancy, and heat andmore » mass transport in the crucible. The model predicts the effects of stirring on the anode boundary layer and its time scale of formation, and the effect of natural convection at the outer wall. MOxST has developed this model as a tool for scale-up design of these closely-related processes.« less

High-frequency drug purity and price series as tools for explaining drug trends and harms in Victoria, Australia.

PubMed

Scott, Nick; Caulkins, Jonathan P; Ritter, Alison; Quinn, Catherine; Dietze, Paul

2015-01-01

Methamphetamine-related harms in Victoria have increased recently in the context of stable or declining use prevalence. We determine how changes in price and purity of methamphetamine compared to other drugs such as heroin may, in part, explain these divergent patterns. Detailed methamphetamine and heroin purchase price data from 2152 participant interviews from the Melbourne Injecting Drug User cohort study were used to generate drug price series for the period January 2009-June 2013. Data on drug purity from 8818 seizures made within Victoria were used to generate drug purity series during the same period. Purity-adjusted price data for methamphetamine and heroin were obtained for the period 2009-13 by combining the two data sets. While the average purity of heroin seizures remained consistent and low, the average purity of powder and of crystal methamphetamine seizures increased from 12% [95% confidence interval (CI) = 10-14%] to 37% (95% CI = 20-54%) and 21% (95% CI = 18-23%) to 64% (95% CI = 60-68%), respectively. Crystal methamphetamine purity was bimodal, with observations generally less than 20% or greater than 70%. The average unadjusted price per gram for heroin decreased from $374 (95% CI = $367-381) to $294 (95% CI = $280-308), powder methamphetamine did not change significantly from $252 (95% CI = $233-271), and crystal methamphetamine increased substantially from $464 (95% CI = $416-511) in 2009 to $795 (95% CI = $737-853) in 2011. This increase was offset by an even greater increase in purity, meaning the average purity-adjusted price per gram declined. Furthermore, pure prices of both methamphetamine forms were similar, whereas their unadjusted prices were not. The pure price of heroin fluctuated with no ongoing trends. Decreases in methamphetamine purity-adjusted price along with the bimodality of crystal methamphetamine purity may account for some of the recent increase in methamphetamine-related harm. For a given amount spent, methamphetamine purchase power has increased and the presence of extreme purity variations may challenge individuals' control of consumption. © 2014 Society for the Study of Addiction.

APPARATUS FOR THE PRODUCTION OF LITHIUM METAL

DOEpatents

Baker, P.S.; Duncan, F.R.; Greene, H.B.

1961-08-22

Methods and apparatus for the production of high-purity lithium from lithium halides are described. The apparatus is provided for continuously contacting a molten lithium halide with molten barium, thereby forming lithium metal and a barium halide, establishing separate layers of these reaction products and unreacted barium and lithium halide, and continuously withdrawing lithium and barium halide from the reaction zone. (AEC)

Comparison of analytical performances of inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry for trace analysis of bismuth and bismuth oxide

NASA Astrophysics Data System (ADS)

Medvedev, Nickolay S.; Shaverina, Anastasiya V.; Tsygankova, Alphiya R.; Saprykin, Anatoly I.

2018-04-01

The paper presents а comparison of analytical performances of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) for trace analysis of high purity bismuth and bismuth oxide. Matrix effects in the ICP-MS and ICP-AES methods were studied as a function of Bi concentration, ICP power and nebulizer flow rate. For ICP-MS the strong dependence of the matrix effects versus the atomic mass of analytes was observed. For ICP-AES the minimal matrix effects were achieved for spectral lines of analytes with low excitation potentials. The optimum degree of sample dilution providing minimum values of the limits of detection (LODs) was chosen. Both methods let us to reach LODs from n·10-7 to n·10-4 wt% for more than 50 trace elements. For most elements the LODs of ICP-MS were lower in comparison to ICP-AES. Validation of accuracy of the developed techniques was performed by "added-found" experiments and by comparison of the results of ICP-MS and ICP-AES analysis of high-purity bismuth oxide.

Production of High-Purity Anhydrous Nickel(II) Perrhenate for Tungsten-Based Sintered Heavy Alloys

PubMed Central

Leszczyńska-Sejda, Katarzyna; Benke, Grzegorz; Kopyto, Dorota; Majewski, Tomasz; Drzazga, Michał

2017-01-01

This paper presents a method for the production of high-purity anhydrous nickel(II) perrhenate. The method comprises sorption of nickel(II) ions from aqueous nickel(II) nitrate solutions, using strongly acidic C160 cation exchange resin, and subsequent elution of sorbed nickel(II) ions using concentrated perrhenic acid solutions. After the neutralization of the resulting rhenium-nickel solutions, hydrated nickel(II) perrhenate is then separated and then dried at 160 °C to obtain the anhydrous form. The resulting compound is reduced in an atmosphere of dissociated ammonia in order to produce a Re-Ni alloy powder. This study provides information on the selected properties of the resulting Re-Ni powder. This powder was used as a starting material for the production of 77W-20Re-3Ni heavy alloys. Microstructure examination results and selected properties of the produced sintered heavy alloys were compared to sintered alloys produced using elemental W, Re, and Ni powders. This study showed that the application of anhydrous nickel(II) perrhenate in the production of 77W-20Re-3Ni results in better properties of the sintered alloys compared to those made from elemental powders. PMID:28772808

An effective method for preparation of high-purity pelargonidin-3-O-glucoside from strawberry and its protective effect on cellular oxidative stress.

PubMed

Xu, Yang; Hu, Dongwen; Li, Yuting; Sun, Chongde; Chen, Wei

2018-01-01

Accumulating evidence indicates that consumption of berries may exert beneficial effects against oxidative stress mediated diseases. Pelargonidin-3-O-glucoside (Pg3G), a bioactive ingredient in strawberry, has been reported to possess a potent antioxidant capacity. This study was therefore designed to develop an effective method to prepare pure Pg3G from strawberry and investigate its protective effect against H 2 O 2 -induced oxidative stress. According to our results, Pg3G occupied 85.55% of total anthocyanin content in strawberry. 240mg of Pg3G with the purity of 97.26% was finally isolated from 320g of strawberry lyophilized powder (SLP) by combination of AB-8 macroporous resin and high-speed counter-current chromatography (HSCCC) technologies. Further study unveiled that Pg3G significantly inhibited H 2 O 2 -induced ROS generation, GSH depletion and mitochondrial dysfunction, thereby ameliorating H 2 O 2 -induced oxidative stress. Overall, this study suggests that pelargonidin-3-O-glucoside can be used as a natural bioactive agent to prevent cellular oxidative stress. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of Cr doping on the structural, morphological, optical and electrical properties of indium tin oxide films

NASA Astrophysics Data System (ADS)

Mirzaee, Majid; Dolati, Abolghasem

2015-03-01

We report on the preparation and characterization of high-purity chromium (0.5-2.5 at.%)-doped indium tin oxide (ITO, In:Sn = 90:10) films deposited by sol-gel-mediated dip coating. The effects of different Cr-doping contents on structural, morphological, optical and electrical properties of the films were characterized by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV-Vis spectroscopy and four-point probe methods. XRD showed high phase purity cubic In2O3 and indicated a contraction of the lattice with Cr doping. FESEM micrographs show that grain size decreased with increasing the Cr-doping content. A method to determine chromium species in the sample was developed through the decomposition of the Cr 2 p XPS spectrum in Cr6+ and Cr3+ standard spectra. Optical and electrical studies revealed that optimum opto-electronic properties, including minimum sheet resistance of 4,300 Ω/Sq and an average optical transmittance of 85 % in the visible region with a band gap of 3.421 eV, were achieved for the films doped with Cr-doping content of 2 at.%.

Low energy consumption method for separating gaseous mixtures and in particular for medium purity oxygen production

DOEpatents

Jujasz, Albert J.; Burkhart, James A.; Greenberg, Ralph

1988-01-01

A method for the separation of gaseous mixtures such as air and for producing medium purity oxygen, comprising compressing the gaseous mixture in a first compressor to about 3.9-4.1 atmospheres pressure, passing said compressed gaseous mixture in heat exchange relationship with sub-ambient temperature gaseous nitrogen, dividing the cooled, pressurized gaseous mixture into first and second streams, introducing the first stream into the high pressure chamber of a double rectification column, separating the gaseous mixture in the rectification column into a liquid oxygen-enriched stream and a gaseous nitrogen stream and supplying the gaseous nitrogen stream for cooling the compressed gaseous mixture, removing the liquid oxygen-enriched stream from the low pressure chamber of the rectification column and pumping the liquid, oxygen-enriched steam to a predetermined pressure, cooling the second stream, condensing the cooled second stream and evaporating the oxygen-enriched stream in an evaporator-condenser, delivering the condensed second stream to the high pressure chamber of the rectification column, and heating the oxygen-enriched stream and blending the oxygen-enriched stream with a compressed blend-air stream to the desired oxygen concentration.

Power partial-discard strategy to obtain improved performance for simulated moving bed chromatography.

PubMed

Chung, Ji-Woo; Kim, Kyung-Min; Yoon, Tae-Ung; Kim, Seung-Ik; Jung, Tae-Sung; Han, Sang-Sup; Bae, Youn-Sang

2017-12-22

A novel power partial-discard (PPD) strategy was developed as a variant of the partial-discard (PD) operation to further improve the separation performance of the simulated moving bed (SMB) process. The PPD operation varied the flow rates of discard streams by introducing a new variable, the discard amount (DA) as well as varying the reported variable, discard length (DL), while the conventional PD used fixed discard flow rates. The PPD operations showed significantly improved purities in spite of losses in recoveries. Remarkably, the PPD operation could provide more enhanced purity for a given recovery or more enhanced recovery for a given purity than the PD operation. The two variables, DA and DL, in the PPD operation played a key role in achieving the desired purity and recovery. The PPD operations will be useful for attaining high-purity products with reasonable recoveries. Copyright © 2017 Elsevier B.V. All rights reserved.

Standardized methods for the production of high specific-activity zirconium-89

PubMed Central

Holland, Jason P.; Sheh, Yiauchung; Lewis, Jason S.

2009-01-01

Zirconium-89 is an attractive metallo-radionuclide for use in immunoPET due to the favorable decay characteristics. Standardized methods for the routine production and isolation of high purity and high specific-activity 89Zr using a small cyclotron are reported. Optimized cyclotron conditions reveal high average yields of 1.52 ± 0.11 mCi/μA·h at a proton beam energy of 15 MeV and current of 15 μA using a solid, commercially available 89Y-foil target (0.1 mm, 100% natural abundance). 89Zr was isolated in high radionuclidic and radiochemical purity (>99.99%) as [89Zr]Zr-oxalate by using a solid-phase hydroxamate resin with >99.5% recovery of the radioactivity. The effective specific-activity of 89Zr was found to be in the range 5.28 – 13.43 mCi/μg (470 – 1195 Ci/mmol) of zirconium. New methods for the facile production of [89Zr]Zr-chloride are reported. Radiolabeling studies using the trihydroxamate ligand desferrioxamine B (DFO) gave 100% radiochemical yields in <15 min. at room temperature and in vitro stability measurements confirmed that [89Zr]Zr-DFO is stable with respect to ligand dissociation in human serum for >7 days. Small-animal PET imaging studies have demonstrated that free 89Zr(IV) ions administered as [89Zr]Zr-chloride accumulate in the liver whilst [89Zr]Zr-DFO is excreted rapidly via the kidneys within <20 min. These results have important implication for the analysis of immunoPET imaging of 89Zr-labeled monoclonal antibodies. The detailed methods described can be easily translated to other radiochemistry facilities and will facilitate the use of 89Zr in both basic science and clinical investigations. PMID:19720285

High-speed counter-current chromatography coupled online to high performance liquid chromatography-diode array detector-mass spectrometry for purification, analysis and identification of target compounds from natural products.

PubMed

Liang, Xuejuan; Zhang, Yuping; Chen, Wei; Cai, Ping; Zhang, Shuihan; Chen, Xiaoqin; Shi, Shuyun

2015-03-13

A challenge in coupling high-speed counter-current chromatography (HSCCC) online with high performance liquid chromatography (HPLC) for purity analysis was their time incompatibility. Consequently, HSCCC-HPLC was conducted by either controlling HPLC analysis time and HSCCC flow rate or using stop-and-go scheme. For natural products containing compounds with a wide range of polarities, the former would optimize experimental conditions, while the latter required more time. Here, a novel HSCCC-HPLC-diode array detector-mass spectrometry (HSCCC-HPLC-DAD-MS) was developed for undisrupted purification, analysis and identification of multi-compounds from natural products. Two six-port injection valves and a six-port switching valve were used as interface for collecting key HSCCC effluents alternatively for HPLC-DAD-MS analysis and identification. The ethyl acetate extract of Malus doumeri was performed on the hyphenated system to verify its efficacy. Five main flavonoids, 3-hydroxyphloridzin (1), phloridzin (2), 4',6'-dihydroxyhydrochalcone-2'-O-β-D-glucopyranoside (3, first found in M. doumeri), phloretin (4), and chrysin (5), were purified with purities over 99% by extrusion elution and/or stepwise elution mode in two-step HSCCC, and 25mM ammonium acetate solution was selected instead of water to depress emulsification in the first HSCCC. The online system shortened manipulation time largely compared with off-line analysis procedure and stop-and-go scheme. The results indicated that the present method could serve as a simple, rapid and effective way to achieve target compounds with high purity from natural products. Copyright © 2015 Elsevier B.V. All rights reserved.

Synchronization of optical photons for quantum information processing.

PubMed

Makino, Kenzo; Hashimoto, Yosuke; Yoshikawa, Jun-Ichi; Ohdan, Hideaki; Toyama, Takeshi; van Loock, Peter; Furusawa, Akira

2016-05-01

A fundamental element of quantum information processing with photonic qubits is the nonclassical quantum interference between two photons when they bunch together via the Hong-Ou-Mandel (HOM) effect. Ultimately, many such photons must be processed in complex interferometric networks. For this purpose, it is essential to synchronize the arrival times of the flying photons and to keep their purities high. On the basis of the recent experimental success of single-photon storage with high purity, we demonstrate for the first time the HOM interference of two heralded, nearly pure optical photons synchronized through two independent quantum memories. Controlled storage times of up to 1.8 μs for about 90 events per second were achieved with purities that were sufficiently high for a negative Wigner function confirmed with homodyne measurements.

Synchronization of optical photons for quantum information processing

PubMed Central

Makino, Kenzo; Hashimoto, Yosuke; Yoshikawa, Jun-ichi; Ohdan, Hideaki; Toyama, Takeshi; van Loock, Peter; Furusawa, Akira

2016-01-01

A fundamental element of quantum information processing with photonic qubits is the nonclassical quantum interference between two photons when they bunch together via the Hong-Ou-Mandel (HOM) effect. Ultimately, many such photons must be processed in complex interferometric networks. For this purpose, it is essential to synchronize the arrival times of the flying photons and to keep their purities high. On the basis of the recent experimental success of single-photon storage with high purity, we demonstrate for the first time the HOM interference of two heralded, nearly pure optical photons synchronized through two independent quantum memories. Controlled storage times of up to 1.8 μs for about 90 events per second were achieved with purities that were sufficiently high for a negative Wigner function confirmed with homodyne measurements. PMID:27386536

Synthesis of an allergy inducing tetrasaccharide "4P-X".

PubMed

Moriya, Takashi; Nagahata, Naoki; Odaka, Rei; Nakamura, Hirohide; Yoshikawa, Jun; Kurashima, Katsumi; Saito, Tadao

2017-02-01

4P-X (β-D-galactopyranosyl-(1 → 4)-β-D-galactopyranosyl-(1 → 6)-[β-D-galactopyranosyl-(1 → 4)]-β-D-glucopyranose) is included in galacto-oligosaccharides (GOSs) produced by β-galactosidase derived from Bacillus circulans. 4P-X has been known to induce particularly strong allergies. High purity 4P-X is essential for use as a standard to quantify the amount of 4P-X in GOSs; however, the isolation of high purity 4P-X has never been reported. In this study, we achieved the synthesis of 4P-X by a combination of organic and enzymatic chemical syntheses in a short time. This is the first report of isolated, high purity 4P-X. Copyright © 2017 Elsevier Ltd. All rights reserved.

Purity assessment of condensed tannin fractions by nuclear magnetic resonance (NMR) spectroscopy

USDA-ARS?s Scientific Manuscript database

Unambiguous investigation of condensed tannin (CT) structure-activity relationships in biological systems requires the use of highly enriched CT fractions of defined chemical purity. Purification of CTs from Sorghum bicolor, Trifolium repens, Theobroma cacao, Lespedeza cuneata, Lotus pedunculatus, a...

Mechanisms for Ductile Rupture - FY16 ESC Progress Report

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

Boyce, Brad L.; Carroll, Jay D.; Noell, Phillip

2017-01-01

Ductile rupture in metals is generally a multi-step process of void nucleation, growth, and coalescence. Particle decohesion and particle fracture are generally invoked as the primary microstructural mechanisms for room-temperature void nucleation. However, because high-purity materials also fail by void nucleation and coalescence, other microstructural features must also act as sites for void nucleation. Early studies of void initiation in high-purity materials, which included post-mortem fracture surface characterization using scanning electron microscopy (SEM) and high-voltage electron microscopy (HVEM) and in-situ HVEM observations of fracture, established the presence of dislocation cell walls as void initiation sites in high-purity materials. Direct experimentalmore » evidence for this contention was obtained during in-situ HVEM tensile tests of Be single crystals. Voids between 0.2 and 1 μm long appeared suddenly along dislocation cell walls during tensile straining. However, subsequent attempts to replicate these results in other materials, particularly α -Fe single crystals, were unsuccessful because of the small size of the dislocation cells, and these remain the only published in-situ HVEM observations of void nucleation at dislocation cell walls in the absence of a growing macrocrack. Despite this challenge, other approaches to studying void nucleation in high-purity metals also indicate that dislocation cell walls are nucleation sites for voids.« less

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

PubMed

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

2015-04-01

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

Method and apparatus for measuring lung density by Compton backscattering

DOEpatents

Loo, B.W.; Goulding, F.S.

1988-03-11

The density of the lung of a patient suffering from pulmonary edema is monitored by irradiating the lung by a single collimated beam of monochromatic photons and measuring the energies of photons compton back-scattered from the lung by a single high-resolution, high-purity germanium detector. A compact system geometry and a unique data extraction scheme are utilized to minimize systematic errors due to the presence of the chestwall and multiple scattering. 11 figs., 1 tab.

Super-SERS-active and highly effective antimicrobial Ag nanodendrites

NASA Astrophysics Data System (ADS)

Li, H. B.; Liu, P.; Liang, Y.; Xiao, J.; Yang, G. W.

2012-07-01

We have developed simple and green electrochemistry to synthesize Ag nanostructures with high purity, good crystallinity and smooth surface for applications as super-SERS (surface-enhanced Raman scattering), SERS-active substrates and with highly effective antimicrobial activities. This synthesis takes place in a clean and slow reaction environment without any chemical additives, which ensures an ultrahigh active surface of the as-synthesized Ag nanostructures owing to their purity, good crystallinity and smooth morphology. Using this method, we synthesized nearly perfect Ag nanodendrites (NDs), which exhibit super-SERS sensitivity when they are used to detect the SERS spectra of rhodamine 6G at concentrations as low as 5 × 10-16 M, and have an ultrahigh electromagnetic (EM) enhancement factor of the order of 1013, breaking through the theoretical limit of EM enhancement. Meanwhile, the as-synthesized Ag NDs possess highly effective antimicrobial activities for Escherichia coli, Candida albicans and Staphylococcus aureus, which are over 10 times that of silver nanoparticles. Additionally, the basic physics and chemistry involved in the fabrication of Ag nanostructures are pursued. These investigations show that silver nanostructures with highly active surfaces can make the most of Ag nanostructures functioning as super-SERS-active substrates and multiple antibiotics.

The 124Sb activity standardization by gamma spectrometry for medical applications

NASA Astrophysics Data System (ADS)

de Almeida, M. C. M.; Iwahara, A.; Delgado, J. U.; Poledna, R.; da Silva, R. L.

2010-07-01

This work describes a metrological activity determination of 124Sb, which can be used as radiotracer, applying gamma spectrometry methods with hyper pure germanium detector and efficiency curves. This isotope with good activity and high radionuclidic purity is employed in the form of meglumine antimoniate (Glucantime) or sodium stibogluconate (Pentostam) to treat leishmaniasis. 124Sb is also applied in animal organ distribution studies to solve some questions in pharmacology. 124Sb decays by β-emission and it produces several photons (X and gamma rays) with energy varying from 27 to 2700 keV. Efficiency curves to measure point 124Sb solid sources were obtained from a 166mHo standard that is a multi-gamma reference source. These curves depend on radiation energy, sample geometry, photon attenuation, dead time and sample-detector position. Results for activity determination of 124Sb samples using efficiency curves and a high purity coaxial germanium detector were consistent in different counting geometries. Also uncertainties of about 2% ( k=2) were obtained.

Green synthesis of copper oxide (CuO) nanoparticles using banana peel extract and their photocatalytic activities

NASA Astrophysics Data System (ADS)

Aminuzzaman, Mohammod; Kei, Leong Mei; Liang, Wong Hong

2017-04-01

Copper oxide nanoparticles (CuO NPs) are interesting class of materials having multifunctional properties with promising applications in the areas of catalysts, gas sensors, batteries, magnetic storage media, solar energy, superconductors etc. Thus synthesis of CuO NPs has attracted tremendous interest to scientists and researchers Herein, we reported a green and simple method for biosynthesizing CuO NPs using banana peel extract as reducing and stabilizing agent. XRD, EDX, FE-SEM, FTIR have been used for characterization of biosynthesized CuO NPs. The results indicating that the CuO NPs synthesized by banana peel extract have high purity and the average particles size is 60 nm. The photocatalytic activity of the CuO NPs has been investigated by degradation of Congo red (CR) dye under solar irradiation. The extent of CR dye degradation by CuO NPs is monitored by using a UV-visible spectrophotometer. Due to the smaller size and high purity, the biosynthesized CuO NPs showed an excellent photocatlytic activity.

Pretreatment with ethanol as an alternative to improve steviol glycosides extraction and purification from a new variety of stevia.

PubMed

Formigoni, Maysa; Milani, Paula Gimenez; da Silva Avíncola, Alexandre; Dos Santos, Vanessa Jorge; Benossi, Livia; Dacome, Antônio Sergio; Pilau, Eduardo Jorge; da Costa, Silvio Claudio

2018-02-15

Leaves of a new variety of Stevia rebaudiana with a high content of rebaudioside A were pretreated with ethanol. The ethanolic extract showed high antioxidant potential and 39 compounds were identified, by UPLC/HRMS, among them one not yet mentioned in the literature for stevia leaves. From the in natura leaves and pretreated leaves, the conditions of aqueous extraction of steviol glycosides were investigated using response surface methodology. The aqueous extracts obtained were purified by ion exchange chromatography techniques and membrane separation methods. The recuperation of steviol glycosides was 4.02g for pretreated leaves and 2.20g for in natura leaves. The level of purity was, respectively, 87% and 84.8%. The results obtained demonstrate that pretreatment increases the yield and purity level of stevia sweeteners by the use of environmentally friendly methodologies and the final product presented acceptable sensory characteristics. Copyright © 2017 Elsevier Ltd. All rights reserved.

A novel algorithm for solving the true coincident counting issues in Monte Carlo simulations for radiation spectroscopy.

PubMed

Guan, Fada; Johns, Jesse M; Vasudevan, Latha; Zhang, Guoqing; Tang, Xiaobin; Poston, John W; Braby, Leslie A

2015-06-01

Coincident counts can be observed in experimental radiation spectroscopy. Accurate quantification of the radiation source requires the detection efficiency of the spectrometer, which is often experimentally determined. However, Monte Carlo analysis can be used to supplement experimental approaches to determine the detection efficiency a priori. The traditional Monte Carlo method overestimates the detection efficiency as a result of omitting coincident counts caused mainly by multiple cascade source particles. In this study, a novel "multi-primary coincident counting" algorithm was developed using the Geant4 Monte Carlo simulation toolkit. A high-purity Germanium detector for ⁶⁰Co gamma-ray spectroscopy problems was accurately modeled to validate the developed algorithm. The simulated pulse height spectrum agreed well qualitatively with the measured spectrum obtained using the high-purity Germanium detector. The developed algorithm can be extended to other applications, with a particular emphasis on challenging radiation fields, such as counting multiple types of coincident radiations released from nuclear fission or used nuclear fuel.

Tuning single-photon sources for telecom multi-photon experiments.

PubMed

Greganti, Chiara; Schiansky, Peter; Calafell, Irati Alonso; Procopio, Lorenzo M; Rozema, Lee A; Walther, Philip

2018-02-05

Multi-photon state generation is of great interest for near-future quantum simulation and quantum computation experiments. To-date spontaneous parametric down-conversion is still the most promising process, even though two major impediments still exist: accidental photon noise (caused by the probabilistic non-linear process) and imperfect single-photon purity (arising from spectral entanglement between the photon pairs). In this work, we overcome both of these difficulties by (1) exploiting a passive temporal multiplexing scheme and (2) carefully optimizing the spectral properties of the down-converted photons using periodically-poled KTP crystals. We construct two down-conversion sources in the telecom wavelength regime, finding spectral purities of > 91%, while maintaining high four-photon count rates. We use single-photon grating spectrometers together with superconducting nanowire single-photon detectors to perform a detailed characterization of our multi-photon source. Our methods provide practical solutions to produce high-quality multi-photon states, which are in demand for many quantum photonics applications.

Purity-activity relationships of natural products: the case of anti-TB active ursolic acid.

PubMed

Jaki, Birgit U; Franzblau, Scott G; Chadwick, Lucas R; Lankin, David C; Zhang, Fangqiu; Wang, Yuehong; Pauli, Guido F

2008-10-01

The present study explores the variability of biological responses from the perspective of sample purity and introduces the concept of purity-activity relationships (PARs) in natural product research. The abundant plant triterpene ursolic acid (1) was selected as an exemplary natural product due to the overwhelming number yet inconsistent nature of its approximate 120 reported biological activities, which include anti-TB potential. Nine different samples of ursolic acid with purity certifications were obtained, and their purity was independently assessed by means of quantitative 1H NMR (qHNMR). Biological evaluation consisted of determining MICs against two strains of virulent Mycobacterium tuberculosis and IC50 values in Vero cells. Ab initio structure elucidation provided unequivocal structural confirmation and included an extensive 1H NMR spin system analysis, determination of nearly all J couplings and the complete NOE pattern, and led to the revision of earlier reports. As a net result, a sigmoid PAR profile of 1 was obtained, demonstrating the inverse correlation of purity and anti-TB bioactivity. The results imply that synergistic effects of 1 and its varying impurities are the likely cause of previously reported antimycobacterial potential. Generating PARs is a powerful extension of the routinely performed quantitative correlation of structure and activity ([Q]SAR). Advanced by the use of primary analytical methods such as qHNMR, PARs enable the elucidation of cases like 1 when increasing purity voids biological activity. This underlines the potential of PARs as a tool in drug discovery and synergy research and accentuates the need to routinely combine biological testing with purity assessment.

Hybrid pulse anodization for the fabrication of porous anodic alumina films from commercial purity (99%) aluminum at room temperature.

PubMed

Chung, C K; Zhou, R X; Liu, T Y; Chang, W T

2009-02-04

Most porous anodic alumina (PAA) or anodic aluminum oxide (AAO) films are fabricated using the potentiostatic method from high-purity (99.999%) aluminum films at a low temperature of approximately 0-10 degrees C to avoid dissolution effects at room temperature (RT). In this study, we have demonstrated the fabrication of PAA film from commercial purity (99%) aluminum at RT using a hybrid pulse technique which combines pulse reverse and pulse voltages for the two-step anodization. The reaction mechanism is investigated by the real-time monitoring of current. A possible mechanism of hybrid pulse anodization is proposed for the formation of pronounced nanoporous film at RT. The structure and morphology of the anodic films were greatly influenced by the duration of anodization and the type of voltage. The best result was obtained by first applying pulse reverse voltage and then pulse voltage. The first pulse reverse anodization step was used to form new small cells and pre-texture concave aluminum as a self-assembled mask while the second pulse anodization step was for the resulting PAA film. The diameter of the nanopores in the arrays could reach 30-60 nm.

Cleaning and passivation of copper surfaces to remove surface radioactivity and prevent oxide formation

NASA Astrophysics Data System (ADS)

Hoppe, E. W.; Seifert, A.; Aalseth, C. E.; Bachelor, P. P.; Day, A. R.; Edwards, D. J.; Hossbach, T. W.; Litke, K. E.; McIntyre, J. I.; Miley, H. S.; Schulte, S. M.; Smart, J. E.; Warren, G. A.

2007-08-01

High-purity copper is an attractive material for constructing ultra-low-background radiation measurement devices. Many low-background experiments using high-purity copper have indicated surface contamination emerges as the dominant background. Radon daughters plate out on exposed surfaces, leaving a residual 210Pb background that is difficult to avoid. Dust is also a problem; even under cleanroom conditions, the amount of U and Th deposited on surfaces can represent the largest remaining background. To control these backgrounds, a copper cleaning chemistry has been developed. Designed to replace an effective, but overly aggressive concentrated nitric acid etch, this peroxide-based solution allows for a more controlled cleaning of surfaces. The acidified hydrogen peroxide solution will generally target the Cu +/Cu 2+ species which are the predominant surface participants, leaving the bulk of copper metal intact. This preserves the critical tolerances of parts and eliminates significant waste disposal issues. Accompanying passivation chemistry has also been developed that protects copper surfaces from oxidation. Using a high-activity polonium surface spike, the most difficult-to-remove daughter isotope of radon, the performance of these methods are quantified.

Mechanical and physicochemical properties of AlN thin films obtained by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Cibert, C.; Tétard, F.; Djemia, P.; Champeaux, C.; Catherinot, A.; Tétard, D.

2004-10-01

AlN thin films have been deposited on Si(100) substrates by a pulsed laser deposition method. The deposition parameters (pressure, temperature, purity of target) play an important role in the mechanical and physicochemical properties. The films have been characterized using X-ray diffraction, atomic force microscopy, Brillouin light scattering, Fourier transform infrared spectroscopy and wettability testing. With a high purity target of AlN and a temperature deposition of 750 ∘C, the measured Rayleigh wave velocity is close to the one previously determined for AlN films grown at high temperature by metal-organic chemical vapour deposition. Growth of nanocrystalline AlN at low temperature and of AlN film with good crystallinity for samples deposited at higher temperature is confirmed by infrared spectroscopy, as it was by atomic force microscopy, in agreement with X-ray diffraction results. A high hydrophobicity has been measured with zero polar contribution for the surface energy. These results confirm that films made by pulsed laser deposition of pure AlN at relatively low temperature have good prospects for microelectromechanical systems applications.

Analysis of the High-Performance Liquid Chromatography Fingerprints and Quantitative Analysis of Multicomponents by Single Marker of Products of Fermented Cordyceps sinensis

PubMed Central

Guan, Yong-mei; Jin, Chen; Zhu, Wei-feng; Yang, Ming

2018-01-01

Fermented Cordyceps sinensis, the succedaneum of Cordyceps sinensis which is extracted and separated from Cordyceps sinensis by artificial fermentation, is commonly used in eastern Asia in clinical treatments due to its health benefit. In this paper, a new strategy for differentiating and comprehensively evaluating the quality of products of fermented Cordyceps sinensis has been established, based on high-performance liquid chromatography (HPLC) fingerprint analysis combined with similar analysis (SA), hierarchical cluster analysis (HCA), and the quantitative analysis of multicomponents by single marker (QAMS). Ten common peaks were collected and analysed using SA, HCA, and QAMS. These methods indicated that 30 fermented Cordyceps sinensis samples could be categorized into two groups by HCA. Five peaks were identified as uracil, uridine, adenine, guanosine, and adenosine, and according to the results from the diode array detector, which can be used to confirm peak purity, the purities of these compounds were greater than 990. Adenosine was chosen as the internal reference substance. The relative correction factors (RCF) between adenosine and the other four nucleosides were calculated and investigated using the QAMS method. Meanwhile, the accuracy of the QAMS method was confirmed by comparing the results of that method with those of an external standard method with cosines of the angles between the groups. No significant difference between the two methods was observed. In conclusion, the method established herein was efficient, successful in identifying the products of fermented Cordyceps sinensis, and scientifically valid to be applicable in the systematic quality control of fermented Cordyceps sinensis products. PMID:29850373

Analysis of the High-Performance Liquid Chromatography Fingerprints and Quantitative Analysis of Multicomponents by Single Marker of Products of Fermented Cordyceps sinensis.

PubMed

Chen, Li-Hua; Wu, Yao; Guan, Yong-Mei; Jin, Chen; Zhu, Wei-Feng; Yang, Ming

2018-01-01

Fermented Cordyceps sinensis , the succedaneum of Cordyceps sinensis which is extracted and separated from Cordyceps sinensis by artificial fermentation, is commonly used in eastern Asia in clinical treatments due to its health benefit. In this paper, a new strategy for differentiating and comprehensively evaluating the quality of products of fermented Cordyceps sinensis has been established, based on high-performance liquid chromatography (HPLC) fingerprint analysis combined with similar analysis (SA), hierarchical cluster analysis (HCA), and the quantitative analysis of multicomponents by single marker (QAMS). Ten common peaks were collected and analysed using SA, HCA, and QAMS. These methods indicated that 30 fermented Cordyceps sinensis samples could be categorized into two groups by HCA. Five peaks were identified as uracil, uridine, adenine, guanosine, and adenosine, and according to the results from the diode array detector, which can be used to confirm peak purity, the purities of these compounds were greater than 990. Adenosine was chosen as the internal reference substance. The relative correction factors (RCF) between adenosine and the other four nucleosides were calculated and investigated using the QAMS method. Meanwhile, the accuracy of the QAMS method was confirmed by comparing the results of that method with those of an external standard method with cosines of the angles between the groups. No significant difference between the two methods was observed. In conclusion, the method established herein was efficient, successful in identifying the products of fermented Cordyceps sinensis , and scientifically valid to be applicable in the systematic quality control of fermented Cordyceps sinensis products.

Comparison of six methods for the recovery of PCR-compatible microbial DNA from an agricultural biogas plant.

PubMed

Stagnati, L; Soffritti, G; Lanubile, A; Busconi, M

2017-05-01

Six different commercial methods were compared to evaluate their efficiency in recovering high quantity/quality PCR compatible microbial DNA from an agricultural biogas plant. Within the last two decades, biogas plants have been developed to produce energy from organic wastes and from devoted biomass. The complex biotransformations are performed by a diverse consortium of microorganisms that is an important reserve of genes and enzymatic activities with a huge range of applications in various commercial fields. In this respect, the ability to isolate DNA from a complex matrix is of high importance. Important parameters of the recovered DNA are good yield, purity, and quality. The methods examined showed considerable differences about quantity and quality of the recovered DNA and, usually, it was observed that a higher amount was accompanied by more degradation. DNA purity was determined by its PCR amplificability. Only two methods were able to provide DNA pure enough to be directly amplified. For the rest of the methods, a few intermediate steps such as dilution and/or the addition of polyvinylpyrrolidone were necessary to remove the inhibitors present and to amplify the DNA. Real-time PCR analysis evidenced that, as expected, prokaryotic DNA was much more abundant than eukaryotic DNA, but some methods were more suited to recovering prokaryotic or eukaryotic DNA. The digestion analysis of ribosomal DNA amplicons confirmed the influence of the methods on the final output, allowing the recovery of only a fraction of the present species as determined by sequencing a small prokaryotic and eukaryotic ribosomal library.

High purity silica reflecting heat shield development

NASA Technical Reports Server (NTRS)

Congdon, W.

1974-01-01

A reflecting heat shield composed of fused silica in which the scattering results from the refractive index mismatch between silica particles and the voids introduced during the fabrication process is developed. Major considerations and conclusions of the development are: the best material to use is Type A, which is capable of ultra-high-purity and which does not show the 0.243 micrometer absorption band; the reflection efficiency of fused silica is decreased at higher temperatures due to the bathochromic shift of the ultraviolet cut-off; for a given silica material, over the wavelength region and particle sizes tested, the monodisperse particle size configurations produce higher reflectances than continuous particle size configurations; and the smaller monodisperse particle size configurations give higher reflectance than the larger ones. A reflecting silica configuration that is an efficient reflector of shock layer radiation at high ablation temperatures is achieved by tailoring the matrix for optimum scattering and using an ultra-high-purity material.

Radiolabeled Exosomes for the Early Detection of Metastases and to Predict Breast Cancer Premetastatic Niche

DTIC Science & Technology

2014-08-01

purification methods such as ultra-centrifugation at 100,000g for 2-3 hours and/or gel filtration on PD-10 columns. Specific Aim 2.2. Iodine - 131 ...with I- 131 was performed 6 5 using the Iodogen method and PIERCE® pre-coated iodination tubes. Na131I of high radiochemical purity was supplied by...hydroxyphenylpropionic acid that serves as free I- 131 scavenger. Unbound I- 131 was removed by size exclusion chromatography on PD-10 columns pre

The Separation of a High Purity Tellurium Contained in the Roumain Ores; LA SEPARATION DE TELLURE TRES PUR CONTENU DANS LES MINERAIS ROUMAINS

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

Ripan, R.; Hulubei, H.; Marco, G.

1959-10-31

A method is descrihed for the recovery of tellurium from the by-products of gold and silver refintng. The tellurium is separated with acetic acid and recovered by distillation. A method of purifying the crude tellurium is given. An economic process for the purification of tellurium as the water soluble product Te(OH)/sub 6/, used in the preparation of I/sup 131/, is also discussed. (J.S.R.)

Nondestructive inspection of explosive materials using linearly polarized two-colored photon beam

NASA Astrophysics Data System (ADS)

Toyokawa, H.; Hayakawa, T.; Shizuma, T.; Hajima, R.; Masuda, K.; Ohgaki, H.

2011-10-01

A nondestructive inspection method for screening explosive materials that are hidden in passenger vehicles, trucks, and cargo containers with radiation shielding was presented. The method was examined experimentally using linearly polarized two-colored photon beam. A sample object was irradiated with the photon beam, followed by an emission of gamma-rays in nuclear resonance fluorescence. The gamma-rays from oxygen and nitrogen emitted through nuclear resonance fluorescence were measured using high-purity germanium detectors. We were able to evaluate the element concentration ratio.

Compact Layers of Hybrid Halide Perovskites Fabricated via the Aerosol Deposition Process-Uncoupling Material Synthesis and Layer Formation.

PubMed

Panzer, Fabian; Hanft, Dominik; Gujar, Tanaji P; Kahle, Frank-Julian; Thelakkat, Mukundan; Köhler, Anna; Moos, Ralf

2016-04-08

We present the successful fabrication of CH₃NH₃PbI₃ perovskite layers by the aerosol deposition method (ADM). The layers show high structural purity and compactness, thus making them suitable for application in perovskite-based optoelectronic devices. By using the aerosol deposition method we are able to decouple material synthesis from layer processing. Our results therefore allow for enhanced and easy control over the fabrication of perovskite-based devices, further paving the way for their commercialization.

Isolation of oxidative degradation products of atorvastatin with supercritical fluid chromatography.

PubMed

Klobčar, Slavko; Prosen, Helena

2015-12-01

The isolation of four oxidative degradation products of atorvastatin using preparative high-performance liquid chromatography applying at least two chromatographic steps is known from the literature. In this paper it is shown that the same four impurities could be isolated from similarly prepared mixtures in only one step using supercritical fluid chromatography. The methods for separation were developed and optimized. The preparation of the mixtures was altered in such a way as to enhance the concentration of desired impurities. Appropriate solvents were applied for collection of separated impurities in order to prevent degradation. The structures of the isolated impurities were confirmed and their purity determined. The preparative supercritical fluid chromatography has proven to be superior to preparative HPLC regarding achieved purity of standards applying fewer chromatographic as well as isolation steps. Copyright © 2015 John Wiley & Sons, Ltd.

High-efficiency spectral purity filter for EUV lithography

DOEpatents

Chapman, Henry N [Livermore, CA

2006-05-23

An asymmetric-cut multilayer diffracts EUV light. A multilayer cut at an angle has the same properties as a blazed grating, and has been demonstrated to have near-perfect performance. Instead of having to nano-fabricate a grating structure with imperfections no greater than several tens of nanometers, a thick multilayer is grown on a substrate and then cut at an inclined angle using coarse and inexpensive methods. Effective grating periods can be produced this way that are 10 to 100 times smaller than those produced today, and the diffraction efficiency of these asymmetric multilayers is higher than conventional gratings. Besides their ease of manufacture, the use of an asymmetric multilayer as a spectral purity filter does not require that the design of an EUV optical system be modified in any way, unlike the proposed use of blazed gratings for such systems.

Recovery behavior of high purity cubic SiC polycrystals by post-irradiation annealing up to 1673 K after low temperature neutron irradiation

NASA Astrophysics Data System (ADS)

Idris, Mohd Idzat; Yamazaki, Saishun; Yoshida, Katsumi; Yano, Toyohiko

2015-10-01

Two kinds of high purity cubic (β) SiC polycrystals, PureBeta-SiC and CVD-SiC, were irradiated in the BR2 reactor (Belgium) up to a fluence of 2.0-2.5 × 1024 (E > 0.1 MeV) at 333-363 K. Changes in macroscopic lengths were examined by post-irradiation thermal annealing using a precision dilatometer up to 1673 K with a step-heating method. The specimen was held at each temperature step for 6 h and the change in length of the specimen was recorded during each isothermal annealing step from 373 K to 1673 K with 50 K increments. The recovery curves were analyzed with the first order model, and rate constants at each annealing step were obtained. Recovery of defects, induced by neutron irradiation in high purity β-SiC, has four stages of different activation energies. At 373-573 K, the activation energy of PureBeta-SiC and CVD-SiC was in the range of 0.17-0.24 eV and 0.12-0.14 eV; 0.002-0.04 eV and 0.006-0.04 eV at 723-923 K; 0.20-0.27 eV and 0.26-0.31 eV at 923-1223 K; and 1.37-1.38 eV and 1.26-1.29 eV at 1323-1523 K, respectively. Below ∼1223 K the recombination occurred possibly for closely positioned C and Si Frenkel pairs, and no long range migration is deemed essential. Nearly three-fourths of recovery, induced by neutron irradiation, occur by this mechanism. In addition, at 1323-1523 K, recombination of slightly separated C Frenkel pairs and more long-range migration of Si interstitials may have occurred for PureBeta-SiC and CVD-SiC specimens. Migration of both vacancies may be restricted up to ∼1523 K. Comparing to hexagonal α-SiC, high purity β-SiC recovered more quickly in the lower annealing temperature range of less than 873 K, in particular less than 573 K.

Pulsed laser activated cell sorter (PLACS) for high-throughput fluorescent mammalian cell sorting

NASA Astrophysics Data System (ADS)

Chen, Yue; Wu, Ting-Hsiang; Chung, Aram; Kung, Yu-Chung; Teitell, Michael A.; Di Carlo, Dino; Chiou, Pei-Yu

2014-09-01

We present a Pulsed Laser Activated Cell Sorter (PLACS) realized by exciting laser induced cavitation bubbles in a PDMS microfluidic channel to create high speed liquid jets to deflect detected fluorescent samples for high speed sorting. Pulse laser triggered cavitation bubbles can expand in few microseconds and provide a pressure higher than tens of MPa for fluid perturbation near the focused spot. This ultrafast switching mechanism has a complete on-off cycle less than 20 μsec. Two approaches have been utilized to achieve 3D sample focusing in PLACS. One is relying on multilayer PDMS channels to provide 3D hydrodynamic sheath flows. It offers accurate timing control of fast (2 m sec-1) passing particles so that synchronization with laser bubble excitation is possible, an critically important factor for high purity and high throughput sorting. PLACS with 3D hydrodynamic focusing is capable of sorting at 11,000 cells/sec with >95% purity, and 45,000 cells/sec with 45% purity using a single channel in a single step. We have also demonstrated 3D focusing using inertial flows in PLACS. This sheathless focusing approach requires 10 times lower initial cell concentration than that in sheath-based focusing and avoids severe sample dilution from high volume sheath flows. Inertia PLACS is capable of sorting at 10,000 particles sec-1 with >90% sort purity.

Radiopharmaceutical considerations for using Tc-99m MAA in lung transplant patients.

PubMed

Ponto, James A

2010-01-01

To elucidate radiopharmaceutical considerations for using technetium Tc-99m albumin aggregated (Tc-99m MAA) in lung transplant patients and to establish an appropriate routine dose and preparation procedure. Tertiary care academic hospital during May 2007 to May 2009. Nuclear pharmacist working in nuclear medicine department. Radiopharmaceutical considerations deemed important for the use of Tc-99m MAA in lung transplant patients included radioactivity dose, particulate dose, rate of the radiolabeling reaction (preparation time), and final radiochemical purity. Evaluation of our initial 12-month experience, published literature, and professional practice guidelines provided the basis for establishing an appropriate dose and preparation procedure of Tc-99m MAA for use in lung transplant patients. Radiochemical purity at typical incubation times and image quality in subsequent lung transplant patients imaged during the next 12 months. Based on considerations of radioactivity dose, particulate dose, rate of the radiolabeling reaction (preparation time), and final radiochemical purity, a routine dose consisting of 3 mCi (111 MBq) and 100,000 particles of Tc-99m MAA for planar perfusion lung imaging of adult lung transplant patients was established as reasonable and appropriate. MAA kits were prepared with a more reasonable amount of Tc-99m and yielded high radiochemical purity values in typical incubation times. Images have continued to be of high diagnostic quality. Tc-99m MAA used for lung transplant imaging can be readily prepared with high radiochemical purity to provide a dose of 3 mCi (111 GBq)/100,000 particles, which provides images of high diagnostic quality.

Preparation of 99Tcm-MAG3: no confirmation that sodium chloride injections from plastic containers affect radiochemical purity.

PubMed

Millar, A M; O'Brien, L M

1998-05-01

Reports have suggested that when sodium chloride injections from a plastic ampoule are used during the preparation of 99Tcm-mercaptoacetyltriglycine (99Tcm-MAG3), the radiochemical purity of the final product might be reduced. A study was therefore undertaken to examine the effect of sodium chloride injections from five manufacturers on the radiochemical purity and stability of 99Tcm-MAG3. One sodium chloride injection was supplied in a glass vial, three in plastic ampoules and one in a plastic infusion bag. Three batches of sodium chloride injections from each manufacturer were tested. The radiopharmaceutical was prepared at a radioactive concentration of 1.1 GBq in 10 ml according to the instructions of the manufacturer of TechneScan MAG3. Analysis of radiochemical purity was performed by high-performance liquid chromatography immediately after preparation and 6 h later. Using 95% as the minimum acceptable radiochemical purity, all the products were satisfactory over the 6 h test period. No manufacturer's sodium chloride injection was found to have a statistically significant effect on the radiochemical purity. Based on the 15 batches of sodium chloride injection tested, this study cannot confirm that sodium chloride injections from a plastic container affect the radiochemical purity of 99Tcm-MAG3. However, in view of the known sensitivity of some 99Tcm radiopharmaceuticals to external influences, it is probably good practice to test radiochemical purity when new batches of ancillary materials, such as sodium chloride injections, are introduced.

Ultrasound-assisted phase-transfer catalysis method in an aqueous medium to promote the Knoevenagel reaction: advantages over the conventional and microwave-assisted solvent-free/catalyst-free method.

PubMed

De-la-Torre, Pedro; Osorio, Edison; Alzate-Morales, Jans H; Caballero, Julio; Trilleras, Jorge; Astudillo-Saavedra, Luis; Brito, Iván; Cárdenas, Alejandro; Quiroga, Jairo; Gutiérrez, Margarita

2014-09-01

Given the broad spectrum of uses of acrylonitrile derivatives as fluorescent probes, AChE inhibitors, and others, it is necessary to find easy, efficient and simple methods to synthesize and diversify these compounds. We report the results of a comparative study of the effects of three techniques on the reactions between heterocyclic aldehydes and 2-(benzo[d]thiazol-2-yl)acetonitrile: stirring; ultrasound coupled to PTC conditions (US-PTC); and MW irradiation (MWI) under solvent and catalyst-free conditions. The effects of conditions on reaction parameters were evaluated and compared in terms of reaction time, yield, purity and outcomes. The US-PTC method is more efficient than the MWI and conventional methods. The reaction times were considerably shorter, with high yields (>90%) and good levels of purity. In addition, X-ray diffraction analysis and quantum mechanical calculations, at the level of density functional theory (DFT), ratify obtaining acrylonitrile isomers with E configurations. The crystal structure of 3c is stabilized by weak C-Ho⋯N intermolecular interactions (Ho⋯NC=2.45 Å, Co⋯NC=3.348(3) Å, Ho⋯NC=162°), forming centrosymmetric ring R2(2) (20) along the crystallographic a axis. Copyright © 2014 Elsevier B.V. All rights reserved.

Cross Purposes: Love and Purity at a Puerto Rican Protestant High School

ERIC Educational Resources Information Center

Seale-Collazo, James

2013-01-01

A "native" Christian ethnographer finds religious education at this church-sponsored school to pursue two distinct, and occasionally conflicting, curricula: "love" and "purity." The curriculum of love draws on what Turner called liminality and communitas in an effort to promote spiritual "encounters with…

Characterization of a high-purity germanium detector for small-animal SPECT

PubMed Central

Johnson, Lindsay C; Campbell, Desmond L; Hull, Ethan L; Peterson, Todd E

2011-01-01

We present an initial evaluation of a mechanically-cooled, high-purity germanium double-sided strip detector as a potential gamma camera for small-animal SPECT. It is 90 mm in diameter and 10 mm thick with two sets of 16 orthogonal strips that have a 4.5 mm width with a 5 mm pitch. We found an energy resolution of 0.96% at 140 keV, an intrinsic efficiency of 43.3% at 122 keV and a FWHM spatial resolution of approximately 1.5 mm. We demonstrated depth-of-interaction estimation capability through comparison of pinhole acquisitions with a point source on and off axis. Finally, a flood-corrected-flood image exhibited a strip-level uniformity of less than 1%. This high-purity germanium offers many desirable properties for small-animal SPECT. PMID:21852723

Characterization of a high-purity germanium detector for small-animal SPECT.

PubMed

Johnson, Lindsay C; Campbell, Desmond L; Hull, Ethan L; Peterson, Todd E

2011-09-21

We present an initial evaluation of a mechanically cooled, high-purity germanium double-sided strip detector as a potential gamma camera for small-animal SPECT. It is 90 mm in diameter and 10 mm thick with two sets of 16 orthogonal strips that have a 4.5 mm width with a 5 mm pitch. We found an energy resolution of 0.96% at 140 keV, an intrinsic efficiency of 43.3% at 122 keV and a FWHM spatial resolution of approximately 1.5 mm. We demonstrated depth-of-interaction estimation capability through comparison of pinhole acquisitions with a point source on and off axes. Finally, a flood-corrected flood image exhibited a strip-level uniformity of less than 1%. This high-purity germanium offers many desirable properties for small-animal SPECT.

A review of the developments of radioxenon detectors for nuclear explosion monitoring

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

Sivels, Ciara B.; McIntyre, Justin I.; Bowyer, Theodore W.

Developments in radioxenon monitoring since the implementation of the International Monitoring System are reviewed with emphasis on the most current technologies to improve detector sensitivity and resolution. The nuclear detectors reviewed include combinations of plastic and NaI(Tl) detectors, high purity germanium detectors, silicon detectors, and phoswich detectors. The minimum detectable activity and calibration methods for the various detectors are also discussed.

[Study on seed quality test and quality standard of Pesudostellaria heterophylla].

PubMed

Xiao, Cheng-Hong; Zhou, Tao; Jiang, Wei-Ke; Chen, Min; Xiong, Hou-Xi; Liao, Ming-Wu

2014-08-01

Referring to the rules for agricultural seed testing (GB /T 3543-1995) issued by China, the test of sampling, seed purity, weight per 1 000 seeds, seed moisture, seed viability and germination rate had been studied for screening seed quality test methods of Pesudostellaria heterophylla. The seed quality from different collection areas was measured. The results showed that at least 6.5 g seeds should be sampled and passed through 10-mesh sieve for purity analysis. The weight of 1 000 seeds was determined by using the 500-seed method. The phenotypic observation and size measurement were used for authenticity testing. The seed moisture was determined under the higher temperature (130 ± 2) degrees C for 5 hours. The seeds were dipped into 0.2% TTC sustaining 1 hour at 40 degrees C, then the viability could be determined. The break dormancy seeds were cultured on sand at 10 degrees C. K cluster analysis was applied for the data analysis, the seed quality from different collection areas grading of P. Heterophylla was described as three grades. The seed quality of each grade should reach following requirements: for first grade seeds, germination rate ≥ 86%, 1 000-grain weight ≥ 2.59 g, purity ≥ 87%, moisture ≤ 13.1%; for second grade seeds, germination rate ≥ 70%, 1 000-grain weight ≥ 2.40 g, purity ≥ 77%, moisture ≤ 14.3%; for third grade seeds, germination rate ≥ 41%, 1 000-grain weight ≥ 2.29 g, purity ≥ 76%, moisture ≤ 15.8%. The seed testing methods for quality items of P. heterophylla had been initially established, as well as the primary P. heterophylla seed quality classification standard.

Chemical purity using quantitative 1H-nuclear magnetic resonance: a hierarchical Bayesian approach for traceable calibrations

NASA Astrophysics Data System (ADS)

Toman, Blaza; Nelson, Michael A.; Lippa, Katrice A.

2016-10-01

Chemical purity assessment using quantitative 1H-nuclear magnetic resonance spectroscopy is a method based on ratio references of mass and signal intensity of the analyte species to that of chemical standards of known purity. As such, it is an example of a calculation using a known measurement equation with multiple inputs. Though multiple samples are often analyzed during purity evaluations in order to assess measurement repeatability, the uncertainty evaluation must also account for contributions from inputs to the measurement equation. Furthermore, there may be other uncertainty components inherent in the experimental design, such as independent implementation of multiple calibration standards. As such, the uncertainty evaluation is not purely bottom up (based on the measurement equation) or top down (based on the experimental design), but inherently contains elements of both. This hybrid form of uncertainty analysis is readily implemented with Bayesian statistical analysis. In this article we describe this type of analysis in detail and illustrate it using data from an evaluation of chemical purity and its uncertainty for a folic acid material.

All-in-one centrifugal microfluidic device for size-selective circulating tumor cell isolation with high purity.

PubMed

Lee, Ada; Park, Juhee; Lim, Minji; Sunkara, Vijaya; Kim, Shine Young; Kim, Gwang Ha; Kim, Mi-Hyun; Cho, Yoon-Kyoung

2014-11-18

Circulating tumor cells (CTCs) have gained increasing attention owing to their roles in cancer recurrence and progression. Due to the rarity of CTCs in the bloodstream, an enrichment process is essential for effective target cell characterization. However, in a typical pressure-driven microfluidic system, the enrichment process generally requires complicated equipment and long processing times. Furthermore, the commonly used immunoaffinity-based positive selection method is limited, as its recovery rate relies on EpCAM expression of target CTCs, which shows heterogeneity among cell types. Here, we propose a centrifugal-force-based size-selective CTC isolation platform that can isolate and enumerate CTCs from whole blood within 30 s with high purity. The device was validated using the MCF-7 breast cancer cell line spiked in phosphate-buffered saline and whole blood, and an average capture efficiency of 61% was achieved, which is typical for size-based filtration. The capture efficiency for whole blood samples varied from 44% to 84% under various flow conditions and dilution factors. Under the optimized operating conditions, a few hundred white blood cells per 1 mL of whole blood were captured, representing a 20-fold decrease compared to those obtained using a commercialized size-based CTC isolation device. In clinical validation, normalized CTC counts varied from 10 to 60 per 7.5 mL of blood from gastric and lung cancer patients, yielding a detection rate of 50% and 38%, respectively. Overall, our CTC isolation device enables rapid and label-free isolation of CTCs with high purity, which should greatly improve downstream molecular analyses of captured CTCs.

Automated digital image analysis of islet cell mass using Nikon's inverted eclipse Ti microscope and software to improve engraftment may help to advance the therapeutic efficacy and accessibility of islet transplantation across centers.

PubMed

Gmyr, Valery; Bonner, Caroline; Lukowiak, Bruno; Pawlowski, Valerie; Dellaleau, Nathalie; Belaich, Sandrine; Aluka, Isanga; Moermann, Ericka; Thevenet, Julien; Ezzouaoui, Rimed; Queniat, Gurvan; Pattou, Francois; Kerr-Conte, Julie

2015-01-01

Reliable assessment of islet viability, mass, and purity must be met prior to transplanting an islet preparation into patients with type 1 diabetes. The standard method for quantifying human islet preparations is by direct microscopic analysis of dithizone-stained islet samples, but this technique may be susceptible to inter-/intraobserver variability, which may induce false positive/negative islet counts. Here we describe a simple, reliable, automated digital image analysis (ADIA) technique for accurately quantifying islets into total islet number, islet equivalent number (IEQ), and islet purity before islet transplantation. Islets were isolated and purified from n = 42 human pancreata according to the automated method of Ricordi et al. For each preparation, three islet samples were stained with dithizone and expressed as IEQ number. Islets were analyzed manually by microscopy or automatically quantified using Nikon's inverted Eclipse Ti microscope with built-in NIS-Elements Advanced Research (AR) software. The AIDA method significantly enhanced the number of islet preparations eligible for engraftment compared to the standard manual method (p < 0.001). Comparisons of individual methods showed good correlations between mean values of IEQ number (r(2) = 0.91) and total islet number (r(2) = 0.88) and thus increased to r(2) = 0.93 when islet surface area was estimated comparatively with IEQ number. The ADIA method showed very high intraobserver reproducibility compared to the standard manual method (p < 0.001). However, islet purity was routinely estimated as significantly higher with the manual method versus the ADIA method (p < 0.001). The ADIA method also detected small islets between 10 and 50 µm in size. Automated digital image analysis utilizing the Nikon Instruments software is an unbiased, simple, and reliable teaching tool to comprehensively assess the individual size of each islet cell preparation prior to transplantation. Implementation of this technology to improve engraftment may help to advance the therapeutic efficacy and accessibility of islet transplantation across centers.

Capillary zone electrophoresis method for a highly glycosylated and sialylated recombinant protein: development, characterization and application for process development.

PubMed

Zhang, Le; Lawson, Ken; Yeung, Bernice; Wypych, Jette

2015-01-06

A purity method based on capillary zone electrophoresis (CZE) has been developed for the separation of isoforms of a highly glycosylated protein. The separation was found to be driven by the number of sialic acids attached to each isoform. The method has been characterized using orthogonal assays and shown to have excellent specificity, precision and accuracy. We have demonstrated the CZE method is a useful in-process assay to support cell culture and purification development of this glycoprotein. Compared to isoelectric focusing (IEF), the CZE method provides more quantitative results and higher sample throughput with excellent accuracy, qualities that are required for process development. In addition, the CZE method has been applied in the stability testing of purified glycoprotein samples.

Crystal growth of Bi{sub 2}Te{sub 3} and noble cleaved (0001) surface properties

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

Atuchin, V.V., E-mail: atuchin@thermo.isp.nsc.ru; Functional Electronics Laboratory, Tomsk State University, Tomsk 634050; Golyashov, V.A.

2016-04-15

A high quality Bi{sub 2}Te{sub 3} crystal has been grown by Bridgman method with the use of rotating heat field. The phase purity and bulk structural quality of the crystal have been verified by XRD analysis and rocking curve observation. The atomically smooth Bi{sub 2}Te{sub 3}(0001) surface with an excellent crystallographic quality is formed by cleavage in the air. The chemical and microstructural properties of the surface have been evaluated with RHEED, AFM, STM, SE and XPS. The Bi{sub 2}Te{sub 3}(0001) cleaved surface is formed by atomically smooth terraces with the height of the elemental step of ~1.04±0.1 nm, asmore » estimated by AFM. There is no surface oxidation process detected over a month keeping in the air at normal conditions, as shown by comparative core level photoelectron spectroscopy. - Graphical abstract: A high quality Bi{sub 2}Te{sub 3} crystal has been grown by Bridgman method with the use of rotating heat field and the Bi{sub 2}Te{sub 3}(0001) cleaved surface has been evaluated with RHEED, AFM, STM, SE and XPS. - Highlights: • High-quality Bi{sub 2}Te{sub 3} crystal of 10 mm in diameter and 50 mm long have been grown. • The high-purity cleaved Bi{sub 2}Te{sub 3}(0001) surface has been evaluated by RHEED, AFM, STM and XPS methods. • The Bi{sub 2}Te{sub 3} surface covered by atomically smooth (0001) terraces is chemically stable for a long time.« less

Genome sequence of the thermophilic strain Bacillus coagulans 2-6, an efficient producer of high-optical-purity L-lactic acid.

PubMed

Su, Fei; Yu, Bo; Sun, Jibin; Ou, Hong-Yu; Zhao, Bo; Wang, Limin; Qin, Jiayang; Tang, Hongzhi; Tao, Fei; Jarek, Michael; Scharfe, Maren; Ma, Cuiqing; Ma, Yanhe; Xu, Ping

2011-09-01

Bacillus coagulans 2-6 is an efficient producer of lactic acid. The genome of B. coagulans 2-6 has the smallest genome among the members of the genus Bacillus known to date. The frameshift mutation at the start of the d-lactate dehydrogenase sequence might be responsible for the production of high-optical-purity l-lactic acid.

Process for preparing higher oxides of the alkali and alkaline earth metals

NASA Technical Reports Server (NTRS)

Sadhukhan, P.; Bell, A. (Inventor)

1978-01-01

High purity inorganic higher oxides of the alkali and alkaline earth metals are prepared by subjecting the hydroxide of the alkali and alkaline earth metal to a radio frequency discharge sustained in oxygen. The process is particulary adaptable to the production of high purity potassium superoxide by subjecting potassium hydroxide to glow discharge sustained in oxygen under the pressure of about 0.75 to 1.00 torr.

Normal and polar-organic-phase high-performance liquid chromatographic enantioresolution of omeprazole, rabeprazole, lansoprazole and pantoprazole using monochloro-methylated cellulose-based chiral stationary phase and determination of dexrabeprazole.

PubMed

Dixit, Shuchi; Dubey, Rituraj; Bhushan, Ravi

2014-01-01

Enantioresolution of four anti-ulcer drugs (chiral sulfoxides), namely, omeprazole, rabeprazole, lansoprazole and pantoprazole, was carried out by high-performance liquid chromatography using a polysaccharide-based chiral stationary phase consisting of monochloromethylated cellulose (Lux cellulose-2) under normal and polar-organic-phase conditions with ultraviolet detection at 285 nm. The method was validated for linearity, accuracy, precision, robustness and limit of detection. The optimized enantioresolution method was compared for both the elution modes. The optimized method was further utilized to check the enantiomeric purity of dexrabeprazole. Copyright © 2013 John Wiley & Sons, Ltd.

Synthesis of the proteinase inhibitor LEKTI domain 6 by the fragment condensation method and regioselective disulfide bond formation.

PubMed

Vasileiou, Zoe; Barlos, Kostas K; Gatos, Dimitrios; Adermann, Knut; Deraison, Celine; Barlos, Kleomenis

2010-01-01

Proteinase inhibitors are of high pharmaceutical interest and are drug candidates for a variety of indications. Specific kallikrein inhibitors are important for their antitumor activity and their potential application to the treatment of skin diseases. In this study we describe the synthesis of domain 6 of the kallikrein inhibitor Lympho-Epithilial Kazal-Type Inhibitor (LEKTI) by the fragment condensation method and site-directed cystine bridge formation. To obtain the linear LEKTI precursor, the condensation was best performed in solution, coupling the protected fragment 1-22 to 23-68. This method yielded LEKTI domain 6 of high purity and equipotent to the recombinantly produced peptide. (c) 2010 Wiley Periodicals, Inc.

Trace analysis of high-purity graphite by LA-ICP-MS.

PubMed

Pickhardt, C; Becker, J S

2001-07-01

Laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been established as a very efficient and sensitive technique for the direct analysis of solids. In this work the capability of LA-ICP-MS was investigated for determination of trace elements in high-purity graphite. Synthetic laboratory standards with a graphite matrix were prepared for the purpose of quantifying the analytical results. Doped trace elements, concentration 0.5 microg g(-1), in a laboratory standard were determined with an accuracy of 1% to +/- 7% and a relative standard deviation (RSD) of 2-13%. Solution-based calibration was also used for quantitative analysis of high-purity graphite. It was found that such calibration led to analytical results for trace-element determination in graphite with accuracy similar to that obtained by use of synthetic laboratory standards for quantification of analytical results. Results from quantitative determination of trace impurities in a real reactor-graphite sample, using both quantification approaches, were in good agreement. Detection limits for all elements of interest were determined in the low ng g(-1) concentration range. Improvement of detection limits by a factor of 10 was achieved for analyses of high-purity graphite with LA-ICP-MS under wet plasma conditions, because the lower background signal and increased element sensitivity.

Simple LED spectrophotometer for analysis of color information.

PubMed

Kim, Ji-Sun; Kim, A-Hee; Oh, Han-Byeol; Goh, Bong-Jun; Lee, Eun-Suk; Kim, Jun-Sik; Jung, Gu-In; Baek, Jin-Young; Jun, Jae-Hoon

2015-01-01

A spectrophotometer is the basic measuring equipment essential to most research activity fields requiring samples to be measured, such as physics, biotechnology and food engineering. This paper proposes a system that is able to detect sample concentration and color information by using LED and color sensor. Purity and wavelength information can be detected by CIE diagram, and the concentration can be estimated with purity information. This method is more economical and efficient than existing spectrophotometry, and can also be used by ordinary persons. This contribution is applicable to a number of fields because it can be used as a colorimeter to detect the wavelength and purity of samples.

A combined simple bubbling method with high performance liquid chromatography purification strategy, higher radiochemical yield and purity and faster preparation of carbon-11-raclopride.

PubMed

Huang, Huacheng; Ning, Yanli; Zhang, Bucheng; Lou, Cen

2015-01-01

Carbon-11-raclopride (¹¹C-R) is a positron-emitting radiotracer successfully used for the study of cognitive control and widely applied in PET imaging. A simple automated preparation of ¹¹C-R by using the reaction of carbon-(11)-methyl triflate (¹¹C-MeOTF) or ¹¹C-methyl iodide (¹¹C-MeI) with demethylraclopride is described. Specifically we used a simple setup applied an additional "U" reaction vessel for ¹¹C-MeOTf compared with ¹¹C-MeI and assessed the influence of several solvents and of the amount of the percussor for ¹¹C-methylation of demethylraclopride by the bubbling method. The reversal of retention order between product and its precursor has been achieved for ¹¹C-R, enabling collection of the purified ¹¹C-R by using the HPLC column after shorter retention time. By the improved radiosynthesis and purification strategy, ¹¹C-R could be prepared with higher radiochemical yield than that of the previous studies. The yield for ¹¹C-MeOTf was 76% and for ¹¹C-CH3I >26% and with better radiochemical purity (>99% based on both ¹¹C-MeOTf and ¹¹C-MeI) as compared to the previously obtained purity of ¹¹C-R using HPLC method with acetonitrile as a part of mobile phase. Furthermore, by using ethanol as the organic modifier, residual solvent analysis prior to human injection could be avoided and ¹¹C-R could be injected directly following simple dilution and sterile filtration. Improved radiosynthesis and HPLC purification in combination with ethanol containing eluent, extremely shortened the time for preparation of ¹¹C-R, gave a higher radiochemical yield and purity for ¹¹C-R and can be used for multiple and faster synthesis of ¹¹C-R and probably for other ¹¹C-labeled radiopharmaceuticals.

Engineering triangular carbon quantum dots with unprecedented narrow bandwidth emission for multicolored LEDs.

PubMed

Yuan, Fanglong; Yuan, Ting; Sui, Laizhi; Wang, Zhibin; Xi, Zifan; Li, Yunchao; Li, Xiaohong; Fan, Louzhen; Tan, Zhan'ao; Chen, Anmin; Jin, Mingxing; Yang, Shihe

2018-06-08

Carbon quantum dots (CQDs) have emerged as promising materials for optoelectronic applications on account of carbon's intrinsic merits of high stability, low cost, and environment-friendliness. However, the CQDs usually give broad emission with full width at half maximum exceeding 80 nm, which fundamentally limit their display applications. Here we demonstrate multicolored narrow bandwidth emission (full width at half maximum of 30 nm) from triangular CQDs with a quantum yield up to 54-72%. Detailed structural and optical characterizations together with theoretical calculations reveal that the molecular purity and crystalline perfection of the triangular CQDs are key to the high color-purity. Moreover, multicolored light-emitting diodes based on these CQDs display good stability, high color-purity, and high-performance with maximum luminance of 1882-4762 cd m -2 and current efficiency of 1.22-5.11 cd A -1 . This work will set the stage for developing next-generation high-performance CQDs-based light-emitting diodes.

Effective Method of Purification of Betulin from Birch Bark: The Importance of Its Purity for Scientific and Medicinal Use

PubMed Central

Šiman, Pavel; Filipová, Alžběta; Tichá, Alena; Niang, Mohamed; Bezrouk, Aleš; Havelek, Radim

2016-01-01

A new and relatively simple method for purification of betulin from birch bark extract was developed in this study. Its five purification steps are based on the differential solubility of extract components in various solvents and their crystallization and/or precipitation, on their affinity for Ca(OH)2 in ethanol, and on the affinity of some impurities for silica gel in chloroform. In addition, all used solvents can be simply recycled. Betulin of more than 99% purity can be prepared by this method with minimal costs. Various observations including crystallization of betulin, changes in crystals during heating, and attempt of localization of betulin in outer birch bark are also described in this work. The original extract, fraction without betulinic acid and lupeol, amorphous fraction of pure betulin, final crystalline fraction of pure betulin and commercial betulin as a standard were employed to determine the antiproliferative/cytotoxic effect. We used WST-1 tetrazolium-based assays with triple negative breast cancer cell line BT-549. The decrease in cell survival showed clear relationship with the purity of the samples, being most pronounced using our final product of pure crystalline betulin. WST-1 proliferation/cytotoxicity test using triple negative breast cancer cell line BT-549 clearly showed the importance of purity of betulin for biological experiments and, apparently, for its medicinal use. PMID:27152419

Metrological approaches to organic chemical purity: primary reference materials for vitamin D metabolites.

PubMed

Nelson, Michael A; Bedner, Mary; Lang, Brian E; Toman, Blaza; Lippa, Katrice A

2015-11-01

Given the critical role of pure, organic compound primary reference standards used to characterize and certify chemical Certified Reference Materials (CRMs), it is essential that associated mass purity assessments be fit-for-purpose, represented by an appropriate uncertainty interval, and metrologically sound. The mass fraction purities (% g/g) of 25-hydroxyvitamin D (25(OH)D) reference standards used to produce and certify values for clinical vitamin D metabolite CRMs were investigated by multiple orthogonal quantitative measurement techniques. Quantitative (1)H-nuclear magnetic resonance spectroscopy (qNMR) was performed to establish traceability of these materials to the International System of Units (SI) and to directly assess the principal analyte species. The 25(OH)D standards contained volatile and water impurities, as well as structurally-related impurities that are difficult to observe by chromatographic methods or to distinguish from the principal 25(OH)D species by one-dimensional NMR. These impurities have the potential to introduce significant biases to purity investigations in which a limited number of measurands are quantified. Combining complementary information from multiple analytical methods, using both direct and indirect measurement techniques, enabled mitigation of these biases. Purities of 25(OH)D reference standards and associated uncertainties were determined using frequentist and Bayesian statistical models to combine data acquired via qNMR, liquid chromatography with UV absorbance and atmospheric pressure-chemical ionization mass spectrometric detection (LC-UV, LC-ACPI-MS), thermogravimetric analysis (TGA), and Karl Fischer (KF) titration.

Isolation and purification of food-grade C-phycocyanin from Arthrospira platensis and its determination in confectionery by HPLC with diode array detection.

PubMed

Kissoudi, Maria; Sarakatsianos, Ioannis; Samanidou, Victoria

2018-02-01

C-Phycocyanin is the major phycobiliprotein in Arthrospira platensis, also known as Spirulina, which is a cyanobacterium used as a dietary supplement because of its powerful effects on body and brain. C-phycocyanin is a blue-colored accessory photosynthetic pigment with multiple applications in food industry as natural dye or additive, and in pharmaceuticals. This study presents a simple protocol for the extraction and purification of food-grade C-phycocyanin from Arthrospira platensis. The cell lysis of cyanobacterium was performed by sonication combined with repeated freezing and thawing cycles. The purification of the crude extract of C-phycocyanin was carried out by ammonium sulfate precipitation followed by ion exchange chromatography resulting in 2.5 purity. The purity of phycocyanobilin chromophore has been tested by UV-visible spectrophotometry by monitoring the absorption after each stage of purification. A high-performance liquid chromatography method has been developed and validated for the determination of food-grade C-phycocyanin. Intra- and interday precision values less than 5.6% and recovery greater than 91.2% indicated high precision and accuracy of the method for analysis of C-phycocyanin. The method has been applied to commercial confectionery of blue color and to the purified protein obtained in the first stage of the study. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Generation of uniformly oriented in-plane magnetization with near-unity purity in 4π microscopy.

PubMed

Wang, Sicong; Cao, Yaoyu; Li, Xiangping

2017-12-01

In this Letter, we numerically demonstrate the all-optical generation of uniformly oriented in-plane magnetization with near-unity purity (more than 99%) under a 4π microscopic configuration. This is achieved through focusing two counter-propagating vector beams consisting of coherently configured linear and radial components. Based on the Debye diffraction theory, constructive and destructive interferences of the focal field components can be tailored under the 4π configuration to generate high-purity uniformly polarized transverse and longitudinal electric-field components in the center of the focal region. Consequently, near-unity purity in-plane magnetization with a uniform orientation within the focal volume defined by the full width at half-maximum can be created through the inverse Faraday effect. In addition, it reveals that the purity of the in-plane magnetization is robust against the numerical aperture of the focal lens. This result expands the flexibility of magnetization manipulations through light and holds great potential in all-optical magnetic recording and spintronics.

Fractionation and physicochemical characterization of lignin from waste jute bags: Effect of process parameters on yield and thermal degradation.

PubMed

Ahuja, Dheeraj; Kaushik, Anupama; Chauhan, Ghanshyam S

2017-04-01

In this work lignin was extracted from waste jute bags using soda cooking method and effect of varying alkali concentration and pH on yield, purity, structure and thermal degradation of lignin were studied. The Lignin yield, chemical composition and purity were assessed using TAPPI method and UV-vis spectroscopy. Yield and purity of lignin ranged from 27 to 58% and 50-94%, respectively for all the samples and was maximum for 8% alkali concentration and at pH 2 giving higher thermal stability. Chemical structure, thermal stability and elementary analysis of lignin were studied using FTIR, H NMR, thermo gravimetric analysis (TGA) and Elemental analyzer. FTIR and H NMR results showed that core structure of lignin starts breaking beyond 10% alkali concentration. S/G ratio shows the dominance of Syringyl unit over guaiacyl unit. Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of stoichiometry, purity, etching and distilling on resistance of MgB 2 pellets and wire segments

NASA Astrophysics Data System (ADS)

Ribeiro, R. A.; Bud'ko, S. L.; Petrovic, C.; Canfield, P. C.

2002-11-01

We present a study of the effects of non-stoichiometry, boron purity, wire diameter and post-synthesis treatment (etching and Mg distilling) on the temperature dependent resistance and resistivity of sintered MgB 2 pellets and wire segments. Whereas the residual resistivity ratio (RRR) varies between RRR≈4 to RRR⩾20 for different boron purity, it is only moderately affected by non-stoichiometry (from 20% Mg deficiency to 20% Mg excess) and is apparently independent of wire diameter and presence of Mg metal traces on the wire surface. The obtained set of data indicates that RRR values in excess of 20 and residual resistivities as low as ρ 0≈0.4 μΩ cm are intrinsic material properties of high purity MgB 2.

A Structural Model of the Retail Market for Illicit Drugs.

PubMed

Galenianos, Manolis; Gavazza, Alessandro

2017-03-01

We estimate a model of illicit drugs markets using data on purchases of crack cocaine. Buyers are searching for high-quality drugs, but they determine drugs' quality (i.e., their purity) only after consuming them. Hence, sellers can rip off first-time buyers or can offer higher-quality drugs to induce buyers to purchase from them again. In equilibrium, a distribution of qualities persists. The estimated model implies that if drugs were legalized, in which case purity could be regulated and hence observable, the average purity of drugs would increase by approximately 20 percent and the dispersion would decrease by approximately 80 percent. Moreover, increasing penalties may raise the purity and affordability of the drugs traded by increasing sellers’ relative profitability of targeting loyal buyers versus first-time buyers.

An Efficient Method for the Isolation of Highly Purified RNA from Seeds for Use in Quantitative Transcriptome Analysis.

PubMed

Kanai, Masatake; Mano, Shoji; Nishimura, Mikio

2017-01-11

Plant seeds accumulate large amounts of storage reserves comprising biodegradable organic matter. Humans rely on seed storage reserves for food and as industrial materials. Gene expression profiles are powerful tools for investigating metabolic regulation in plant cells. Therefore, detailed, accurate gene expression profiles during seed development are required for crop breeding. Acquiring highly purified RNA is essential for producing these profiles. Efficient methods are needed to isolate highly purified RNA from seeds. Here, we describe a method for isolating RNA from seeds containing large amounts of oils, proteins, and polyphenols, which have inhibitory effects on high-purity RNA isolation. Our method enables highly purified RNA to be obtained from seeds without the use of phenol, chloroform, or additional processes for RNA purification. This method is applicable to Arabidopsis, rapeseed, and soybean seeds. Our method will be useful for monitoring the expression patterns of low level transcripts in developing and mature seeds.

Expression and purification of recombinant apolipoprotein A-I Zaragoza (L144R) and formation of reconstituted HDL particles.

PubMed

Fiddyment, Sarah; Barceló-Batllori, Sílvia; Pocoví, Miguel; García-Otín, Angel-Luis

2011-11-01

Apolipoprotein A-I Zaragoza (L144R) (apo A-I Z), has been associated with severe hypoalphalipoproteinemia and an enhanced effect of high density lipoprotein (HDL) reverse cholesterol transport. In order to perform further studies with this protein we have optimized an expression and purification method of recombinant wild-type apo A-I and apo A-I Z and produced mimetic HDL particles with each protein. An pET-45 expression system was used to produce N-terminal His-tagged apo A-I, wild-type or mutant, in Escherichia coli BL21 (DE3) which was subsequently purified by affinity chromatography in non-denaturing conditions. HDL particles were generated via a modified sodium cholate method. Expression and purification of both proteins was verified by SDS-PAGE, MALDI-TOF MS and immunochemical procedures. Yield was 30mg of purified protein (94% purity) per liter of culture. The reconstituted HDL particles checked via non-denaturing PAGE showed high homogeneity in their size when reconstituted both with wild-type apo A-I and apo A-I Z. An optimized system for the expression and purification of wild-type apo A-I and apo A-I Z with high yield and purity grade has been achieved, in addition to their use in reconstituted HDL particles, as a basis for further studies. Copyright © 2011 Elsevier Inc. All rights reserved.

Direct measurement of 235U in spent fuel rods with Gamma-ray mirrors

NASA Astrophysics Data System (ADS)

Ruz, J.; Brejnholt, N. F.; Alameda, J. B.; Decker, T. A.; Descalle, M. A.; Fernandez-Perea, M.; Hill, R. M.; Kisner, R. A.; Melin, A. M.; Patton, B. W.; Soufli, R.; Ziock, K.; Pivovaroff, M. J.

2015-03-01

Direct measurement of plutonium and uranium X-rays and gamma-rays is a highly desirable non-destructive analysis method for the use in reprocessing fuel environments. The high background and intense radiation from spent fuel make direct measurements difficult to implement since the relatively low activity of uranium and plutonium is masked by the high activity from fission products. To overcome this problem, we make use of a grazing incidence optic to selectively reflect Kα and Kβ fluorescence of Special Nuclear Materials (SNM) into a high-purity position-sensitive germanium detector and obtain their relative ratios.

Removal and deposition efficiencies of the long-lived 222Rn daughters during etching of germanium surfaces

NASA Astrophysics Data System (ADS)

Zuzel, G.; Wójcik, M.; Majorovits, B.; Lampert, M. O.; Wendling, P.

2012-06-01

Removal and deposition efficiencies of the long-lived 222Rn daughters during etching from and onto surfaces of standard and high purity germanium were investigated. The standard etching procedure of Canberra-France used during production of high purity n-type germanium diodes was applied to germanium discs, which have been exposed earlier to a strong radon source for deposition of its progenies. An uncontaminated sample was etched in a solution containing 210Pb, 210Bi and 210Po. All isotopes were measured before and after etching with appropriate detectors. In contrast to copper and stainless steel, they were removed from germanium very efficiently. However, the reverse process was also observed. Considerable amounts of radioactive lead, bismuth and polonium isotopes present initially in the artificially polluted etchant were transferred to the clean high purity surface during processing of the sample.

Fabrication of novel cryomill for synthesis of high purity metallic nanoparticles

NASA Astrophysics Data System (ADS)

Kumar, Nirmal; Biswas, Krishanu

2015-08-01

The successful preparation of free standing metal nanoparticles with high purity in bulk quantity is the pre-requisite for any potential application. This is possible by using ball milling at cryogenic temperature. However, the most of ball mills available in the market do not allow preparing high purity metal nanoparticles by this route. In addition, it is not possible to carry out in situ measurements of process parameters as well as diagnostic of the process. In the present investigation, we present a detailed study on the fabrication of a cryomill, which is capable of avoiding contaminations in the product. It also provides in situ measurements and diagnostic of the low temperature milling process. Online monitoring of the milling temperature and observation of ball motion are the important aspects in the newly designed mill. The nanoparticles prepared using this fabricated mill have been found to be free standing and also free from contaminations.

Dielectric and transport properties of CaTiO3

NASA Astrophysics Data System (ADS)

Bhadala, Falguni; Suthar, Lokesh; Roy, M.; Jha, Vikash Kumar

2018-05-01

The ceramic sample of CaTiO3 (CTO) has been prepared by standard high temperature solid state reaction method using high purity oxides. The formation of the compound as well as structural analysis has been carried out by X-ray diffraction method. The dielectric constant and dielectric loss as a function of frequency (20kHz-10MHz) and temperature (RT-490K) have been measured. The dc conductivity has been measured and activation energy was calculated using the Arrhenius relation. The Enthalpy change (ΔH), Specific heat and Weight-loss of the compound have been measured using DTA/TGA techniques. The results are discussed in detail.

Clinical-Scale Cell-Surface-Marker Independent Acoustic Microfluidic Enrichment of Tumor Cells from Blood.

PubMed

Magnusson, Cecilia; Augustsson, Per; Lenshof, Andreas; Ceder, Yvonne; Laurell, Thomas; Lilja, Hans

2017-11-21

Enumeration of circulating tumor cells (CTCs) predicts overall survival and treatment response in metastatic cancer, but as many commercialized assays isolate CTCs positive for epithelial cell markers alone, CTCs with little or no epithelial cell adhesion molecule (EpCAM) expression stay undetected. Therefore, CTC enrichment and isolation by label-free methods based on biophysical rather than biochemical properties could provide a more representative spectrum of CTCs. Here, we report on a clinical-scale automated acoustic microfluidic platform processing 5 mL of erythrocyte-depleted paraformaldehyde (PFA)-fixed blood (diluted 1:2) at a flow rate of 75 μL/min, recovering 43/50 (86 ± 2.3%) breast cancer cell line cells (MCF7), with 0.11% cancer cell purity and 162-fold enrichment in close to 2 h based on intrinsic biophysical cell properties. Adjustments of the voltage settings aimed at higher cancer cell purity in the central outlet provided 0.72% cancer cell purity and 1445-fold enrichment that resulted in 62 ± 8.7% cancer cell recovery. Similar rates of cancer-cell recovery, cancer-cell purity, and fold-enrichment were seen with both prostate cancer (DU145, PC3) and breast cancer (MCF7) cell line cells. We identified eosinophil granulocytes as the predominant white blood cell (WBC) contaminant (85%) in the enriched cancer-cell fraction. Processing of viable cancer cells in erythrocyte-depleted blood provided slightly reduced results as to fixed cells (77% cancer cells in the enriched cancer cell fraction, with 0.2% WBC contamination). We demonstrate feasibility of enriching either PFA-fixed or viable cancer cells with a clinical-scale acoustic microfluidic platform that can be adjusted to meet requirements for either high cancer-cell recovery or higher purity and can process 5 mL blood samples in close to 2 h.

In vitro characterization of high purity factor IX concentrates for the treatment of hemophilia B.

PubMed

Limentani, S A; Gowell, K P; Deitcher, S R

1995-04-01

This study employed sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis and immunoblotting to assess the purity of seven high purity factor IX concentrates: Aimafix (Aima), AlphaNine-SD (Alpha Therapeutic), Factor IX VHP (Biotransfusion), Immunine (Immuno), Mononine (Armour Pharmaceutical), Nanotiv (Kabi Pharmacia), and 9MC (Blood Products Laboratory). The mean specific activity of these products ranged from 68 U factor IX/mg (Aimafix) to 246 U factor IX/mg (Mononine). SDS-PAGE analysis showed that the highest purity product, Mononine, had a single contaminating band under non-reducing conditions. Two additional bands were detected when this product was analyzed under reducing conditions. All other products had multiple contaminating bands that were more apparent under reducing than non-reducing conditions. The immunoblot for factor IX showed a dominant factor IX band for all products. In addition, visible light chain of factor IX was detected for AlphaNine-SD, Factor IX VHP, Immunine, Mononine, Nanotiv, and 9MC, suggesting that the factor IX in these products had undergone partial activation to factor IXa. Another contaminating band was visible at 49,500 for all of the products except 9MC. In addition to this band, high molecular weight contaminants were apparent for some products, most notably AlphaNine-SD. The identity of these bands is unknown. Immunoblotting failed to demonstrate factor VII as a contaminant of any of the high purity products, although factor VIIa could be detected in some lots of Immunine, Nanotiv, and 9MC by a clot-based assay. Factor X contaminated Aimafix, AlphaNine-SD, Factor IX VHP, Immunine, Nanotiv, and 9MC, but activation products of factor X were not detected.(ABSTRACT TRUNCATED AT 250 WORDS)

Comparison of the microstructure, deformation and crack initiation behavior of austenitic stainless steel irradiated in-reactor or with protons

NASA Astrophysics Data System (ADS)

Stephenson, Kale J.; Was, Gary S.

2015-01-01

The objective of this study was to compare the microstructures, microchemistry, hardening, susceptibility to IASCC initiation, and deformation behavior resulting from proton or reactor irradiation. Two commercial purity and six high purity austenitic stainless steels with various solute element additions were compared. Samples of each alloy were irradiated in the BOR-60 fast reactor at 320 °C to doses between approximately 4 and 12 dpa or by a 3.2 MeV proton beam at 360 °C to a dose of 5.5 dpa. Irradiated microstructures consisted mainly of dislocation loops, which were similar in size but lower in density after proton irradiation. Both irradiation types resulted in the formation of Ni-Si rich precipitates in a high purity alloy with added Si, but several other high purity neutron irradiated alloys showed precipitation that was not observed after proton irradiation, likely due to their higher irradiation dose. Low densities of small voids were observed in several high purity proton irradiated alloys, and even lower densities in neutron irradiated alloys, implying void nucleation was in process. Elemental segregation at grain boundaries was very similar after each irradiation type. Constant extension rate tensile experiments on the alloys in simulated light water reactor environments showed excellent agreement in terms of the relative amounts of intergranular cracking, and an analysis of localized deformation after straining showed a similar response of cracking to surface step height after both irradiation types. Overall, excellent agreement was observed after proton and reactor irradiation, providing additional evidence that proton irradiation is a useful tool for accelerated testing of irradiation effects in austenitic stainless steel.

Wet powder processing of sol-gel derived mesoporous silica-hydroxyapatite hybrid powders.

PubMed

Andersson, Jenny; Johannessen, Espen; Areva, Sami; Järn, Mikael; Lindén, Mika

2006-08-01

This paper describes a method by which a porous silica coating layer can be obtained on different apatite particles through a simple sol-gel synthesis route. Sol-gel derived powders of hydroxyapatite (HAP) and beta tricalciumphosphate (beta-TCP) were coated with a mesoporous silica using C16TAB (hexadecyltrimethylammonium bromide) as a template in order to induce mesophase formation. Further calcination of the material removes the template from the mesophase and leaves a highly ordered hexagonal arranged mesoporous silica structure with a core of HAP/beta-TCP. The phase purity of the SiO2/apatite composites has been thoroughly investigated by the means of FT-IR, XRD, and solid state 31P MAS NMR. The phase purity of these materials is shown to be dependent on the solubility properties of the used apatites. The hybrid materials are suitable as a multifunctional biomaterial where osteoconductive properties can be combined with drug delivery.

Control of phosphorothioate stereochemistry substantially increases the efficacy of antisense oligonucleotides.

PubMed

Iwamoto, Naoki; Butler, David C D; Svrzikapa, Nenad; Mohapatra, Susovan; Zlatev, Ivan; Sah, Dinah W Y; Meena; Standley, Stephany M; Lu, Genliang; Apponi, Luciano H; Frank-Kamenetsky, Maria; Zhang, Jason Jingxin; Vargeese, Chandra; Verdine, Gregory L

2017-09-01

Whereas stereochemical purity in drugs has become the standard for small molecules, stereoisomeric mixtures containing as many as a half million components persist in antisense oligonucleotide (ASO) therapeutics because it has been feasible neither to separate the individual stereoisomers, nor to synthesize stereochemically pure ASOs. Here we report the development of a scalable synthetic process that yields therapeutic ASOs having high stereochemical and chemical purity. Using this method, we synthesized rationally designed stereopure components of mipomersen, a drug comprising 524,288 stereoisomers. We demonstrate that phosphorothioate (PS) stereochemistry substantially affects the pharmacologic properties of ASOs. We report that Sp-configured PS linkages are stabilized relative to Rp, providing stereochemical protection from pharmacologic inactivation of the drug. Further, we elucidated a triplet stereochemical code in the stereopure ASOs, 3'-SpSpRp, that promotes target RNA cleavage by RNase H1 in vitro and provides a more durable response in mice than stereorandom ASOs.

Isolation and purification of recombinant human plasminogen Kringle 5 by liquid chromatography and ammonium sulfate salting-out.

PubMed

Bian, Liujiao; Ji, Xu; Hu, Wei

2014-07-01

In this work, a novel method was established to isolate and purify Human plasminogen Kringle 5 (HPK5) as a histidine-tagged fusion protein expressed in Escherichia coli BL21 (DE3). This method consisted of sample extraction using a Ni-chelated Sepharose Fast-Flow affinity column, ammonium sulfate salting-out and Sephadex G-75 size-exclusion column in turn. The purity analysis by SDS-PAGE, high-performance size-exclusion and reversed-phase chromatographies showed that the obtained recombinant fusion HPK5 was homogeneous and its purity was higher than 96%; the activity analysis by chorioallantoic membrane model of chicken embryos revealed that the purified recombinant HPK5 exhibited an obvious anti-angiogenic activity under the effective range of 5.0-25.0 µg/mL. Through this procedure, about 19 mg purified recombinant fusion HPK5 can be obtained from 1 L of original fermentation solution. Approximate 32% of the total recombinant fusion HPK5 can be captured and the total yield was approximately 11%. Copyright © 2013 John Wiley & Sons, Ltd.

Nano-sized ZnO powders prepared by co-precipitation method with various pH

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

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro,

2016-04-19

In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, atmore » 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.« less

Spectrophotometric determination of traces of boron in high purity silicon

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

Parashar, D.C.; Sarkar, A.K.; Singh, N.

1989-07-01

A reddish brown complex is formed between boron and curcumin in concentrated sulfuric acid and glacial acetic acid mixture (1:1). The colored complex is highly selective and stable for about 3 hours and has the maximum absorbance at 545 nm. The sensitivity of the method is extremely high and the detection limit is 3 parts per billion based on 0.004 absorbance value. The interference of some of the important cations and anions relevant to silicon were studied and it is found that 100 fold excess of most of these cations and anions do not interfere in the determination of boron.more » The method is successfully employed for the determination of boron in silicon used in semiconductor devices. The results have been verified by standard addition method.« less

Determination of nitrogen monoxide in high purity nitrogen gas with an atmospheric pressure ionization mass spectrometer

NASA Technical Reports Server (NTRS)

Kato, K.

1985-01-01

An atmospheric pressure ionization mass spectrometric (API-MS) method was studied for the determination of residual NO in high purity N2 gas. The API-MS is very sensitive to NO, but the presence of O2 interferes with the NO measurement. Nitrogen gas in cylinders as sample gas was mixed with NO standard gas and/or O2 standard gas, and then introduced into the API-MS. The calibration curves of NO and O2 has linearity in the region of 0 - 2 ppm, but the slopes changed with every cylinder. The effect of O2 on NO+ peak was additive and proportional to O2 concentration in the range of 0 - 0.5 ppm. The increase in NO+ intensity due to O2 was (0.07 - 0.13)%/O2, 1 ppm. Determination of NO and O2 was carried out by the standard addition method to eliminate the influence of variation of slopes. The interference due to O2 was estimated from the product of the O2 concentration and the ratio of slope A to Slope B. Slope A is the change in the NO+ intensity with the O2 concentration. Slope B is the intensity with O2 concentration.

Application of optically-induced-dielectrophoresis in microfluidic system for purification of circulating tumour cells for gene expression analysis- Cancer cell line model

NASA Astrophysics Data System (ADS)

Chiu, Tzu-Keng; Chou, Wen-Pin; Huang, Song-Bin; Wang, Hung-Ming; Lin, Yung-Chang; Hsieh, Chia-Hsun; Wu, Min-Hsien

2016-09-01

Circulating tumour cells (CTCs) in a blood circulation system are associated with cancer metastasis. The analysis of the drug-resistance gene expression of cancer patients’ CTCs holds promise for selecting a more effective therapeutic regimen for an individual patient. However, the current CTC isolation schemes might not be able to harvest CTCs with sufficiently high purity for such applications. To address this issue, this study proposed to integrate the techniques of optically induced dielectrophoretic (ODEP) force-based cell manipulation and fluorescent microscopic imaging in a microfluidic system to further purify CTCs after the conventional CTC isolation methods. In this study, the microfluidic system was developed, and its optimal operating conditions and performance for CTC isolation were evaluated. The results revealed that the presented system was able to isolate CTCs with cell purity as high as 100%, beyond what is possible using the previously existing techniques. In the analysis of CTC gene expression, therefore, this method could exclude the interference of leukocytes in a cell sample and accordingly contribute to higher analytical sensitivity, as demonstrated in this study. Overall, this study has presented an ODEP-based microfluidic system capable of simply and effectively isolating a specific cell species from a cell mixture.

Application of optically-induced-dielectrophoresis in microfluidic system for purification of circulating tumour cells for gene expression analysis- Cancer cell line model.

PubMed

Chiu, Tzu-Keng; Chou, Wen-Pin; Huang, Song-Bin; Wang, Hung-Ming; Lin, Yung-Chang; Hsieh, Chia-Hsun; Wu, Min-Hsien

2016-09-09

Circulating tumour cells (CTCs) in a blood circulation system are associated with cancer metastasis. The analysis of the drug-resistance gene expression of cancer patients' CTCs holds promise for selecting a more effective therapeutic regimen for an individual patient. However, the current CTC isolation schemes might not be able to harvest CTCs with sufficiently high purity for such applications. To address this issue, this study proposed to integrate the techniques of optically induced dielectrophoretic (ODEP) force-based cell manipulation and fluorescent microscopic imaging in a microfluidic system to further purify CTCs after the conventional CTC isolation methods. In this study, the microfluidic system was developed, and its optimal operating conditions and performance for CTC isolation were evaluated. The results revealed that the presented system was able to isolate CTCs with cell purity as high as 100%, beyond what is possible using the previously existing techniques. In the analysis of CTC gene expression, therefore, this method could exclude the interference of leukocytes in a cell sample and accordingly contribute to higher analytical sensitivity, as demonstrated in this study. Overall, this study has presented an ODEP-based microfluidic system capable of simply and effectively isolating a specific cell species from a cell mixture.

Application of optically-induced-dielectrophoresis in microfluidic system for purification of circulating tumour cells for gene expression analysis- Cancer cell line model

PubMed Central

Chiu, Tzu-Keng; Chou, Wen-Pin; Huang, Song-Bin; Wang, Hung-Ming; Lin, Yung-Chang; Hsieh, Chia-Hsun; Wu, Min-Hsien

2016-01-01

Circulating tumour cells (CTCs) in a blood circulation system are associated with cancer metastasis. The analysis of the drug-resistance gene expression of cancer patients’ CTCs holds promise for selecting a more effective therapeutic regimen for an individual patient. However, the current CTC isolation schemes might not be able to harvest CTCs with sufficiently high purity for such applications. To address this issue, this study proposed to integrate the techniques of optically induced dielectrophoretic (ODEP) force-based cell manipulation and fluorescent microscopic imaging in a microfluidic system to further purify CTCs after the conventional CTC isolation methods. In this study, the microfluidic system was developed, and its optimal operating conditions and performance for CTC isolation were evaluated. The results revealed that the presented system was able to isolate CTCs with cell purity as high as 100%, beyond what is possible using the previously existing techniques. In the analysis of CTC gene expression, therefore, this method could exclude the interference of leukocytes in a cell sample and accordingly contribute to higher analytical sensitivity, as demonstrated in this study. Overall, this study has presented an ODEP-based microfluidic system capable of simply and effectively isolating a specific cell species from a cell mixture. PMID:27609546

Optimizing purification process of MIM-I-BAR domain by introducing atomic force microscope and dynamics simulations.

PubMed

Zhang, Yue; Lou, Zhichao; Lin, Xubo; Wang, Qiwei; Cao, Meng; Gu, Ning

2017-09-01

MIM (missing in metastasis) is a member of I-BAR (inverse BAR) domain protein family, which functions as a putative metastasis suppressor. However, methods of gaining high purity MIM-I-BAR protein are barely reported. Here, by optimizing the purification process including changing the conditions of cell lysate and protein elution, we successfully purified MIM protein. The purity of the obtained protein was up to ∼90%. High-resolution atomic force microscope (AFM) provides more visual images, ensuring that we can observe the microenvironment around the target protein, as well as the conformations of the purification products following each purification process. MIM protein with two different sizes were observed on mica surface with AFM. Combining with molecular dynamics simulations, these molecules were revealed as MIM monomer and dimer. Furthermore, our study attaches importance to the usage of imidazole with suitable concentrations during the affinity chromatography process, as well as the removal of excessive imidazole after the affinity chromatography process. All these results indicate that the method described here was successful in purifying MIM protein and maintaining their natural properties, and is supposed to be used to purify other proteins with low solubility. Copyright © 2017. Published by Elsevier B.V.

Rapid Synthesis of Thin and Long Mo17O47 Nanowire-Arrays in an Oxygen Deficient Flame

PubMed Central

Allen, Patrick; Cai, Lili; Zhou, Lite; Zhao, Chenqi; Rao, Pratap M.

2016-01-01

Mo17O47 nanowire-arrays are promising active materials and electrically-conductive supports for batteries and other devices. While high surface area resulting from long, thin, densely packed nanowires generally leads to improved performance in a wide variety of applications, the Mo17O47 nanowire-arrays synthesized previously by electrically-heated chemical vapor deposition under vacuum conditions were relatively thick and short. Here, we demonstrate a method to grow significantly thinner and longer, densely packed, high-purity Mo17O47 nanowire-arrays with diameters of 20–60 nm and lengths of 4–6 μm on metal foil substrates using rapid atmospheric flame vapor deposition without any chamber or walls. The atmospheric pressure and 1000 °C evaporation temperature resulted in smaller diameters, longer lengths and order-of-magnitude faster growth rate than previously demonstrated. As explained by kinetic and thermodynamic calculations, the selective synthesis of high-purity Mo17O47 nanowires is achieved due to low oxygen partial pressure in the flame products as a result of the high ratio of fuel to oxidizer supplied to the flame, which enables the correct ratio of MoO2 and MoO3 vapor concentrations for the growth of Mo17O47. This flame synthesis method is therefore a promising route for the growth of composition-controlled one-dimensional metal oxide nanomaterials for many applications. PMID:27271194

Non-iridescent Transmissive Structural Color Filter Featuring Highly Efficient Transmission and High Excitation Purity

PubMed Central

Shrestha, Vivek Raj; Lee, Sang-Shin; Kim, Eun-Soo; Choi, Duk-Yong

2014-01-01

Nanostructure based color filtering has been considered an attractive replacement for current colorant pigmentation in the display technologies, in view of its increased efficiencies, ease of fabrication and eco-friendliness. For such structural filtering, iridescence relevant to its angular dependency, which poses a detrimental barrier to the practical development of high performance display and sensing devices, should be mitigated. We report on a non-iridescent transmissive structural color filter, fabricated in a large area of 76.2 × 25.4 mm2, taking advantage of a stack of three etalon resonators in dielectric films based on a high-index cavity in amorphous silicon. The proposed filter features a high transmission above 80%, a high excitation purity of 0.93 and non-iridescence over a range of 160°, exhibiting no significant change in the center wavelength, dominant wavelength and excitation purity, which implies no change in hue and saturation of the output color. The proposed structure may find its potential applications to large-scale display and imaging sensor systems. PMID:24815530

Tunable and high-purity room temperature single-photon emission from atomic defects in hexagonal boron nitride

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

Grosso, Gabriele; Moon, Hyowon; Lienhard, Benjamin

Two-dimensional van der Waals materials have emerged as promising platforms for solid-state quantum information processing devices with unusual potential for heterogeneous assembly. Recently, bright and photostable single photon emitters were reported from atomic defects in layered hexagonal boron nitride (hBN), but controlling inhomogeneous spectral distribution and reducing multi-photon emission presented open challenges. Here, we demonstrate that strain control allows spectral tunability of hBN single photon emitters over 6 meV, and material processing sharply improves the single photon purity. We observe high single photon count rates exceeding 7 × 10 6 counts per second at saturation, after correcting for uncorrelated photonmore » background. Furthermore, these emitters are stable to material transfer to other substrates. High-purity and photostable single photon emission at room temperature, together with spectral tunability and transferability, opens the door to scalable integration of high-quality quantum emitters in photonic quantum technologies.« less

Process for producing high purity isoolefins and dimers thereof by dissociation of ethers

DOEpatents

Smith, L.A. Jr.; Jones, E.M. Jr.; Hearn, D.

1984-05-08

Alkyl tertiary butyl ether or alkyl tertiary amyl ether is dissociated by vapor phase contact with a cation acidic exchange resin at temperatures in the range of 150 to 250 F at LHSV of 0.1 to 20 to produce a stream consisting of unreacted ether, isobutene or isoamylene and an alcohol corresponding to the alkyl radical. After the alcohol is removed, the ether/isoolefin stream may be fractionated to obtain a high purity isoolefin (99+%) or the ether/isoolefin stream can be contacted in liquid phase with a cation acidic exchange resin to selectively dimerize the isoolefin in a highly exothermic reaction, followed by fractionation of the dimerization product to produce high purity diisoolefin (97+%). In the case where the alkyl is C[sub 3] to C[sub 6] and the corresponding alcohol is produced on dissociation of the ether, combined dissociation-distillation may be carried out such that isoolefin is the overhead product and alcohol the bottom. 2 figs.

Process for producing high purity isoolefins and dimers thereof by dissociation of ethers

DOEpatents

Smith, Jr., Lawrence A.; Jones, Jr., Edward M.; Hearn, Dennis

1984-01-01

Alkyl tertiary butyl ether or alkyl tertiary amyl ether is dissociated by vapor phase contact with a cation acidic exchange resin at temperatures in the range of 150.degree. to 250.degree. F. at LHSV of 0.1 to 20 to produce a stream consisting of unreacted ether, isobutene or isoamylene and an alcohol corresponding to the alkyl radical. After the alcohol is removed, the ether/isoolefin stream may be fractionated to obtain a high purity isoolefin (99+%) or the ether/isoolefin stream can be contacted in liquid phase with a cation acidic exchange resin to selectively dimerize the isoolefin in a highly exothermic reaction, followed by fractionation of the dimerization product to produce high purity diisoolefin (97+%). In the case where the alkyl is C.sub.3 to C.sub.6 and the corresponding alcohol is produced on dissociation of the ether, combined dissociation-distillation may be carried out such that isoolefin is the overhead product and alcohol the bottom.

Tunable and high-purity room temperature single-photon emission from atomic defects in hexagonal boron nitride

DOE PAGES

Grosso, Gabriele; Moon, Hyowon; Lienhard, Benjamin; ...

2017-09-26

Two-dimensional van der Waals materials have emerged as promising platforms for solid-state quantum information processing devices with unusual potential for heterogeneous assembly. Recently, bright and photostable single photon emitters were reported from atomic defects in layered hexagonal boron nitride (hBN), but controlling inhomogeneous spectral distribution and reducing multi-photon emission presented open challenges. Here, we demonstrate that strain control allows spectral tunability of hBN single photon emitters over 6 meV, and material processing sharply improves the single photon purity. We observe high single photon count rates exceeding 7 × 10 6 counts per second at saturation, after correcting for uncorrelated photonmore » background. Furthermore, these emitters are stable to material transfer to other substrates. High-purity and photostable single photon emission at room temperature, together with spectral tunability and transferability, opens the door to scalable integration of high-quality quantum emitters in photonic quantum technologies.« less

The use of Whatman-31ET paper for an efficient method for radiochemical purity test of 131I-Hippuran

NASA Astrophysics Data System (ADS)

Rezka Putra, Amal; Maskur; Sugiharto, Yono; Chairuman; Hardi Gunawan, Adang; Awaludin, Rohadi

2018-01-01

Current chromatography methods used for radiochemical purity test of 131I-Hippuran is time consuming. Therefore, in this study we explored several static and mobile phases in order to have a chromatography method which is accurate and efficient or less time consuming. In this study, stationary phases (Whatman-1, 31ET, and 3MM papers) and several mobile phases were explored to separate 131I-Hippuran from its impurity (131I iodide ion). The results of this study showed that the most efficient chromatography system for measurement of radiochemical purity of 131I-Hippuran was by using Whatman-31ET paper and n-butanol: acetic acid: water (4:1:1) as a static phase and mobile phase respectively. Developing time for this method was of approximately 75.7 ± 2.7 minutes. The result of radiochemical purity (%RCP) of 131I-Hippuran measured with this chromatography system either using Whatman-1 or Whatman-31ET paper strips was 98.7%. The short size of Whatman-31ET paper strip (1 x 8 cm) was found to have shorter developing time compared to that of long size paper. This system showed a good separation of 131I-Hippuran from its impurities and gave %RCP of 98.1% ± 0.04% with developing time approximately 44.3 ± 9.4 minutes. The short size of Whatman-31ET paper strips was found to be more efficient compared to that of Whatman-1 and Whatman-3MM paper strips in term of developing time.

Synthesis, characterization and photocatalysis enhancement of Eu2O3-ZnO mixed oxide nanoparticles

NASA Astrophysics Data System (ADS)

Mohamed, W. S.; Abu-Dief, Ahmed M.

2018-05-01

Pure ZnO nanoparticles (NPs) and mixed Eu2O3 and ZnO NPs with different Eu2O3 ratios (5%, 10%, and 15%) were synthesized by a precipitation method under optimum conditions. The synthesized samples were characterized by means of X-ray diffraction, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy, transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, and UV-vis diffuse reflectance spectroscopy. The as-synthesized ZnO NPs exhibit high phase purity and a highly crystalline wurtzite ZnO structure. The mixed Eu2O3 and ZnO NPs exhibit a Eu2O3 zinc blend phase in addition to the wurtzite phase of pure ZnO, confirming the high purity and good crystallinity of the as-synthesized samples. The high-purity formation of ZnO and Eu2O3 phases was confirmed by FTIR and Raman spectra. Microstructural analysis by SEM and TEM confirmed the sphere-like morphology with different particle sizes (29-40 nm) of the as-synthesized samples. The photocatalytic activities of pure ZnO NPs and mixed Eu2O3 and ZnO NPs for the degradation of methylene blue were evaluated under ultraviolet (UV) irradiation. The results show that Eu2O3 plays an important role in the enhancement of the photocatalytic properties of ZnO NPs. We found that mixed 5% Eu2O3 and ZnO NPs exhibit the highest photocatalytic activity (degradation efficiency of 96.5% after 180 min of UV irradiation) as compared with pure ZnO NPs (degradation efficiency of 80.3% after 180 min of UV irradiation). The increased photocatalytic activity of the optimum mixed Eu2O3 and ZnO NPs is due to the high crystallinity, high surface area with small particle size, and narrow energy gap.

A nonchromatographic process for purification of secretory immunoglobulins from caprine whey.

PubMed

Matlschweiger, Alexander; Himmler, Gottfried; Linhart, Clemens; Harasek, Michael; Hahn, Rainer

2017-05-01

Secretory immunoglobulins are an important antibody class being primarily responsible for immunoprotection of mucosal surfaces. A simple, non-chromatographic purification process for secretory immunoglobulins from caprine whey was developed. In the first process step whey was concentrated 30-40-fold on a 500 kDa membrane, thereby increasing the purity from 3% to 15%. The second step consisted of a fractionated PEG precipitation, in which high molecular weight impurities were removed first and in the second stage the secretory immunoglobulins were precipitated, leaving a majority of the low molecular weight proteins in solution. The re-dissolved secretory immunoglobulin fraction had a purity of 43% which could then be increased to 72% by diafiltration at a volume exchange factor of 10. Further increase of purity was only possible at the expense of very high buffer consumption. If diafiltration was performed directly after ultrafiltration, followed by precipitation, the yield was higher but purity was only 54%. Overall, filtration performance was characterized by high concentration polarization, therefore process conditions were set to low trans-membrane pressure and moderate protein concentration. As such purity and to a lesser extent throughput were the major objectives rather than yield, since whey, as a by-product of the dairy industry, is a cheap raw material of almost unlimited supply. Ultra-/diafiltration performance was described well by correlations using dimensionless numbers. Compared with a theoretical model (Graetz/Leveque solution) the flux was slightly overestimated. © 2017 American Institute of Chemical Engineers Biotechnol. Prog., 33:642-653, 2017. © 2017 American Institute of Chemical Engineers.

Using IR spectroscopy to determine biodiesel conversion

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

Tirla, Cornelia; Dooling, Thomas; Smith, Rachel B.

This project’s aim was to develop a way to use Infrared (IR) Spectroscopy to determine the extent of the conversion of oil to biodiesel produced during a typical transesterification process. The most reliable method of biodiesel analysis is gas chromatography with flame ionization detector (GC-FID) analysis. This analysis is not ideal for the educational or field applications since it is time intensive and requires expensive, specialized equipment. The use of the FT-IR is faster and more affordable. A calibration curve was created by comparing data on the purity of biodiesel samples obtained from the GC-FID analysis to the ratio ofmore » the absorbances at 1197 cm -1 to 1166 cm -1 from the FT-IR spectrum. For field application, a similar method was developed using a portable IR spectrometer, the InfraSpecTM VFA-IR spectrometer. As a result, the data collected gave a good linear fit for % purity of the samples and can be used as a method for monitoring the conversion of different types of oils to biodiesel and determining the purity of biodiesel produced from oil.« less

Using IR spectroscopy to determine biodiesel conversion

DOE PAGES

Tirla, Cornelia; Dooling, Thomas; Smith, Rachel B.; ...

2013-01-01

This project’s aim was to develop a way to use Infrared (IR) Spectroscopy to determine the extent of the conversion of oil to biodiesel produced during a typical transesterification process. The most reliable method of biodiesel analysis is gas chromatography with flame ionization detector (GC-FID) analysis. This analysis is not ideal for the educational or field applications since it is time intensive and requires expensive, specialized equipment. The use of the FT-IR is faster and more affordable. A calibration curve was created by comparing data on the purity of biodiesel samples obtained from the GC-FID analysis to the ratio ofmore » the absorbances at 1197 cm -1 to 1166 cm -1 from the FT-IR spectrum. For field application, a similar method was developed using a portable IR spectrometer, the InfraSpecTM VFA-IR spectrometer. As a result, the data collected gave a good linear fit for % purity of the samples and can be used as a method for monitoring the conversion of different types of oils to biodiesel and determining the purity of biodiesel produced from oil.« less

Silicon crystal growth in vacuum

NASA Technical Reports Server (NTRS)

Khattak, C. P.; Schmid, F.

1982-01-01

The most developed process for silicon crystal growth is the Czochralski (CZ) method which was in production for over two decades. In an effort to reduce cost of single crystal silicon for photovoltaic applications, a directional solidification technique, Heat Exchanger Method (HEM), was adapted. Materials used in HEM and CZ furnaces are quite similar (heaters, crucibles, insulation, etc.). To eliminate the cost of high purity argon, it was intended to use vacuum operation in HEM. Two of the major problems encountered in vacuum processing of silicon are crucible decomposition and silicon carbide formation in the melt.

METHOD AND APPARATUS FOR MAKING URANIUM-HYDRIDE COMPACTS

DOEpatents

Wellborn, W.; Armstrong, J.R.

1959-03-10

A method and apparatus are presented for making compacts of pyrophoric hydrides in a continuous operation out of contact with air. It is particularly useful for the preparation of a canned compact of uranium hydride possessing high density and purity. The metallic uranium is enclosed in a container, positioned in a die body evacuated and nvert the uranium to the hydride is admitted and the container sealed. Heat is applied to bring about the formation of the hydride, following which compression is used to form the compact sealed in a container ready for use.

Acoustic emission from a solidifying aluminum-lithium alloy

NASA Technical Reports Server (NTRS)

Henkel, D. P.; Wood, J. D.

1992-01-01

Physical phenomena associated with the solidification of an AA2090 Al-Li alloy have been characterized by AE methods. Repeatable patterns of AE activity as a function of solidification time are recorded and explained for ultrahigh-purity (UHP) aluminum and an Al-4.7 wt pct Cu binary alloy, in addition to the AA2090 Al-Li alloy, by the complementary utilization of thermal, AE, and metallographic methods. One result shows that the solidification of UHP aluminum produces one discrete period of high AE activity as the last 10 percent of solid forms.

Preparative separation of bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze using steam distillation extraction and one step high-speed counter-current chromatography.

PubMed

Wei, Yun; Du, Jilin; Lu, Yuanyuan

2012-10-01

In order to utilize and control the invasive weed, bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze were studied. Steam distillation extraction and one step high-speed counter-current chromatography were applied to separate and purify the caryophyllene oxide, 7,11-dimethyl-3-methylene-1,6,10-dodecatriene, and caryophyllene from essential oil of Flaveria bidentis (L.) Kuntze. The two-phase solvent system containing n-hexane/acetonitrile/ethanol (5:4:3, v/v/v) was selected for the one step separation mode according to the partition coefficient values (K) of the target compounds and the separation factor (α). The purity of each isolated fraction after a single high-speed counter-current chromatography run was determined by high performance liquid chromatography. A 3.2 mg of caryophyllene oxide at a purity of 92.6%, 10.4 mg of 7,11-dimethyl-3-methylene-1,6,10-dodecatriene at a purity of 99.1% and 5.7 mg of caryophyllene at a purity of 98.8% were obtained from 200 mg essential oil of Flaveria bidentis (L.) Kuntze. The chemical structures of these components were identified by GC-MS, (1) H-NMR, and (13) C-NMR. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigation of the plastic fracture of high strength steels

NASA Technical Reports Server (NTRS)

Cox, T. B.; Low, J. R., Jr.

1972-01-01

An investigation of the plastic fracture process to improve tensile strength in high strength steels is presented. Two generic types of steels are considered: a quenched and tempered grade and a maraging grade, in order to compare two different matrix microstructures. Each type of steel was studied in commercial grade purity and in special melted high purity form, low in residual and impurity elements. The specific alloys dealt with include AISI 4340 and 18 Ni, 200 grade maraging steel, both heat treated to the same yield strength level of approximately 200 ksi.

Neutron energy determination with a high-purity germanium detector

NASA Technical Reports Server (NTRS)

Beck, Gene A.

1992-01-01

Two areas that are related to planetary gamma-ray spectrometry are investigated. The first task was the investigation of gamma rays produced by high-energy charged particles and their secondaries in planetary surfaces by means of thick target bombardments. The second task was the investigation of the effects of high-energy neutrons on gamma-ray spectral features obtained with high-purity Ge-detectors. For both tasks, as a function of the funding level, the experimental work was predominantly tied to that of other researchers, whenever there was an opportunity to participate in bombardment experiments at large or small accelerators for charged particles.

Isolation and purification of macrocyclic components from Penicillium fermentation broth by high-speed counter-current chromatography.

PubMed

Gao, Xiang; Zhuang, Rongqiang; Guo, Jiannan; Bao, Jian; Fang, Meijuan; Liu, Yan; Xu, Pengxiang; Zhao, Yufen

2010-02-01

In this paper, high-speed counter-current chromatography (HSCCC), assisted with ESI-MS, was first successfully applied to the preparative separation of three macrolide antibiotics, brefeldin A (12.6 mg, 99.0%), 7'-O-formylbrefeldin A (6.5 mg, 95.0%) and 7'-O-acetylbrefeldin A (5.0 mg, 92.3%) from the crude extract of the microbe Penicillium SHZK-15. Considering the chemical nature and partition coefficient (K) values of the three target compounds, a two-step HSCCC isolation protocol was developed in order to obtain products with high purity. In the two-step method, the crude ethyl acetate extract was first fractionated and resulted in two peak fractions by HSCCC using solvent system n-hexane/ethyl acetate/methanol/water (HEMWat) (3:7:5:5 v/v/v/v), then purified using solvent systems HEMWat (3:5:3:5 v/v/v/v) and HEMWat (7:3:5:5 v/v/v/v) for each fraction. The purities and structures of the isolated compounds were determined by HPLC, X-ray crystallography, ESI-MS and NMR. The results demonstrated that HSCCC is a fast and efficient technique for systematic isolation of bioactive compounds from the microbes.

Cleaning and passivation of copper surfaces to remove surface radioactivity and prevent oxide formation

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

Hoppe, Eric W.; Seifert, Allen; Aalseth, Craig E.

High-purity copper is an attractive material for constructing ultra-low-background radiation measurement devices. Many low-background experiments using high-purity copper have indicated surface contamination emerges as the dominant background. Radon daughters plate out on exposed surfaces, leaving a residual 210Pb background that is difficult to avoid. Dust is also a problem; even under cleanroom conditions, the amount of U and Th deposited on surfaces can represent the largest remaining background. To control these backgrounds, a copper cleaning chemistry has been developed. Designed to replace an effective, but overly aggressive concentrated nitric acid etch, this peroxide-based solution allows for a more controlled cleaningmore » of surfaces. The acidified hydrogen peroxide solution will generally target the Cu+/Cu2+ species which are the predominant surface participants, leaving the bulk of copper metal intact. This preserves the critical tolerances of parts and eliminates significant waste disposal issues. Accompanying passivation chemistry has also been developed that protects copper surfaces from oxidation. Using a high-activity polonium surface spike, the most difficult-to-remove daughter isotope of radon, the performance of these methods are quantified. © 2001 Elsevier Science. All rights reserved« less

One-pot production of chitin with high purity from lobster shells using choline chloride-malonic acid deep eutectic solvent.

PubMed

Zhu, Ping; Gu, Zhongji; Hong, Shu; Lian, Hailan

2017-12-01

For the first time in this study, chitin was solely extracted from lobster shells through a fast, easy and eco-friendly method using deep eutectic solvents (DESs), consisting of mixtures of choline chloride-thiourea (CCT), choline chloride-urea (CCU), choline chloride-glycerol (CCG) and choline chloride-malonic acid (CCMA). The physiochemical properties of the isolated chitins were compared with those of the chemically prepared one and commercial one from shrimp shells. Results showed that CCT, CCU and CCG DESs had no important effect on the elimination of proteins and minerals, while chitin obtained by CCMA DES showed a high purity. The yield (20.63±3.30%) of chitin isolated by CCMA DES was higher than that (16.53±2.35%) of the chemically prepared chitin. The chitin obtained by CCMA DES could be divided into two parts with different crystallinity (67.2% and 80.6%), which also had different thermal stability. Chitin from lobster shells showed porous structure, which is expected to be used for adsorption materials and tissue engineering. Copyright © 2017 Elsevier Ltd. All rights reserved.

1,1-dimethylhydrazine as a high purity nitrogen source for MOVPE-water reduction and quantification using nuclear magnetic resonance, gas chromatography-atomic emission detection spectroscopy and cryogenic-mass spectroscopy analytical techniques

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

Odedra, R.; Smith, L.M.; Rushworth, S.A.

2000-01-01

Hydrazine derivatives are attractive low temperature nitrogen sources for use in MOVPE due to their low thermal stability. However their purification and subsequent analysis has not previously been investigated in depth for this application. A detailed study on 1,1-dimethylhydrazine {l{underscore}brace}(CH{sub 3}){sub 2}N-NH{sub 2}{r{underscore}brace} purified by eight different methods and the subsequent quantitative measurements of water present in the samples obtained is reported here. A correlation between {sup 1}H nuclear magnetic resonance spectroscopy (NMR), gas chromatography-atomic emission detection (GC-AED) and cryogenic mass spectroscopy (Cryogenic-MS) has been performed. All three analysis techniques can be used to measure water in the samples andmore » with the best purification the water content can be lowered well below 100 ppm. The high purity of this material has been demonstrated by growth results and the state-of-the-art performance of laser diodes.« less

Method for removing metal vapor from gas streams

DOEpatents

Ahluwalia, R.K.; Im, K.H.

1996-04-02

A process for cleaning an inert gas contaminated with a metallic vapor, such as cadmium, involves withdrawing gas containing the metallic contaminant from a gas atmosphere of high purity argon; passing the gas containing the metallic contaminant to a mass transfer unit having a plurality of hot gas channels separated by a plurality of coolant gas channels; cooling the contaminated gas as it flows upward through the mass transfer unit to cause contaminated gas vapor to condense on the gas channel walls; regenerating the gas channels of the mass transfer unit; and, returning the cleaned gas to the gas atmosphere of high purity argon. The condensing of the contaminant-containing vapor occurs while suppressing contaminant particulate formation, and is promoted by providing a sufficient amount of surface area in the mass transfer unit to cause the vapor to condense and relieve supersaturation buildup such that contaminant particulates are not formed. Condensation of the contaminant is prevented on supply and return lines in which the contaminant containing gas is withdrawn and returned from and to the electrorefiner and mass transfer unit by heating and insulating the supply and return lines. 13 figs.

Effect of alkali treatment on surface morphology of titanium

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

Tan, K. J., E-mail: gd130056@siswa.uthm.edu.my; Wahab, M. A. A., E-mail: cd110006@siswa.uthm.edu.my; Mahmod, S., E-mail: cd110201@siswa.uthm.edu.my

2015-07-22

Alkali and heat treatments were first introduced by Kim et al. to prepare a bioactive surface on titanium. This method has been proven very effective and widely used in other studies to promote titanium osteointegration. This study aims to investigate further the effect of alkali treatment on surface morphology of high purity titanium. High purity titanium foils were immersed in NaOH aqueous solutions of 0.5 M, 5 M and 15 M at 60°C and 80 °C for 1, 3 and 7 days. The surface morphology was examined using Field Emission Scanning Electron Microscope (FESEM). The obtained phases were analysed usingmore » Fourier Transform Infrared Spectroscopy (FTIR) in the spectra range of 4000-600 cm{sup −1} at 4 cm{sup −1} resolution and 50 scans. At the same soaking temperature and soaking time, a thicker porous network was observed with increasing concentration of NaOH. At the same soaking temperature, a much porous structure was observed with increasing soaking time. At constant alkali concentration, more homogenously distributed porous surface structure was observed with increasing soaking temperature.« less

Development of electrically insulating coatings for service in a lithium environment

NASA Astrophysics Data System (ADS)

Natesan, K.; Uz, M.; Wieder, S.

2000-12-01

Several experiments were conducted to develop electrically insulating CaO coatings on a V-4Cr-4Ti alloy for application in a Li environment. The coatings were developed by vapor-phase transport external to Li, and also in situ in a Li-Ca environment at elevated temperature. In the vapor-phase study, several geometrical arrangements were examined to obtain a uniform coating of Ca on the specimens, which were typically coupons measuring 5 to 10 × 5 × 1 mm 3. After Ca deposition from the vapor phase, the specimens were oxidized in a high-purity argon environment at 600°C to convert the deposited metal into oxide. The specimens exhibited insulating characteristics after this oxidation step. Several promising coated specimens were then exposed to high-purity Li at 500°C for 48-68 h to determine coating integrity. Microstructural characteristics of the coatings were evaluated by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) analysis. Electrical resistances of the coatings were measured by a two-probe method between room temperature and 700°C before and after exposure to Li.

Method for removing metal vapor from gas streams

DOEpatents

Ahluwalia, R. K.; Im, K. H.

1996-01-01

A process for cleaning an inert gas contaminated with a metallic vapor, such as cadmium, involves withdrawing gas containing the metallic contaminant from a gas atmosphere of high purity argon; passing the gas containing the metallic contaminant to a mass transfer unit having a plurality of hot gas channels separated by a plurality of coolant gas channels; cooling the contaminated gas as it flows upward through the mass transfer unit to cause contaminated gas vapor to condense on the gas channel walls; regenerating the gas channels of the mass transfer unit; and, returning the cleaned gas to the gas atmosphere of high purity argon. The condensing of the contaminant-containing vapor occurs while suppressing contaminant particulate formation, and is promoted by providing a sufficient amount of surface area in the mass transfer unit to cause the vapor to condense and relieve supersaturation buildup such that contaminant particulates are not formed. Condensation of the contaminant is prevented on supply and return lines in which the contaminant containing gas is withdrawn and returned from and to the electrorefiner and mass transfer unit by heating and insulating the supply and return lines.

Lecithin-based microemulsion of a peptide for oral administration: preparation, characterization, and physical stability of the formulation.

PubMed

Cilek, Ayşe; Celebi, Nevin; Tirnaksiz, Figen

2006-01-01

The objective of our study was to prepare and characterize a stable microemulsion formulation for oral administration of a peptide, e.g., rh-insulin. The microemulsions were prepared using Labrafil M 1944 CS, Phospholipon 90G (lecithin), absolute alcohol, and bidistilled water. Commercially available soybean lecithins (namely, Phospholipon 80, phosphatidylcholine purity 76 +/- 3%, and Phospholipon 90G, phosphatidylcholine purity 93 +/- 3%) were used in the study. The results showed that the phase diagram obtained using a low purity lecithin was not similar to that obtained with a high purity lecithin. We observed that the microemulsion area was wider at the phase diagram obtained with the higher purity lecithin. We found that the extent of the microemulsion region depended upon both the purity of the lecithin and the surfactant/co-surfactant (s/co-s) mixing ratios (K(m)). The rheological studies showed that microemulsions followed a Newtonian behavior. Such physical characteristics as viscosity, turbidity, density, conductivity, refractive index, droplet size, physical appearance, and phase separation of the microemulsion were measured at different temperatures (4 degrees C, 25 degrees C, and 40 degrees C) during 6 months. The results indicated that the physical characteristics of the developed microemulsions did not change under different storage temperatures (p > 0.05).

Expression, Purification and Characterization of GMZ2'.10C, a Complex Disulphide-Bonded Fusion Protein Vaccine Candidate against the Asexual and Sexual Life-Stages of the Malaria-Causing Plasmodium falciparum Parasite.

PubMed

Mistarz, Ulrik H; Singh, Susheel K; Nguyen, Tam T T N; Roeffen, Will; Yang, Fen; Lissau, Casper; Madsen, Søren M; Vrang, Astrid; Tiendrebeogo, Régis W; Kana, Ikhlaq H; Sauerwein, Robert W; Theisen, Michael; Rand, Kasper D

2017-09-01

Production and characterization of a chimeric fusion protein (GMZ2'.10C) which combines epitopes of key malaria parasite antigens: glutamate-rich protein (GLURP), merozoite surface protein 3 (MSP3), and the highly disulphide bonded Pfs48/45 (10C). GMZ2'.10C is a potential candidate for a multi-stage malaria vaccine that targets both transmission and asexual life-cycle stages of the parasite. GMZ2'.10C was produced in Lactococcus lactis and purified using either an immunoaffinity purification (IP) or a conventional purification (CP) method. Protein purity and stability was analysed by RP-HPLC, SEC-HPLC, 2-site ELISA, gel-electrophoresis and Western blotting. Structural characterization (mass analysis, peptide mapping and cysteine connectivity mapping) was performed by LC-MS/MS. CP-GMZ2'.10C resulted in similar purity, yield, structure and stability as compared to IP-GMZ2'.10C. CP-GMZ2'.10C and IP-GMZ2'.10C both elicited a high titer of transmission blocking (TB) antibodies in rodents. The intricate disulphide-bond connectivity of C-terminus Pfs48/45 was analysed by tandem mass spectrometry and was established for GMZ2'.10C and two reference fusion proteins encompassing similar parts of Pfs48/45. GMZ2'.10C, combining GMZ2' and correctly-folded Pfs48/45 can be produced by the Lactoccus lactis P170 based expression system in purity and quality for pharmaceutical development and elicit high level of TB antibodies. The cysteine connectivity for the 10C region of Pfs48/45 was revealed experimentally, providing an important guideline for employing the Pfs48/45 antigen in vaccine design.

Selective dispersion of high-purity semiconducting carbon nanotubes using indacenodithiophene-based conjugated polymer

NASA Astrophysics Data System (ADS)

Ji, Dongseob; Lee, Seung-Hoon; Noh, Yong-Young

2018-01-01

The facile sorting of highly pure semiconducting single-walled carbon nanotubes (s-SWNTs) is still one of the challenging issues for the next-generation wearable electronic devices such as various opto-electric devices and field-effect transistors (FETs). Herein, we demonstrate the selective dispersion of high-purity s-SWNTs using indacenodithiophene-co-benzothiadiazole (IDT-BT), which is a state-of-the-art high-mobility conjugated polymer. By the selective wrapping of the IDT-BT copolymer, SWNTs of chiral indices (6, 5), (7, 5), (7, 6), (8, 4), (9, 4), (8, 6), (8, 7), (10, 5), (9, 7), (10, 6), (11, 1), and (13, 3) are sorted. Finally, the networked s-SWNT film formed by spin-coating is applied as an active layer of FETs that exhibited ambipolar characteristics with an average mobility of 2.28 cm2/V s in the p-channel and 2.10 cm2/V s in the n-channel. The ON/OFF ratios in both p- and n-channels are approximately 105, which supports the high purity separation of s-SWNTs wrapped by IDT-BT.

Process and apparatus for separating fine particles by microbubble flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1991-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine particles, especially coal, so as to produce a high purity and large recovery efficiently. This is accomplished through the use of a high aspect ratio flotation column, microbubbles, and a countercurrent use of wash water to gently wash the froth. Also, disclosed are unique processes and apparatus for generating microbubbles for flotation in a high efficient and inexpensive manner using either a porous tube or an in-line static generator. 23 figures.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1992-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1998-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

Small-scale purification of butyrylcholinesterase from human plasma and implementation of a μLC-UV/ESI MS/MS method to detect its organophosphorus adducts.

PubMed

John, Harald; Breyer, Felicitas; Schmidt, Christian; Mizaikoff, Boris; Worek, Franz; Thiermann, Horst

2015-10-01

Human butyrylcholinesterase (hBChE) is a serine hydrolase (EC 3.1.1.8) present in all mammalian tissues and the bloodstream. Similar to acetylcholinesterase, the enzyme reacts with organophosphorus compounds (OP) like nerve agents or pesticides that cause enzyme inhibition (BChE adducts). These adducts represent valuable biomarkers for analytical verification of OP exposure. For establishment of these mass spectrometry based methods sufficient amounts of hBChE in high purity are required. Unfortunately, commercial lots are of inappropriate purity thus favouring in-house isolation. Therefore, we developed a small scale procedure to isolate hBChE from citrate plasma. After precipitation by polyethylene glycol (8% w/v and 20% w/v PEG 6000) hBChE was purified from plasma by four consecutive chromatographic steps including anion exchange, affinity extraction and size exclusion. Protein elution was monitored on-line by UV-absorbance (280 nm) followed by continuous fractionation for off-line analysis of (1) hBChE enzyme activity by Ellman assay, (2) protein purity by gel electrophoresis, and (3) protein identity by matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). Numerous major impurities separated from hBChE were identified. The purified material was used for in vitro incubation with diverse OP to establish a μ-liquid chromatography-ultra violet detection/electrospray ionization tandem-mass spectrometric method (μLC-UV/ESI MS/MS) for detection of hBChE adducts suitable for verification analysis. Analytical data for diverse OP pesticides including deuterated analogues as well as G- and V-type nerve agents and their precursor are summarized. This method was successfully applied to plasma samples provided by the Organisation for the Prohibition of Chemical Weapons (OPCW) for the 4th Biomedical Exercise. Copyright © 2015 John Wiley & Sons, Ltd.

On the purity assessment of solid sodium borohydride

NASA Astrophysics Data System (ADS)

Botasini, Santiago; Méndez, Eduardo

2012-01-01

Since sodium borohydride has become extensively used as chemical hydrogen storage material in fuel cells, many techniques have been proposed to assess the purity of this substance. However, all of them are developed in aqueous media, where the reagent is unstable. In addition, its hygroscopic nature was difficults in any attempt to make precise quantifications. The present work compares three different methods, namely, voltammetric, titrimetric, and Fourier transformed infrared spectroscopy (FTIR) in order to assess the purity of sodium borohydride, using an expired and a new sodium borohydride samples as references. Our results show that only the FTIR measurements provide a simple and semi-quantitative means to assess the purity of sodium borohydride due to the fact that it is the only one that measures the sample in the solid state. A comparison between the experimental data and theoretical calculation reveals the identification of the absorption bands at 1437 cm-1 of sodium metaborate and 2291 cm-1 of sodium borohydride which represent a good fingerprint for the qualitative assessment of the sample quality.

Water-Assisted Highly Efficient Synthesis of Impurity-Free Single-Walled Carbon Nanotubes

NASA Astrophysics Data System (ADS)

Hata, Kenji; Futaba, Don N.; Mizuno, Kohei; Namai, Tatsunori; Yumura, Motoo; Iijima, Sumio

2004-11-01

We demonstrate the efficient chemical vapor deposition synthesis of single-walled carbon nanotubes where the activity and lifetime of the catalysts are enhanced by water. Water-stimulated enhanced catalytic activity results in massive growth of superdense and vertically aligned nanotube forests with heights up to 2.5 millimeters that can be easily separated from the catalysts, providing nanotube material with carbon purity above 99.98%. Moreover, patterned, highly organized intrinsic nanotube structures were successfully fabricated. The water-assisted synthesis method addresses many critical problems that currently plague carbon nanotube synthesis.

Engineering of Pulsatile Conduits from Human Pluripotent Stem Cell Derived Cardiomyocytes

DTIC Science & Technology

2017-06-01

patients with coronary heart disease . Oncotarget [Internet]. 2016 Nov 7; Available from: http://www.ncbi.nlm.nih.gov/pubmed/27835576. 4. Veronesi G...13. SUPPLEMENTARY NOTES 14. ABSTRACT We have derived cardiomyocytes ( heart cells) with high purity using an optimized approach that can coax human...induced pluripotent stem cells (hiPSCs) into heart cells in combination with a two-day lactate selection method that can remove non- cardiomyocytes from

Researching the Possibility of Creating Highly Effective Catalysts for the Thermochemical Heat Regeneration and Hydrocarbon Reforming

DTIC Science & Technology

2006-11-01

PHYSICAL PROPERTIES OF THE PLASMA SPRAYING PROCESS The sprayed -on material is formed by gradual deposition of separate discretely solidifying with great... deposition processes and their ecological purity. Essentially, the method of ion-plasma spraying is evaporation of a metal (or alloy ) atoms from the...29 5.1 PHYSICAL PROPERTIES OF THE PLASMA SPRAYING PROCESS ...................34 6. CATALYST SUPPORTERS FOR THE 1ST STAGE OF

Reactor for fluidized bed silane decomposition

NASA Technical Reports Server (NTRS)

Iya, Sridhar K. (Inventor)

1989-01-01

An improved heated fluidized bed reactor and method for the production of high purity polycrystalline silicon by silane pyrolysis wherein silicon seed particles are heated in an upper heating zone of the reactor and admixed with particles in a lower zone, in which zone a silane-containing gas stream, having passed through a lower cooled gas distribution zone not conducive to silane pyrolysis, contacts the heated seed particles whereon the silane is heterogeneously reduced to silicon.

The Pharmacology of p-Aminopropiophenone in the Detoxification of Cyanide

DTIC Science & Technology

1992-01-01

45). High purity PAPP ( melting point of 140°C) is available as a light yellow crystal commercially from Eastman Kodak (Rochester, NY, U.S.A...synthesized in 1900 from acetanilide and propionyl chloride (58). More modern methods of chemical synthesis from aniline derivatives appear in the literature...Other chemicals (i.e., acetanilide ) are known to produce methemoglobinemia as well as hemolysis (dogs) (100), but the mechanism is not thought to be due

21 CFR 172.869 - Sucrose oligoesters.

Code of Federal Regulations, 2011 CFR

2011-04-01

... Obtaining Method (1) Sucrose esters Not less than 90% “Method for Analyzing the Purity of Sucrose Fatty Acid... sample). Do. (8) Residual Methanol Not more than 10 milligrams/kilogram Method listed in the monograph...

21 CFR 172.869 - Sucrose oligoesters.

Code of Federal Regulations, 2010 CFR

2010-04-01

... Obtaining Method (1) Sucrose esters Not less than 90% “Method for Analyzing the Purity of Sucrose Fatty Acid... sample). Do. (8) Residual Methanol Not more than 10 milligrams/kilogram Method listed in the monograph...

Separation and purification of polyphenols from red wine extracts using high speed counter current chromatography.

PubMed

Li, Yuanyuan; Li, Lingxi; Cui, Yan; Zhang, Shuting; Sun, Baoshan

2017-06-01

Polyphenols are important compounds of red wine owing to their contribution to sensory properties and antioxidant activities. In this study, high-speed counter-current chromatography (HSCCC) coupled with semi-preparative HPLC was used for large-scale separation and purification of polyphenols from red wine extracts. With the solvent system of hexane-ethyl acetate-water (1-50-50), various oligomeric procyanidins including monomer catechin, epicatechin, dimers B1, B2; phenolic acids including coutaric acid, caftaric acid and other type of polyphenols were largely separated within 370min and most of these compounds presented high yields (0.97mg to 13.79mg) with high purity (90.34% to 98.91%) after the semi-preparative HPLC isolation. Using the solvent system of Methyl tert-Butyl Ether (MTBE) - n-butyl alcohol- acetonitrile-water (1-40-1-50, acidified with 0.01% trifluoroacetic acid (TFA)) by one-step HSCCC of 100mg of the red wine extracts, the major anthocyanins, i.e., malvidin-3-O-glucoside, delphinidin-3-O-glucoside and peonidin-3-O-glucoside, as well as two polymeric proanthocyanidin fractions were successfully separated one another within 320min. The yields of malvidin-3-O-glucoside, delphinidin-3-O-glucoside and peonidin-3-O-glucoside were 12.12mg, 1.78mg and 11.57mg with the purity of 92.74%, 91.03% and 91.21%, respectively. Thiolysis-UPLC analysis indicated that the two polymeric proanthocyanidin fractions presented high purity, with mean degree of polymerization of 7.66±0.12 and 6.20±0.09, respectively. The further experiments on the antioxidant activities by DPPH radical test, FRAP assay and ABTS method showed that all of the isolated procyandins and anthocyanins and the two polymeric proanthocyanidin fractions, with exception of phenolic acids possessed much greater antioxidant activities compared to standard Trolox andl-ascorbic acid (2-14 times). Copyright © 2017 Elsevier B.V. All rights reserved.

Converting biomass waste into microporous carbon with simultaneously high surface area and carbon purity as advanced electrochemical energy storage materials

NASA Astrophysics Data System (ADS)

Sun, Fei; Wang, Lijie; Peng, Yiting; Gao, Jihui; Pi, Xinxin; Qu, Zhibin; Zhao, Guangbo; Qin, Yukun

2018-04-01

Developing carbon materials featuring both high accessible surface area and high structure stability are desirable to boost the performance of constructed electrochemical electrodes and devices. Herein, we report a new type of microporous carbon (MPC) derived from biomass waste based on a simple high-temperature chemical activation procedure. The optimized MPC-900 possesses microporous structure, high surface area, partially graphitic structure, and particularly low impurity content, which are critical features for enhancing carbon-based electrochemical process. The constructed MPC-900 symmetric supercapacitor exhibits high performances in commercial organic electrolyte such as widened voltage window up to 3 V and thereby high energy/power densities (50.95 Wh kg-1 at 0.44 kW kg-1; 25.3 Wh kg-1 at 21.5 kW kg-1). Furthermore, a simple melt infiltration method has been employed to enclose SnO2 nanocrystals onto the carbon matrix of MPC-900 as a high-performance lithium storage material. The obtained SnO2-MPC composite with ultrafine SnO2 nanocrystals delivers high capacities (1115 mAh g-1 at 0.2 A g-1; 402 mAh g-1 at 10 A g-1) and high-rate cycling lifespan of over 2000 cycles. This work not only develops a microporous carbon with high carbon purity and high surface area, but also provides a general platform for combining electrochemically active materials.

Electrochemical Deposition of High Purity Silicon from Molten Salts

NASA Astrophysics Data System (ADS)

Haarberg, Geir Martin

Several approaches were tried in order to develop an electrochemical route for producing high purity silicon from molten salts. SiO2, K2SiF6 and metallurgical silicon were used as the source of silicon. Molten electrolytes based on chloride (CaCl2-NaCl) and fluoride (LiF-KF) at temperatures from 550 - 900 oC were used. Transient electrochemical techniques were used to study the electrochemical behaviour of dissolved silicon species. Electrolysis experiments were carried out to deposit silicon.

Electrochemical Deposition of High Purity Silicon in Molten Salts

NASA Astrophysics Data System (ADS)

Haarberg, Geir Martin

Several approaches were tried in order to develop an electrochemical route for producing high purity silicon from molten salts. SiO2, K2SiF6 and metallurgical silicon were used as the source of silicon. Molten electrolytes based on chloride (CaCl2-NaCl) and fluoride (LiF-KF) at temperatures from 550 - 900 °C were used. Transient electrochemical techniques were used to study the electrochemical behaviour of dissolved silicon species. Electrolysis experiments were carried out to deposit silicon.

Internal friction measurement in high purity tungsten single crystal

NASA Technical Reports Server (NTRS)

Rieu, G. E.

1974-01-01

Internal friction peaks observed after small deformation in high purity tungsten single crystals between liquid helium temperature and 800 K in the frequency range 30-50 KHz, are studied as a function of orientation. An orientation effect is observed in the internal friction spectra due to the creation of internal stresses. The elementary processes related to these peaks are discussed in terms of kink generation and geometric kink motion on screw and edge dislocations in an internal stress field.

Market-driven emissions from recovery of carbon dioxide gas.

PubMed

Supekar, Sarang D; Skerlos, Steven J

2014-12-16

This article uses a market-based allocation method in a consequential life cycle assessment (LCA) framework to estimate the environmental emissions created by recovering carbon dioxide (CO2). We find that 1 ton of CO2 recovered as a coproduct of chemicals manufacturing leads to additional greenhouse gas emissions of 147-210 kg CO2 eq , while consuming 160-248 kWh of electricity, 254-480 MJ of heat, and 1836-4027 kg of water. The ranges depend on the initial and final purity of the CO2, particularly because higher purity grades require additional processing steps such as distillation, as well as higher temperature and flow rate of regeneration as needed for activated carbon treatment and desiccant beds. Higher purity also reduces process efficiency due to increased yield losses from regeneration gas and distillation reflux. Mass- and revenue-based allocation methods used in attributional LCA estimate that recovering CO2 leads to 19 and 11 times the global warming impact estimated from a market-based allocation used in consequential LCA.

Efficient method for preparation of highly purified lipopolysaccharides by hydrophobic interaction chromatography.

PubMed

Muck, A; Ramm, M; Hamburger, M

1999-09-10

A method for the efficient preparation of highly purified lipopolysaccharides (LPSs) by hydrophobic interaction chromatography (HIC) has been developed. The procedure can be used for the purification of cell wall bound LPSs after hot phenol-water extraction and for the isolation of extracellular LPSs from the supernatant, respectively. The method described has been tested with artificial mixtures containing LPSs, polysaccharide, protein and RNA and subsequently employed for the preparative purification of two LPSs of different origin, namely the extracellular LPS secreted by Escherichia coli E49 into the culture medium, and the cell wall bound LPS from Pseudomonas aeruginosa VA11465/1. Compared to currently used methods for LPS purification such as enzymatic digestion and ultracentrifugation, the chromatographic separation reported here combines superior purity with minimal loss of LPS, high reproducibility and simple handling. The removal of contaminants such as protein, RNA and polysaccharides and the recovery of LPSs were monitored by appropriate assays.

Rapid isolation and purification of phorbol esters from Jatropha curcas by high-speed countercurrent chromatography.

PubMed

Hua, Wan; Hu, Huiling; Chen, Fang; Tang, Lin; Peng, Tong; Wang, Zhanguo

2015-03-18

In this work, a high-speed countercurrent chromatography (HSCCC) method was established for the preparation of phorbol esters (PEs) from Jatropha curcas. n-Hexane-ethyl acetate-methanol-water (1.5:1.5:1.2:0.5, v/v) was selected as the optimum two-phase solvent system to separate and purify jatropha factor C1 (JC1) with a purity of 85.2%, as determined by HPLC, and to obtain a mixture containing four or five PEs. Subsequently, continuous semipreparative HPLC was applied to further purify JC1 (99.8% as determined by HPLC). In addition, UPLC-PDA and UPLC-MS were established and successfully used to evaluate the isolated JC1 and PE-rich crude extract. The purity of JC1 was only 87.8% by UPLC-UV. A peak (a compound highly similar to JC1) was indentified as the isomer of JC1 by comparing the characteristic UV absorption and MS spectra. Meanwhile, this strategy was also applied to analyze the PE-rich crude extract from J. curcas. It is interesting that there may be more than 15 PEs according to the same quasi-molecular ion peaks, highly similar sequence-specific fragment ions, and similar UV absorption spectrum.

Radio Frequency Plasma Synthesis of Boron Nitride Nanotubes (BNNTs) for Structural Applications: Part I

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Alexa, Joel A.; Jensen, Brian J.; Thomsen, Donald L.

2016-01-01

It is evident that nanotubes, such as carbon, boron nitride and even silicon, offer great potential for many aerospace applications. The opportunity exists to harness the extremely high strength and stiffness exhibited by high-purity, low-defect nanotubes in structural materials. Even though the technology associated with carbon nanotube (CNT) development is mature, the mechanical property benefits have yet to be fully realized. Boron nitride nanotubes (BNNTs) offer similar structural benefits, but exhibit superior chemical and thermal stability. A broader range of potential structural applications results, particularly as reinforcing agents for metal- and ceramic- based composites. However, synthesis of BNNTs is more challenging than CNTs mainly because of the higher processing temperatures required, and mass production techniques have yet to emerge. A promising technique is radio frequency plasma spray (RFPS), which is an inductively coupled, very high temperature process. The lack of electrodes and the self- contained, inert gas environment lend themselves to an ultraclean product. It is the aim of this White Paper to survey the state of the art with regard to nano-material production by analyzing the pros and cons of existing methods. The intention is to combine the best concepts and apply the NASA Langley Research Center (LaRC) RFPS facility to reliably synthesize large quantities of consistent, high-purity BNNTs.

Discrimination between biologically relevant calcium phosphate phases by surface-analytical techniques

NASA Astrophysics Data System (ADS)

Kleine-Boymann, Matthias; Rohnke, Marcus; Henss, Anja; Peppler, Klaus; Sann, Joachim; Janek, Juergen

2014-08-01

The spatially resolved phase identification of biologically relevant calcium phosphate phases (CPPs) in bone tissue is essential for the elucidation of bone remodeling mechanisms and for the diagnosis of bone diseases. Analytical methods with high spatial resolution for the discrimination between chemically quite close phases are rare. Therefore the applicability of state-of-the-art ToF-SIMS, XPS and EDX as chemically specific techniques was investigated. The eight CPPs hydroxyapatite (HAP), β-tricalcium phosphate (β-TCP), α-tricalcium phosphate (α-TCP), octacalcium phosphate (OCP), dicalcium phosphate dihydrate (DCPD), dicalcium phosphate (DCP), monocalcium phosphate (MCP) and amorphous calcium phosphate (ACP) were either commercial materials in high purity or synthesized by ourselves. The phase purity was proven by XRD analysis. All of the eight CPPs show different mass spectra and the phases can be discriminated by applying the principal component analysis method to the mass spectrometric data. The Ca/P ratios of all phosphates were determined by XPS and EDX. With both methods some CPPs can be distinguished, but the obtained Ca/P ratios deviate systematically from their theoretical values. It is necessary in any case to determine a calibration curve, respectively the ZAF values, from appropriate standards. In XPS also the O(1s)-satellite signals are correlated to the CPPs composition. Angle resolved and long-term XPS measurements of HAP clearly prove that there is no phosphate excess at the surface. Decomposition due to X-ray irradiation has not been observed.

Study of structural properties of cubic InN films on GaAs(001) substrates by molecular beam epitaxy and migration enhanced epitaxy

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

Casallas-Moreno, Y. L.; Perez-Caro, M.; Gallardo-Hernandez, S.

InN epitaxial films with cubic phase were grown by rf-plasma-assisted molecular beam epitaxy (RF-MBE) on GaAs(001) substrates employing two methods: migration-enhanced epitaxy (MEE) and conventional MBE technique. The films were synthesized at different growth temperatures ranging from 490 to 550 Degree-Sign C, and different In beam fluxes (BEP{sub In}) ranging from 5.9 Multiplication-Sign 10{sup -7} to 9.7 Multiplication-Sign 10{sup -7} Torr. We found the optimum conditions for the nucleation of the cubic phase of the InN using a buffer composed of several thin layers, according to reflection high-energy electron diffraction (RHEED) patterns. Crystallographic analysis by high resolution X-ray diffraction (HR-XRD)more » and RHEED confirmed the growth of c-InN by the two methods. We achieved with the MEE method a higher crystal quality and higher cubic phase purity. The ratio of cubic to hexagonal components in InN films was estimated from the ratio of the integrated X-ray diffraction intensities of the cubic (002) and hexagonal (1011) planes measured by X-ray reciprocal space mapping (RSM). For MEE samples, the cubic phase of InN increases employing higher In beam fluxes and higher growth temperatures. We have obtained a cubic purity phase of 96.4% for a film grown at 510 Degree-Sign C by MEE.« less

Quality control of positron emission tomography radiopharmaceuticals: An institutional experience.

PubMed

Shukla, Jaya; Vatsa, Rakhee; Garg, Nitasha; Bhusari, Priya; Watts, Ankit; Mittal, Bhagwant R

2013-10-01

To study quality control parameters of routinely prepared positron emission tomography (PET) radiopharmaceuticals. Three PET radiopharmaceuticals fluorine-18 fluorodeoxyglucose (F-18 FDG), N-13 ammonia (N-13 NH3), and Ga-68 DOTATATE (n = 25 each), prepared by standardized protocols were used. The radionuclide purity, radiochemical purity, residual solvents, pH, endotoxins, and sterility of these radiopharmaceuticals were determined. The physical half-life of radionuclide in radiopharmaceuticals, determined by both graphical and formula method, demonstrated purity of radionuclides used. pH of all PET radiopharmaceuticals used was in the range of 5-6.5. No microbial growth was observed in radiopharmaceutical preparations. The residual solvents, chemical impurity, and pyrogens were within the permissible limits. All three PET radiopharmaceuticals were safe for intravenous administration.

Method for producing metal oxide aerogels

DOEpatents

Tillotson, Thomas M.; Poco, John F.; Hrubesh, Lawrence W.; Thomas, Ian M.

1995-01-01

A two-step hydrolysis-condensation method was developed to form metal oxide aerogels of any density, including densities of less than 0.003g/cm.sup.3 and greater than 0.27g/cm.sup.3. High purity metal alkoxide is reacted with water, alcohol solvent, and an additive to form a partially condensed metal intermediate. All solvent and reaction-generated alcohol is removed, and the intermediate is diluted with a nonalcoholic solvent. The intermediate can be stored for future use to make aerogels of any density. The aerogels are formed by reacting the intermediate with water, nonalcoholic solvent, and a catalyst, and extracting the nonalcoholic solvent directly. The resulting monolithic aerogels are hydrophobic and stable under atmospheric conditions, and exhibit good optical transparency, high clarity, and homogeneity. The aerogels have high thermal insulation capacity, high porosity, mechanical strength and stability, and require shorter gelation times than aerogels formed by conventional methods.

Method for producing metal oxide aerogels

DOEpatents

Tillotson, T.M.; Poco, J.F.; Hrubesh, L.W.; Thomas, I.M.

1995-04-25

A two-step hydrolysis-condensation method was developed to form metal oxide aerogels of any density, including densities of less than 0.003g/cm{sup 3} and greater than 0.27g/cm{sup 3}. High purity metal alkoxide is reacted with water, alcohol solvent, and an additive to form a partially condensed metal intermediate. All solvent and reaction-generated alcohol is removed, and the intermediate is diluted with a nonalcoholic solvent. The intermediate can be stored for future use to make aerogels of any density. The aerogels are formed by reacting the intermediate with water, nonalcoholic solvent, and a catalyst, and extracting the nonalcoholic solvent directly. The resulting monolithic aerogels are hydrophobic and stable under atmospheric conditions, and exhibit good optical transparency, high clarity, and homogeneity. The aerogels have high thermal insulation capacity, high porosity, mechanical strength and stability, and require shorter gelation times than aerogels formed by conventional methods. 8 figs.

A novel and rapid method for obtaining high titre intact prion strains from mammalian brain.

PubMed

Wenborn, Adam; Terry, Cassandra; Gros, Nathalie; Joiner, Susan; D'Castro, Laura; Panico, Silvia; Sells, Jessica; Cronier, Sabrina; Linehan, Jacqueline M; Brandner, Sebastian; Saibil, Helen R; Collinge, John; Wadsworth, Jonathan D F

2015-05-07

Mammalian prions exist as multiple strains which produce characteristic and highly reproducible phenotypes in defined hosts. How this strain diversity is encoded by a protein-only agent remains one of the most interesting and challenging questions in biology with wide relevance to understanding other diseases involving the aggregation or polymerisation of misfolded host proteins. Progress in understanding mammalian prion strains has however been severely limited by the complexity and variability of the methods used for their isolation from infected tissue and no high resolution structures have yet been reported. Using high-throughput cell-based prion bioassay to re-examine prion purification from first principles we now report the isolation of prion strains to exceptional levels of purity from small quantities of infected brain and demonstrate faithful retention of biological and biochemical strain properties. The method's effectiveness and simplicity should facilitate its wide application and expedite structural studies of prions.

Separation of catechin constituents from five tea cultivars using high-speed counter-current chromatography.

PubMed

Kumar, N Savitri; Rajapaksha, Maheshinie

2005-08-12

Catechins were extracted from five different tea (Camellia sinensis L.) cultivars. High-speed counter-current chromatography was found to be an efficient method for the separation of seven catechins from the catechin extracts. High-performance liquid chromatography was used to assess the purity of the catechins isolated. Epigallocatechin gallate (EGCG), epicatechin gallate (ECG) and epigallocatechin (EGC) of high purity (91-99%) were isolated in high yield after a single high-speed counter-current chromatography run. The two-phase solvent mixtures used for the separation of the catechin extracts were hexane:ethyl acetate:methanol:water (1:6:1:6 for TRI 2023); (1:7:1:7 for TRI 2025 and TRI 2043); (1:5:1:5 for TRI 3079) and (1:6.5:1:6.5 for TRI 4006). Fresh tea shoots from the tea cultivar TRI 2023 (150 g) gave 440 mg of 96% pure EGCG while TRI 2025 (235 g) gave 347 mg of 99% pure EGCG and 40 mg of 97% ECG, and TRI 3079 (225 g) gave 432 mg of 97% pure EGCG and 32 mg of 96% pure ECG. Tea cultivar TRI 4006 (160 g) gave EGCG (272 mg, 96% pure) and EGC (104 mg, 90% pure). 1H and 13C NMR chemical shifts for catechin gallate (CG), EGC, ECG, EGCG and epigallocatechin 3,5-di-O-gallate (EGCDG) in CD3OD were also recorded.

High-purity 3D nano-objects grown by focused-electron-beam induced deposition.

PubMed

Córdoba, Rosa; Sharma, Nidhi; Kölling, Sebastian; Koenraad, Paul M; Koopmans, Bert

2016-09-02

To increase the efficiency of current electronics, a specific challenge for the next generation of memory, sensing and logic devices is to find suitable strategies to move from two- to three-dimensional (3D) architectures. However, the creation of real 3D nano-objects is not trivial. Emerging non-conventional nanofabrication tools are required for this purpose. One attractive method is focused-electron-beam induced deposition (FEBID), a direct-write process of 3D nano-objects. Here, we grow 3D iron and cobalt nanopillars by FEBID using diiron nonacarbonyl Fe2(CO)9, and dicobalt octacarbonyl Co2(CO)8, respectively, as starting materials. In addition, we systematically study the composition of these nanopillars at the sub-nanometer scale by atom probe tomography, explicitly mapping the homogeneity of the radial and longitudinal composition distributions. We show a way of fabricating high-purity 3D vertical nanostructures of ∼50 nm in diameter and a few micrometers in length. Our results suggest that the purity of such 3D nanoelements (above 90 at% Fe and above 95 at% Co) is directly linked to their growth regime, in which the selected deposition conditions are crucial for the final quality of the nanostructure. Moreover, we demonstrate that FEBID and the proposed characterization technique not only allow for growth and chemical analysis of single-element structures, but also offers a new way to directly study 3D core-shell architectures. This straightforward concept could establish a promising route to the design of 3D elements for future nano-electronic devices.

High-purity 3D nano-objects grown by focused-electron-beam induced deposition

NASA Astrophysics Data System (ADS)

Córdoba, Rosa; Sharma, Nidhi; Kölling, Sebastian; Koenraad, Paul M.; Koopmans, Bert

2016-09-01

To increase the efficiency of current electronics, a specific challenge for the next generation of memory, sensing and logic devices is to find suitable strategies to move from two- to three-dimensional (3D) architectures. However, the creation of real 3D nano-objects is not trivial. Emerging non-conventional nanofabrication tools are required for this purpose. One attractive method is focused-electron-beam induced deposition (FEBID), a direct-write process of 3D nano-objects. Here, we grow 3D iron and cobalt nanopillars by FEBID using diiron nonacarbonyl Fe2(CO)9, and dicobalt octacarbonyl Co2(CO)8, respectively, as starting materials. In addition, we systematically study the composition of these nanopillars at the sub-nanometer scale by atom probe tomography, explicitly mapping the homogeneity of the radial and longitudinal composition distributions. We show a way of fabricating high-purity 3D vertical nanostructures of ˜50 nm in diameter and a few micrometers in length. Our results suggest that the purity of such 3D nanoelements (above 90 at% Fe and above 95 at% Co) is directly linked to their growth regime, in which the selected deposition conditions are crucial for the final quality of the nanostructure. Moreover, we demonstrate that FEBID and the proposed characterization technique not only allow for growth and chemical analysis of single-element structures, but also offers a new way to directly study 3D core-shell architectures. This straightforward concept could establish a promising route to the design of 3D elements for future nano-electronic devices.

Initial Results from the Majorana Demonstrator

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

Elliott, S. R.; Abgrall, N.; Arnquist, I. J.

The Majorana Collaboration has assembled an array of high purity Ge detectors to search for neutrinoless double-beta decay in 76Ge with the goal of establishing the required background and scalability of a Ge-based next-generation tonne-scale experiment. The Majorana Demonstrator consists of 44 kg of high-purity Ge (HPGe) detectors (30 kg enriched in 76Ge) with a low-noise p-type point contact (PPC) geometry. The detectors are split between two modules which are contained in a single lead and high-purity copper shield at the Sanford Underground Research Facility in Lead, South Dakota. Following a commissioning run that started in June 2015, the fullmore » detector array has been acquiring data since August 2016. We will discuss the status of the Majorana Demonstrator and initial results from the first physics run; including current background estimates, exotic low-energy physics searches, projections on the physics reach of the Demonstrator, and implications for a tonne-scale Ge based Neutrinoless double-beta decay search.« less

Production of extreme-purity aluminum and silicon by fractional crystallization processing

NASA Astrophysics Data System (ADS)

Dawless, R. K.; Troup, R. L.; Meier, D. L.; Rohatgi, A.

1988-06-01

Large scale fractional crystallization is used commercially at Alcoa to produce extreme purity aluminum (99.999+% Al). The primary market is sputtering targets used to make interconnects for integrated circuits. For some applications the impurities uranium and thorium are reduced to less than 1 ppbw to avoid "soft errors" associated with α particle emission. The crystallization process achieves segregation coefficients which are close to theoretical at normal yields, and this, coupled with the scale of the units, allows practical production of this material. The silicon purification process involves crystallization of Si from molten aluminum alloys containing about 30% silicon. The crystallites from this process are further treated to remove residual Al and an extreme purity ingot is obtained. This material is considered suitable for single crystal or ribbon type photovoltaic cells and for certain IC applications, including highly doped substrates used for epitaxial growth. In production of both extreme purity Al and Si, impurities are rejected to the remaining melt as the crystals form and some separation is achieved by draining this downgraded melt from the unit. Purification of this downgrade by crystallization has also been demonstrated for both systems and is important for achieving high recoveries.

Miniature Distillation Column for Producing LOX From Air

NASA Technical Reports Server (NTRS)

Rozzi, Jay C.

2006-01-01

The figure shows components of a distillation column intended for use as part of a system that produces high-purity liquid oxygen (LOX) from air by distillation. (The column could be easily modified to produce high-purity liquid nitrogen.) Whereas typical industrial distillation columns for producing high-purity liquid oxygen and/or nitrogen are hundreds of feet tall, this distillation column is less than 3 ft (less than about 0.9 m) tall. This column was developed to trickle-charge a LOX-based emergency oxygen system (EOS) for a large commercial aircraft. A description of the industrial production of liquid oxygen and liquid nitrogen by distillation is prerequisite to a meaningful description of the present miniaturized distillation column. Typically, such industrial production takes place in a chemical processing plant in which large quantities of high-pressure air are expanded in a turboexpander to (1) recover a portion of the electrical power required to compress the air and (2) partially liquefy the air. The resulting two-phase flow of air is sent to the middle of a distillation column. The liquid phase is oxygen-rich, and its oxygen purity increases as it flows down the column. The vapor phase is nitrogen-rich and its nitrogen purity increases as it flows up the column. A heater or heat exchanger, commonly denoted a reboiler, is at the bottom of the column. The reboiler is so named because its role is to reboil some of the liquid oxygen collected at the bottom of the column to provide a flow of oxygen-rich vapor. As the oxygen-rich vapor flows up the column, it absorbs the nitrogen in the down-flowing liquid by mass transfer. Once the vapor leaves the lower portion of the column, it interacts with down-flowing nitrogen liquid that has been condensed in a heat exchanger, commonly denoted a condenser, at the top of the column. Liquid oxygen and liquid nitrogen products are obtained by draining some of the purified product at the bottom and top of the column, respectively. Because distillation is a mass-transfer process, the purity of the product(s) can be increased by increasing the effectiveness of the mass-transfer process (increasing the mass-transfer coefficient) and/or by increasing the available surface area for mass transfer through increased column height. The diameter of a distillation column is fixed by pressure-drop and mass-flow requirements. The approach taken in designing the present distillation column to be short yet capable of yielding a product of acceptably high purity was to pay careful attention to design details that affect mass-transfer processes.

Flightweight Electro-Magnet Systems

NASA Technical Reports Server (NTRS)

Goodrich, Roy G.; Litchford, Ron; Robertson, Tony; Schmidt, Dianne; Rodgers, Stephen L. (Technical Monitor)

2001-01-01

NASA has a need for lightweight high performance magnets to be used in propulsion systems involving plasmas. We report the design, construction, and testing of a six inch diameter by twelve inch long solenoid using high purity aluminum wire operating at a temperature of 77 Kelvin (K) for the current carrying element. High purity aluminum is the material of choice because of three properties that make it optimal for magnetic construction. At 77 K high purity aluminum has one of the lowest resistivities at 77 K of any metal (p = 0.254 muOMEGA-cm), thus reducing the power requirements for creating magnetic fields. Aluminum is a low-density (2.6989 g/cc) material and the end product magnet will be of low total mass compared to similar designs involving copper or other elements. The magneto-resistance of aluminum saturates at low magnetic fields and does not increase indefinitely as is the case in copper. The magnet consists of four layers of closely wound wire and is approximately 150 mm in diameter by 300 mm long. A cylinder made from G - 10 was machined with a spiral groove to hold the high purity Al wire and the wire wound on it. Following the winding, each layer was potted in STYCAST high thermal conductivity epoxy to provide insulation between the turns of the coil and mechanical strength. The magneto-resistance of the coil has been measured at the National High Magnetic Field Laboratory (NHMFL), Tallahassee, FL in externally applied fields to 10 tesla. Following these tests it was energized to the full 2 tesla field it can produce using the facilities of the NHMFL at the Los Alamos National Laboratory. The results of all of these tests will be presented.

pH neutralization of the by-product sludge waste water generated from waste concrete recycling process using the carbon mineralization

NASA Astrophysics Data System (ADS)

Ji, Sangwoo; Shin, Hee-young; Bang, Jun Hwan; Ahn, Ji-Whan

2017-04-01

About 44 Mt/year of waste concrete is generated in South Korea. More than 95% of this waste concrete is recycled. In the process of regenerating and recycling pulmonary concrete, sludge mixed with fine powder generated during repeated pulverization process and water used for washing the surface and water used for impurity separation occurs. In this way, the solid matter contained in the sludge as a by-product is about 40% of the waste concrete that was input. Due to the cement component embedded in the concrete, the sludge supernatant is very strong alkaline (pH about 12). And it is necessary to neutralization for comply with environmental standards. In this study, carbon mineralization method was applied as a method to neutralize the pH of highly alkaline waste water to under pH 8.5, which is the water quality standard of discharged water. CO2 gas (purity 99%, flow rate 10ml/min.) was injected and reacted with the waste water (Ca concentration about 750mg/L) from which solid matter was removed. As a result of the experiment, the pH converged to about 6.5 within 50 minutes of reaction. The precipitate showed high whiteness. XRD and SEM analysis showed that it was high purity CaCO3. For the application to industry, it is needed further study using lower concentration CO2 gas (about 14%) which generated from power plant.

Mass fraction assignment of folic acid in a high purity material

NASA Astrophysics Data System (ADS)

Westwood, Steven; Josephs, Ralf; Choteau, Tiphaine; Daireaux, Adeline; Stoppacher, Norbert; Wielgosz, Robert; Davies, Stephen; de Rego, Eliane; Wollinger, Wagner; Garrido, Bruno; Fernandes, Jane; Lima, Jonathan; Oliveira, Rodrigo; de Sena, Rodrigo; Windust, Anthony; Huang, Ting; Dai, Xinhua; Quan, Can; He, Haihong; Zhang, Wei; Wei, Chao; Li, Na; Gao, Dexin; Liu, Zhao; Lo, Man-fung; Wong, Wai-fun; Pfeifer, Dietmar; Koch, Matthias; Dorgerloh, Ute; Rothe, Robert; Philip, Rosemary; Hirari, Nobuyasu; Fazlin Rezali, Mohd; Salazar Arzate, Claudia Marcela; Pedraza Evelina Berenice, Mercado; Serrano Caballero, Victor; Arce Osuna, Mariana; Krylov, A.; Kharitonov, S.; Lopushanskaya, E.; Liu, Qinde; Tang Lin, Teo; Fernandes-Whaley, Maria; Quinn, Laura; Nhlapo, Nontete; Prevoo-Franzsen, Desiree; Archer, Marcelle; Kim, Byungjoo; Baek, Song-Yee; Lee, Sunyoung; Lee, Joonhee; Marbumrung, Sornkrit; Kankaew, Ponhatai; Chaorenpornpukdee, Kanokrat; Chaipet, Thitiphan; Shearman, Kittiya; Ceyhan Goren, Ahmet; Gunduz, Simay; Yilmaz, Hasibe; Un, Ilker; Bilsel, Gokhan; Clarkson, Cailean; Bedner, Mary; Camara, Johanna E.; Lang, Brian E.; Lippa, Katrice A.; Nelson, Michael A.; Toman, Blaza; Yu, Lee L.

2018-01-01

The comparison required the assignment of the mass fraction of folic acid present as the main component in the comparison sample. Performance in the comparison is representative of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molecular weight range 300–500] and high polarity (pKOW < ‑2). Methods used by the eighteen participating NMIs or DIs were based on a mass balance (summation of impurities) or qNMR approach, or the combination of data obtained using both methods. The qNMR results tended to give slightly lower values for the content of folic acid, albeit with larger associated uncertainties, compared with the results obtained by mass balance procedures. Possible reasons for this divergence are discussed in the report, without reaching a definitive conclusion as to their origin. The comparison demonstrates that for a structurally complex polar organic compound containing a high water content and presenting a number of additional analytical challenges, the assignment of the mass fraction content property value of the main component can reasonably be achieved with an associated relative standard uncertainty in the assigned value of 0.5% Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Influence of Alumina Reaction Tube Impurities on the Oxidation of Chemically-Vapor-Deposited Silicon Carbide

NASA Technical Reports Server (NTRS)

Opila, Elizabeth

1995-01-01

Pure coupons of chemically vapor deposited (CVD) SiC were oxidized for 100 h in dry flowing oxygen at 1300 C. The oxidation kinetics were monitored using thermogravimetry (TGA). The experiments were first performed using high-purity alumina reaction tubes. The experiments were then repeated using fused quartz reaction tubes. Differences in oxidation kinetics, scale composition, and scale morphology were observed. These differences were attributed to impurities in the alumina tubes. Investigators interested in high-temperature oxidation of silica formers should be aware that high-purity alumina can have significant effects on experiment results.

Determination of niobium in rocks by an isotope dilution spectrophotometric method

USGS Publications Warehouse

Greenland, L.P.; Campbell, E.Y.

1970-01-01

Rocks and minerals are fused with sodium peroxide in the presence of carrierfree 95Nb. The fusion cake is leached with water and the precipitate dissolved in hydrofluoric-sulfuric acid mixture. Niobium is extracted into methyl isobutyl ketone and further purified by ion exchange. The amount of niobium is determined spectrophotometrically with 4-(2-pyridylazo)-resorcinol, and the chemical yield of the separations determined by counting 95Nb. This procedure is faster and less sensitive to interferences than previously proposed methods for determining niobium in rocks.The high purity of the separated niobium makes the method applicable to nearly all matrices. ?? 1970.

A high-performance liquid chromatography-electronic circular dichroism online method for assessing the absolute enantiomeric excess and conversion ratio of asymmetric reactions

NASA Astrophysics Data System (ADS)

Zhang, Xiang; Wang, Mingchao; Li, Li; Yin, Dali

2017-03-01

Asymmetric reactions often need to be evaluated during the synthesis of chiral compounds. However, traditional evaluation methods require the isolation of the individual enantiomer, which is tedious and time-consuming. Thus, it is desirable to develop simple, practical online detection methods. We developed a method based on high-performance liquid chromatography-electronic circular dichroism (HPLC-ECD) that simultaneously analyzes the material conversion ratio and absolute optical purity of each enantiomer. In particular, only a reverse-phase C18 column instead of a chiral column is required in our method because the ECD measurement provides a g-factor that describes the ratio of each enantiomer in the mixtures. We used our method to analyze the asymmetric hydrosilylation of β-enamino esters, and we discussed the advantage, feasibility, and effectiveness of this new methodology.

Validation of a method to measure the vector fidelity of triaxial vector sensors

NASA Astrophysics Data System (ADS)

De Freitas, J. M.

2018-06-01

A method to measure the misalignment angles and vector fidelity of a mutually orthogonal arrangement of triaxial accelerometers has been validated by introducing known misalignments into the measurement procedure. The method is based on the excitation of all three accelerometers in equal measure and the determination of the second order responsivity tensor as a metric. The sensor axis misalignment angles measured using a sensor rotation technique as a reference were 1.49°  ±  0.05°, 0.63°  ±  0.02°, and 0.78°  ±  0.04°. The resolution of the new approach against the reference was 0.03° with an accuracy of 0.2° and maximum deviation of 0.4°. An ellipticity tensor β that characterises the extent to which a triaxial system preserves the input polarisation state purity was introduced. In a careful laboratory arrangement, up to 98% input polarisation state purity was shown to be maintained. It is recommended that documentation on commercial and research grade high-precision triaxial sensor systems should give the responsivity matrix . This technique will improve the range of vector fidelity measurement tools for triaxial accelerometers and other vector sensors such as magnetometers, gyroscopes and acoustic vector sensors.

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

Junhua Jiang; Ted Aulich

An electrolytic renewable nitrogen fertilizer process that utilizes wind-generated electricity, N{sub 2} extracted from air, and syngas produced via the gasification of biomass to produce nitrogen fertilizer ammonia was developed at the University of North Dakota Energy & Environmental Research Center. This novel process provides an important way to directly utilize biosyngas generated mainly via the biomass gasification in place of the high-purity hydrogen which is required for Haber Bosch-based production of the fertilizer for the production of the widely used nitrogen fertilizers. Our preliminary economic projection shows that the economic competitiveness of the electrochemical nitrogen fertilizer process strongly dependsmore » upon the cost of hydrogen gas and the cost of electricity. It is therefore expected the cost of nitrogen fertilizer production could be considerably decreased owing to the direct use of cost-effective 'hydrogen-equivalent' biosyngas compared to the high-purity hydrogen. The technical feasibility of the electrolytic process has been proven via studying ammonia production using humidified carbon monoxide as the hydrogen-equivalent vs. the high-purity hydrogen. Process optimization efforts have been focused on the development of catalysts for ammonia formation, electrolytic membrane systems, and membrane-electrode assemblies. The status of the electrochemical ammonia process is characterized by a current efficiency of 43% using humidified carbon monoxide as a feedstock to the anode chamber and a current efficiency of 56% using high-purity hydrogen as the anode gas feedstock. Further optimization of the electrolytic process for higher current efficiency and decreased energy consumption is ongoing at the EERC.« less

Preparative separation of two subsidiary colors of FD&C Yellow No. 5 (Tartrazine) using spiral high-speed counter-current chromatography◊

PubMed Central

Roque, Jose A.; Mazzola, Eugene P.; Ito, Yoichiro

2014-01-01

Specifications in the U.S. Code of Federal Regulations for the color additive FD&C Yellow No. 5 (Colour Index No. 19140) limit the level of the tetrasodium salt of 4-[(4',5-disulfo[1,1'-biphenyl]-2-yl)hydrazono]-4,5-dihydro-5-oxo-1-(4-sulfophenyl)-1H-pyrazole-3-carboxylic acid and that of the trisodium salt of 4,4'-[4,5-dihydro-5-oxo-4-[(4-sulfophenyl)hydrazono]-1H-pyrazol-1,3-diyl]bis[benzenesulfonic acid], which are subsidiary colors abbreviated as Pk5 and Pk7, respectively. Small amounts of Pk5 and Pk7 are needed by the U.S. Food and Drug Administration for confirmatory analyses and for development of analytical methods. The present study describes the use of spiral high-speed counter-current chromatography (HSCCC) with the recently introduced highly polar organic/high-ionic strength aqueous solvent systems to separate Pk5 and Pk7 from a sample of FD&C Yellow No. 5 containing ~3.5% Pk5 and ~0.7% Pk7. Multiple ~1.0 g portions of FD&C Yellow No. 5 (totaling 6.4 g dye) were separated, using the upper phase of the solvent system 1-BuOH/EtOHabs/saturated ammonium sulfate/water, 1.7:0.3:1:1, v/v/v/v, as the mobile phase. After applying a specially developed method for removing the ammonium sulfate from the HSCCC-collected fractions, these separations resulted in an enriched mixture (~160 mg) of Pk5 and Pk7 (~46% and ~21%, respectively). Separation of the enriched mixture, this time using the lower phase of that solvent system as the mobile phase, resulted in ~ 61 mg of Pk5 collected in fractions whose purity ranged from 88.0% to 92.7% (by HPLC at 254 nm). Pk7 (20.7 mg, ~83% purity) was recovered from the upper phase of the column content. Application of this procedure also resulted in purifying the major component of FD&C Yellow No. 5 to >99% purity. The separated compounds were characterized by high-resolution mass spectrometry and several 1H and 13C nuclear magnetic resonance spectroscopic techniques (COSY, NOESY, HSQC, and HMBC). PMID:24755184

Rapid methods for the isolation of actinides Sr, Tc and Po from raw urine.

PubMed

McAlister, Daniel R; Horwitz, E Philip; Harvey, James T

2011-08-01

Rapid methods for the isolation and analysis of individual actinides (Th, U, Pu, Am/Cm) and Sr, Tc and Po from small volumes of raw urine have been developed. The methods involve acidification of the sample and the addition of aluminum nitrate or aluminum chloride salting-out agent prior to isolation of the desired analyte using a tandem combination of prefilter material and extraction chromatographic resin. The method has been applied to the separation of individual analytes from spiked urine samples. Analytes were recovered in high yield and radionuclide purity with separation times as low as 30 min. The chemistry employed is compatible with automation on the ARSIIe instrument.

Separation of two major chalcones from Angelica keiskei by high-speed counter-current chromatography.

PubMed

Kil, Yun-Seo; Nam, Joo-Won; Lee, Jun; Seo, Eun Kyoung

2015-08-01

Angelica keiskei (Shin-sun cho) is an edible higher plant with the beneficial preventive effects on cancer, hypertension, and coronary heart disease. Two bioactive chalcones of Shin-sun cho, xanthoangelol (1) and 4-hydroxyderricin (2), were separated simultaneously by using high-speed counter-current chromatography with a two-phase solvent system composed of n-hexane-EtOAc-MeOH-H2O (9:5:9:4). Only nonconsuming processes, solvent fractionations and Sephadex LH-20 column chromatography, were conducted as presteps. Xanthoangelol (1, 35.9 mg, 99.9 % purity at 254 and 365 nm) and 4-hydroxyderricin (2, 4.4 mg, 98.7 % purity at 254 nm and 98.8 % purity at 365 nm) were successfully purified from 70 mg of the processed extract from A. keiskei. The structures of two compounds were confirmed by (1)H- and (13)C-NMR analysis.

Production of carbon monoxide-free hydrogen and helium from a high-purity source

DOEpatents

Golden, Timothy Christopher [Allentown, PA; Farris, Thomas Stephen [Bethlehem, PA

2008-11-18

The invention provides vacuum swing adsorption processes that produce an essentially carbon monoxide-free hydrogen or helium gas stream from, respectively, a high-purity (e.g., pipeline grade) hydrogen or helium gas stream using one or two adsorber beds. By using physical adsorbents with high heats of nitrogen adsorption, intermediate heats of carbon monoxide adsorption, and low heats of hydrogen and helium adsorption, and by using vacuum purging and high feed stream pressures (e.g., pressures of as high as around 1,000 bar), pipeline grade hydrogen or helium can purified to produce essentially carbon monoxide -free hydrogen and helium, or carbon monoxide, nitrogen, and methane-free hydrogen and helium.

Production and characterization of anti-human IgG F(ab')2 antibody fragment.

PubMed

Valedkarimi, Zahra; Nasiri, Hadi; Aghebati-Maleki, Leili; Abdolalizadeh, Jalal; Esparvarinha, Mojghan; Majidi, Jafar

2018-04-10

In present study an optimized protocol for the separation of antibodies into antigen-binding fragments F(ab')2 using pepsin digestion was investigated. The production of these fragments is a consequential step in the development of medical research, treatment and diagnosis. For production of polyclonal antibody rabbit received antigen in four steps. The rabbit serum at 1/128000 dilution showed high absorbance in reaction with human IgG at the designed ELISA method. Rabbit IgG was purified by Ion-Exchange Chromatography (IEC) method. Purity was assessed by SDS-PAGE method. In non-reduced condition only one band was seen in about 150 kDa MW position and in reduced form, two bands were seen in 50 and 25 kDa MW positions. Rabbit IgG was digested by pepsin enzyme. The antibody fragments solution was applied to Gel filtration column to isolate the F(ab')2. Non-reduced SDS-PAGE for determining the purity of F(ab')2 fragment resulted in one band in 100 kDa corresponds to F(ab')2 fragment and a band in 150 kDa MW position corresponds to undigested IgG antibodies. The activities of FITC conjugated F(ab')2 fragment and commercial ones were compared using flowcytometry method. The activity results implied that the FITC conjugated- anti human F(ab')2 fragment worked as efficiently as the commercial one.

A method for release and multiple strand amplification of small quantities of DNA from endospores of the fastidious bacterium Pasteuria penetrans.

PubMed

Mauchline, T H; Mohan, S; Davies, K G; Schaff, J E; Opperman, C H; Kerry, B R; Hirsch, P R

2010-05-01

To establish a reliable protocol to extract DNA from Pasteuria penetrans endospores for use as template in multiple strand amplification, thus providing sufficient material for genetic analyses. To develop a highly sensitive PCR-based diagnostic tool for P. penetrans. An optimized method to decontaminate endospores, release and purify DNA enabled multiple strand amplification. DNA purity was assessed by cloning and sequencing gyrB and 16S rRNA gene fragments obtained from PCR using generic primers. Samples indicated to be 100%P. penetrans by the gyrB assay were estimated at 46% using the 16S rRNA gene. No bias was detected on cloning and sequencing 12 housekeeping and sporulation gene fragments from amplified DNA. The detection limit by PCR with Pasteuria-specific 16S rRNA gene primers following multiple strand amplification of DNA extracted using the method was a single endospore. Generation of large quantities DNA will facilitate genomic sequencing of P. penetrans. Apparent differences in sample purity are explained by variations in 16S rRNA gene copy number in Eubacteria leading to exaggerated estimations of sample contamination. Detection of single endospores will facilitate investigations of P. penetrans molecular ecology. These methods will advance studies on P. penetrans and facilitate research on other obligate and fastidious micro-organisms where it is currently impractical to obtain DNA in sufficient quantity and quality.

Automated GMP-production of α-[11 C]Methyl-L-tryptophan using a tracer production system (TPS).

PubMed

Nordeman, Patrik; Yngve, Ulrika; Wilking, Helena; Gustavsson, Sven Åke; Eriksson, Jonas; Antoni, Gunnar

2018-06-14

The radiosynthesis and GMP validation of [ 11 C] AMT for human use is described. Three consecutive batches were produced giving 940-3790 MBq (4-17% RCY, decay corrected, based on [ 11 C]CO 2 ). The molar activity at the end of synthesis was 19-35 GBq/μmol, the radiochemical purity was ≥98% and the enantiomeric purity was >99%. While the synthesis method was automated using a new generation of synthesis equipment, Tracer Production System (TPS) developed in house, the method should be readily applicable to other synthesis platforms with minor modifications. This article is protected by copyright. All rights reserved.

Approach to method development and validation in capillary electrophoresis for enantiomeric purity testing of active basic pharmaceutical ingredients.

PubMed

Sokoliess, Torsten; Köller, Gerhard

2005-06-01

A chiral capillary electrophoresis system allowing the determination of the enantiomeric purity of an investigational new drug was developed using a generic method development approach for basic analytes. The method was optimized in terms of type and concentration of both cyclodextrin (CD) and electrolyte, buffer pH, temperature, voltage, and rinsing procedure. Optimal chiral separation of the analyte was obtained using an electrolyte with 2.5% carboxymethyl-beta-CD in 25 mM NaH2PO4 (pH 4.0). Interchanging the inlet and outlet vials after each run improved the method's precision. To assure the method's suitability for the control of enantiomeric impurities in pharmaceutical quality control, its specificity, linearity, precision, accuracy, and robustness were validated according to the requirements of the International Conference on Harmonization. The usefulness of our generic method development approach for the validation of robustness was demonstrated.

Novel duplex vapor electrochemical method for silicon solar cells

NASA Technical Reports Server (NTRS)

Kapur, V.; Sancier, K. M.; Sanjurjo, A.; Leach, S.; Westphal, S.; Bartlett, R.; Nanis, L.

1978-01-01

Progress in the development of low-cost solar arrays is reported. Topics covered include: (1) development of a simplified feed system for the Na used in the Na-SiF4 reactor; (2) production of high purity silicon through the reduction of sodium fluosilicate with sodium metal; (3) the leaching process for recovering silicon from the reaction products of the SiF4-Na reaction; and (4) silicon separation by the melting of the reaction product.

Zone heating for fluidized bed silane pyrolysis

NASA Technical Reports Server (NTRS)

Iya, Sridhar K. (Inventor)

1987-01-01

An improved heated fluidized bed reactor and method for the production of high purity polycrystalline silicon by silane pyrolysis wherein silicon seed particles are heated in an upper heating zone of the reactor and admixed with particles in a lower reaction zone, in which zone a silane-containing gas stream, having passed through a lower cooled gas distribution zone not conducive to silane pyrolysis, contacts the heated seed particles whereon the silane is heterogeneously reduced to silicon.

Biodiesel production with special emphasis on lipase-catalyzed transesterification.

PubMed

Bisen, Prakash S; Sanodiya, Bhagwan S; Thakur, Gulab S; Baghel, Rakesh K; Prasad, G B K S

2010-08-01

The production of biodiesel by transesterification employing acid or base catalyst has been industrially accepted for its high conversion and reaction rates. Downstream processing costs and environmental problems associated with biodiesel production and byproducts recovery have led to the search for alternative production methods. Recently, enzymatic transesterification involving lipases has attracted attention for biodiesel production as it produces high purity product and enables easy separation from the byproduct, glycerol. The use of immobilized lipases and immobilized whole cells may lower the overall cost, while presenting less downstream processing problems, to biodiesel production. The present review gives an overview on biodiesel production technology and analyzes the factors/methods of enzymatic approach reported in the literature and also suggests suitable method on the basis of evidence for industrial production of biodiesel.

Photochemical method for generating superoxide radicals (O.sub.2.sup.-) in aqueous solutions

DOEpatents

Holroyd, Richard A.; Bielski, Benon H. J.

1980-01-01

A photochemical method and apparatus for generating superoxide radicals (ub.2.sup.-) in an aqueous solution by means of a vacuum-ultraviolet lamp of simple design. The lamp is a microwave powered rare gas device that emits far-ultraviolet light. The lamp includes an inner loop of high purity quartz tubing through which flows an oxygen-saturated sodium formate solution. The inner loop is designed so that the solution is subjected to an intense flux of far-ultraviolet light. This causes the solution to photodecompose and form the product radical (O.sub.2.sup.-).

Lyophilized Kit for the Preparation of the PET Perfusion Agent [(68)Ga]-MAA.

PubMed

Amor-Coarasa, Alejandro; Milera, Andrew; Carvajal, Denny; Gulec, Seza; McGoron, Anthony J

2014-01-01

Rapid developments in the field of medical imaging have opened new avenues for the use of positron emitting labeled microparticles. The radioisotope used in our research was (68)Ga, which is easy to obtain from a generator and has good nuclear properties for PET imaging. Methods. Commercially available macroaggregated albumin (MAA) microparticles were suspended in sterile saline, centrifuged to remove the free albumin and stannous chloride, relyophilized, and stored for later labeling with (68)Ga. Labeling was performed at different temperatures and times. (68)Ga purification settings were also tested and optimized. Labeling yield and purity of relyophilized MAA microparticles were compared with those that were not relyophilized. Results. MAA particles kept their original size distribution after relyophilization. Labeling yield was 98% at 75°C when a (68)Ga purification system was used, compared to 80% with unpurified (68)Ga. Radiochemical purity was over 97% up to 4 hours after the labeling. The relyophilized MAA and labeling method eliminate the need for centrifugation purification of the final product and simplify the labeling process. Animal experiments demonstrated the high in vivo stability of the obtained PET agent with more than 95% of the activity remaining in the lungs after 4 hours.

[Study on seed quality test and quality standard of Lonicera macranthoides].

PubMed

Zhang, Ying; Xu, Jin; Li, Long-Yun; Cui, Guang-Lin; She, Yue-Hui

2016-04-01

Referring to the rules for agricultural seed testing (GB/T 3543-1995) issued by China, the test of sampling, purity, thousand seed weight, moisture, viability, relative conductivity and germination rate had been studied for seed quality test methods of Lonicera macranthoides. The seed quality from 38 different collection areas was measured to establish quality classification standard by K-means clustering. The results showed that at least 7.5 g seeds should be sampled, and passed 20-mesh sieve for purity analysis.The 500-seed method used to measure thousand seed weight. The moisture was determined by crushed seeds dried in high temperature (130±2) ℃ for 3 h.The viability determined by 25 ℃ 0.1% TTC stained 5h in dark. 1.0 g seeds soaked in 50 ml ultra pure water in 25 ℃ for 12 hours to determine the relative conductivity. The seed by 4 ℃stratification for 80 days were cultured on paper at 15 ℃. Quality of the seeds from different areas was divided into three grades. The primary seed quality classification standard was established.The I grade and II grade were recommend use in production. Copyright© by the Chinese Pharmaceutical Association.

Residual Gas Effects on Detached Solidification in Microgravity

NASA Technical Reports Server (NTRS)

Wilcox, William R.; Regel, Liya L.; Ramakrishnan; Kota, Arun; Anand, Gaurav

2004-01-01

Our long term goal has been to make detached solidification reproducible, which requires a full understanding of the mechanisms underlying it. Our Moving Meniscus Model of steady-state detachment predicts that it depends strongly on the surface tension of the melt and the advancing contact angle with the ampoule wall. Thus, the objective of the current project was to determine the influence of residual gases on the surface tension and contact angle of molten semiconductors on typical ampoule materials. Our focus was on the influence of oxygen on indium antimonide on clean silica ("quartz"). The research was performed by three chemical engineering graduate students, the third of whom will complete his research in the summer of 2005. Originally, we had planned to use a sealed silica cell containing a zirconia electrochemical element to control the oxygen partial pressure. However, zirconia requires an operating temperature above the 530 C melting point of InSb and is difficult to form a gas-tight seal with silica. Thus, we decided instead to flow an oxygen-containing gas through the cell. A special apparatus was designed, built and perfected. A piece of InSb was placed on a horizontal silica plate in a quartz cell. High purity argon, helium or hydrogen-containing gas is passed continuously through the cell while the oxygen concentration in the effluent gas is measured. The shape of the resulting drop was used to determine contact angle and surface tension of Ga-doped and high purity InSb. Oxygen appeared to decrease the contact angle, and definitely did not increase it. The following section gives the background for the research. Section 2 summarizes the results obtained on Ga-doped InSb with relatively high oxygen concentrations. Section 3 describes recent improvements made to the apparatus and methods of analysis. Section 4 gives recent results for high-purity InSb at low oxygen concentrations. Final results will be obtained only this summer (2005). Each section has its own references.

Purity of targets prepared on Cu substrates

NASA Astrophysics Data System (ADS)

Méens, A.; Rossini, I.; Sens, J. C.

1993-09-01

The purity of several elemental self-supporting targets usually prepared by evaporation onto soluble Cu substrates has been studied. The targets were analysed by Rutherford backscattering and instrumental neutron activation analysis. Because of the high percentage of Cu observed in some Si targets, further measurements, including transmission electron microscopy, have been performed on Si targets deposited by e-gun bombardment onto Cu and ion-beam sputtering onto betaine.

Deformability and size-based cancer cell separation using an integrated microfluidic device.

PubMed

Pang, Long; Shen, Shaofei; Ma, Chao; Ma, Tongtong; Zhang, Rui; Tian, Chang; Zhao, Lei; Liu, Wenming; Wang, Jinyi

2015-11-07

Cell sorting by filtration techniques offers a label-free approach for cell separation on the basis of size and deformability. However, filtration is always limited by the unpredictable variation of the filter hydrodynamic resistance due to cell accumulation and clogging in the microstructures. In this study, we present a new integrated microfluidic device for cell separation based on the cell size and deformability by combining the microstructure-constricted filtration and pneumatic microvalves. Using this device, the cell populations sorted by the microstructures can be easily released in real time for subsequent analysis. Moreover, the periodical sort and release of cells greatly avoided cell accumulation and clogging and improved the selectivity. Separation of cancer cells (MCF-7, MDA-MB-231 and MDA231-LM2) with different deformability showed that the mixture of the less flexible cells (MCF-7) and the flexible cells (MDA-MB-231 and MDA231-LM2) can be well separated with more than 75% purity. Moreover, the device can be used to separate cancer cells from the blood samples with more than 90% cell recovery and more than 80% purity. Compared with the current filtration methods, the device provides a new approach for cancer cell separation with high collection recovery and purity, and also, possesses practical potential to be applied as a sample preparation platform for fundamental studies and clinical applications.

Widely tunable single photon source with high purity at telecom wavelength.

PubMed

Jin, Rui-Bo; Shimizu, Ryosuke; Wakui, Kentaro; Benichi, Hugo; Sasaki, Masahide

2013-05-06

We theoretically and experimentally investigate the spectral tunability and purity of photon pairs generated from spontaneous parametric down conversion in periodically poled KTiOPO(4) crystal with group-velocity matching condition. The numerical simulation predicts that the spectral purity can be kept higher than 0.81 when the wavelength is tuned from 1460 nm to 1675 nm, which covers the S-, C-, L-, and U-band in telecommunication wavelengths. We also experimentally measured the joint spectral intensity at 1565 nm, 1584 nm and 1565 nm, yielding Schmidt numbers of 1.01, 1.02 and 1.04, respectively. Such a photon source is useful for quantum information and communication systems.

Preparation of refractory cermet structures for lithium compatibility testing

NASA Technical Reports Server (NTRS)

Heestand, R. L.; Jones, R. A.; Wright, T. R.; Kizer, D. E.

1973-01-01

High-purity nitride and carbide cermets were synthesized for compatability testing in liquid lithium. A process was developed for the preparation of high-purity hafnium nitride powder, which was subsequently blended with tungsten powder or tantalum nitride and tungsten powders and fabricated into 3 in diameter billets by uniaxial hot pressing. Specimens were then cut from the billets for compatability testing. Similar processing techniques were applied to produce hafnium carbide and zirconium carbide cermets for use in the testing program. All billets produced were characterized with respect to chemistry, structure, density, and strength properties.

Aluminium. II - A review of deformation properties of high purity aluminium and dilute aluminium alloys.

NASA Technical Reports Server (NTRS)

Reed, R. P.

1972-01-01

The elastic and plastic deformation behavior of high-purity aluminum and of dilute aluminum alloys is reviewed. Reliable property data, including elastic moduli, elastic coefficients, tensile, creep, fatigue, hardness, and impact are presented. Single crystal tensile results are discussed. Rather comprehensive reference lists, containing publications of the past 20 years, are included for each of the above categories. Defect structures and mechanisms responsible for mechanical behavior are presented. Strengthening techniques (alloys, cold work, irradiation, quenching, composites) and recovery are briefly reviewed.

Experimental research of phase transitions in a melt of high-purity aluminum

NASA Astrophysics Data System (ADS)

Vorontsov, V. B.; Pershin, V. K.

2017-12-01

This scientific work is devoted to the studying of the genetic connection structures of solid and liquid phases. In this paper Fourier analysis of acoustic emission (AE) signals accompanying heating of high purity aluminum from the melting point up to 860 °C was performed. The experimental data allowed to follow the dynamics of disorder zones in the melt with increasing melt temperature up to their complete destruction. The presented results of spectral analysis of the signals were analyzed from the standpoint of the theory of cluster melting metals.

Free Flow Zonal Electrophoresis for Fractionation of Plant Membrane Compartments Prior to Proteomic Analysis.

PubMed

Barkla, Bronwyn J

2018-01-01

Free flow zonal electrophoresis (FFZE) is a versatile, reproducible, and potentially high-throughput technique for the separation of plant organelles and membranes by differences in membrane surface charge. It offers considerable benefits over traditional fractionation techniques, such as density gradient centrifugation and two-phase partitioning, as it is relatively fast, sample recovery is high, and the method provides unparalleled sample purity. It has been used to successfully purify chloroplasts and mitochondria from plants but also, to obtain highly pure fractions of plasma membrane, tonoplast, ER, Golgi, and thylakoid membranes. Application of the technique can significantly improve protein coverage in large-scale proteomics studies by decreasing sample complexity. Here, we describe the method for the fractionation of plant cellular membranes from leaves by FFZE.

Simple purification method for a recombinantly expressed native His-tag-free aminopeptidase A from Lactobacillus delbrueckii.

PubMed

Stressler, Timo; Tanzer, Coralie; Ewert, Jacob; Claaßen, Wolfgang; Fischer, Lutz

2017-03-01

The aminopeptidase A (PepA; EC 3.4.11.7) is an intracellular exopeptidase present in lactic acid bacteria. The PepA cleaves glutamyl/aspartyl residues from the N-terminal end of peptides and can, therefore, be applied for the production of protein hydrolysates with an increased amount of these amino acids, which results in a savory taste (umami). The first PepA from a lactobacilli strain was recombinantly expressed in Escherichia coli in a recently published study and harbored a C-terminal His 6 -tag for easier purification. Due to the fact that a His-tag might influence the properties of an enzyme, a simple purification method for the non-His-tagged PepA was required. Surprisingly, the PepA precipitated at a very low ammonium sulfate concentration of 5%. Unusual for a precipitating step, the purity of PepA was over 95% and the obtained activity yield was 110%. The high purity allows biochemical characterization and kinetic investigation. As a result, the optimum pH (6.0-6.5) and temperature (60-65 °C) were comparable to the His 6 -tag harboring PepA; the K M value was at 0.79 mM slightly lower compared to 1.21 mM, respectively. Since PepA is a homo dodecamer, it has a high molecular mass of approximately 480 kDa. Therefore, a subsequent preparative size-exclusion chromatography (SEC) step seemed promising. The PepA after SEC was purified to homogeneity. In summary, the simple two-step purification method presented can be applied to purify high amounts of PepA that will allow the performance of experiments in the future to crystalize PepA for the first time. Copyright © 2016 Elsevier Inc. All rights reserved.

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

Mastren, Tara; Radchenko, Valery; Hopkins, Philip D.

Ruthenium-103 is the parent isotope of 103mRh (t1/2 56.1 min), an isotope of interest for Auger electron therapy. During the proton irradiation of thorium targets, large amounts of 103Ru are generated through proton induced fission. Furthermore, the development of a two part chemical separation process to isolate 103Ru in high yield and purity from a proton irradiated thorium matrix on an analytical scale is described herein. The first part employed an anion exchange column to remove cationic actinide/lanthanide impurities along with the majority of the transition metal fission products. Secondly, an extraction chromatographic column utilizing diglycolamide functional groups was usedmore » to decontaminate 103Ru from the remaining impurities. This method then resulted in a final radiochemical yield of 83 ± 5% of 103Ru with a purity of 99.9%. Additionally, measured nuclear reaction cross sections for the formation of 103Ru and 106Ru via the 232Th(p,f) 103,106Ru reactions are reported within.« less

Development of Semiautomated Module for Preparation of 131I Labeled Lipiodol for Liver Cancer Therapy.

PubMed

Mukherjee, Archana; Subramanian, Suresh; Ambade, Rajwardhan; Avhad, Bhaurao; Dash, Ashutosh; Korde, Aruna

2017-02-01

Intra-arterial injection of 131 I Lipiodol is an effective treatment option for primary hepatocellular carcinoma as it delivers high radiation dose to liver tumor tissue with minimal accumulation in adjacent normal tissue. The present article demonstrates design, fabrication, and utilization of a semiautomated radiosynthesis module for preparation of 131 I labeled Lipiodol. The radiolabeling method was standardized for preparation of patient dose of 131 I labeled Lipiodol radiochemical yield (RCY); radiochemical purity (RCP) and pharmaceutical purity of the product were determined using optimized procedures. Sterile and apyrogenic 131 I labeled Lipiodol in >60% RCY could be prepared with >95% RCP. Preclinical evaluation in animals indicated retention of more than 90% of activity at 24 hours postportal vein injection. This is the first report demonstrating potential application of simple user friendly and safe semiautomated system for routine production of 131 I labeled Lipiodol, which is adaptable at centralized hospital radiopharmacies. The described prototype module can be modified as per demand for preparation of other therapeutic radiopharmaceuticals.

Fractionation of sheep cheese whey by a scalable method to sequentially isolate bioactive proteins.

PubMed

Pilbrow, Jodi; Bekhit, Alaa El-Din A; Carne, Alan

2016-07-15

This study reports a procedure for the simultaneous purification of glyco(caseino)macropeptide, immunoglobulin, lactoperoxidase, lactoferrin, α-lactalbumin and β-lactoglobulin from sheep cheese sweet whey, an under-utilized by-product of cheese manufacture generated by an emerging sheep dairy industry in New Zealand. These proteins have recognized value in the nutrition, biomedical and health-promoting supplements industries. A sequential fractionation procedure using economical anion and cation exchange chromatography on HiTrap resins was evaluated. The whey protein fractionation is performed under mild conditions, requires only the adjustment of pH between ion exchange chromatography steps, does not require buffer exchange and uses minimal amounts of chemicals. The purity of the whey protein fractions generated were analyzed by reversed phase-high performance liquid chromatography and the identity of the proteins was confirmed by mass spectrometry. This scalable procedure demonstrates that several proteins of recognized value can be fractionated in reasonable yield and purity from sheep cheese whey in one streamlined process. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis of SrFe12O19 magnetic nanoparticles by EDTA complex method

NASA Astrophysics Data System (ADS)

Wang, Shifa; Li, Danming; Xiao, Yuhua; Dang, Wenqiang; Feng, Jie

2017-10-01

A modified polyacrylamide gel route was used to prepare SrFe12O19 magnetic nanoparticles; ethylenediaminetetraacetic acid (EDTA) was used as a carboxyl chelating agent. The phase purity, morphology and magnetic properties of as-prepared samples were analyzed via X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometery (VSM). XRD analysis indicates that high-purity SrFe12O19 magnetic nanoparticles can be synthesized at 700°C in air. The characteristic peaks of as-prepared sample at 210, 283, 321, 340, 381, 411, 432, 475, 532, 618, 686, and 726 cm-1 were observed in Raman spectra. SEM and TEM show that the synthesized SrFe12O19 magnetic nanoparticles are uniform with the mean particle size of 60 nm. VSM measurement shows that the maximum magnetic energy product (BH)max of sample prepared using EDTA as a chelating agent is higher than that of sample prepared using citric acid as a chelating agent.

(Bi, Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x} superconductor and method of making same utilizing sinter-forging

DOEpatents

Chen, N.; Goretta, K.C.; Lanagan, M.T.

1998-10-13

A (BiPb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x}(Bi223) superconductor with high J{sub c}, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi{sub 2}O{sub 3}, PbO, SrCO{sub 3}, CaCo{sub 3} and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840 C. The partially synthesized powder is then milled for 1--4 hours before calcining further for another 50 hours at 855 C to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties. 5 figs.

(Bi, Pb).sub.2, Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x superconductor and method of making same utilizing sinter-forging

DOEpatents

Chen, Nan; Goretta, Kenneth C.; Lanagan, Michael T.

1998-01-01

A (BiPb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi223) superconductor with high J.sub.c, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi.sub.2 O.sub.3, PbO, SrCO.sub.3, CaCo.sub.3 and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840.degree. C. The partially synthesized powder is then milled for 1-4 hours before calcining further for another 50 hours at 855.degree. C. to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties.

Purification and protein composition of endogenous rat viruses.

PubMed

Hlubinová, K; Prachar, J; Vrbenská, A; Matoska, J; Simkovic, D

1984-01-01

Endogenous retroviruses are not in the majority of cases the cause of any neoplasia, except for the laboratory conditions. As far as they might serve for the evolution of pathogenic retroviruses more attention should have been paid to them. In this paper we introduce some approaches to the purification of rat endogenous retroviruses to such a degree of purity that enabled satisfactory SDS-PAGE analysis of its structural proteins. Purities of samples obtained by usual purification methods, long-term isopycnic centrifugation at a high gravity force and velocity centrifugation are compared. Protein profile of rat endogenous virus in SDS-PAGE is compared with the ones of other retroviruses. For the first time the evidence was obtained for the striking similarity between electrophoretic protein profile of rat endogenous virus WERC and feline leukemia virus. The major structural proteins of rat endogenous retrovirus and feline leukemia virus cannot be distinguished even when resolution long gradient PAGE had been employed. The accordance of electrophoretic mobilities of major structural proteins in SDS-PAGE can indicate the relatedness of retroviruses.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1992-12-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

Hydrostatic extrusion of Cu-Ag melt spun ribbon

DOEpatents

Hill, M.A.; Bingert, J.F.; Bingert, S.A.; Thoma, D.J.

1998-09-08

The present invention provides a method of producing high-strength and high-conductance copper and silver materials comprising the steps of combining a predetermined ratio of the copper with the silver to produce a composite material, and melt spinning the composite material to produce a ribbon of copper and silver. The ribbon of copper and silver is heated in a hydrogen atmosphere, and thereafter die pressed into a slug. The slug then is placed into a high-purity copper vessel and the vessel is sealed with an electron beam. The vessel and slug then are extruded into wire form using a cold hydrostatic extrusion process. 5 figs.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1998-09-29

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

Hydrostatic extrusion of Cu-Ag melt spun ribbon

DOEpatents

Hill, Mary Ann; Bingert, John F.; Bingert, Sherri A.; Thoma, Dan J.

1998-01-01

The present invention provides a method of producing high-strength and high-conductance copper and silver materials comprising the steps of combining a predetermined ratio of the copper with the silver to produce a composite material, and melt spinning the composite material to produce a ribbon of copper and silver. The ribbon of copper and silver is heated in a hydrogen atmosphere, and thereafter die pressed into a slug. The slug then is placed into a high-purity copper vessel and the vessel is sealed with an electron beam. The vessel and slug then are extruded into wire form using a cold hydrostatic extrusion process.

Assessment of the direct cyclotron production of (99m)Tc: An approach to crisis management of (99m)Tc shortage.

PubMed

Rovais, Mohammad Reza Aboudzadeh; Aardaneh, Khosro; Aslani, Gholamreza; Rahiminejad, Ali; Yousefi, Kamran; Boulouri, Fatemeh

2016-06-01

Nowadays, the cyclotron production of technetium-99m ((99m)Tc) has been increased, due to the worldwide (99m)Tc generator shortage. In the present work, an improved strategy for the production of (99m)Tc, using the proton irradiation of the enriched (100)Mo was developed. The performance of this method in terms of the production yield, chemical purity, radiochemical purity, as well as radionuclide purity was evaluated. The average production yield was measured to be 356MBqμA(-1)h(-1). A good agreement was found between the calculated production yield and the experimental one. The radiochemical separation and total recovery yields of (99m)Tc were 92% and 69%, respectively. The radiochemical and the radionuclide purities of the (99m)Tc were 99% and >99.99% at the end of purification, respectively. The results of quality control tests (QC) support the concept that cyclotron-produced (99m)Tc is suitable for preparation of USP-compliant. Copyright © 2016 Elsevier Ltd. All rights reserved.

Purity and adulterant analysis of crack seizures in Brazil.

PubMed

Fukushima, André R; Carvalho, Virginia M; Carvalho, Débora G; Diaz, Ernesto; Bustillos, Jose Oscar William Vega; Spinosa, Helenice de S; Chasin, Alice A M

2014-10-01

Cocaine represents a serious problem to society. Smoked cocaine is very addictive and it is frequently associated with violence and health issues. Knowledge of the purity and adulterants present in seized cocaine, as well as variations in drug characteristics are useful to identify drug source and estimate health impact. No data are available regarding smoked cocaine composition in most countries, and the smoked form is increasing in the Brazilian market. The purpose of the present study is to contribute to the current knowledge on the status of crack cocaine seized samples on the illicit market by the police of São Paulo. Thus, 404 samples obtained from street seizures conducted by the police were examined. The specimens were macroscopically characterized by color, form, odor, purity, and adulterant type, as well as smoke composition. Samples were screened for cocaine using modified Scott test and thin-layer chromatographic (TLC) technique. Analyses of purity and adulterants were performed with gas chromatography equipped with flame ionization detector (GC-FID). Additionally, smoke composition was analyzed by GC-mass spectrometry (MS), after samples burning. Samples showed different colors and forms, the majority of which is yellow (74.0%) or white (20.0%). Samples free of adulterants represented 76.3% of the total. Mean purity of the analyzed drug was 71.3%. Crack cocaine presented no correlations between macroscopic characteristics and purity. Smoke analysis showed compounds found also in the degradation of diesel and gasoline. Therefore, the drug marketed as crack cocaine in São Paulo has similar characteristics to coca paste. High purity can represent a greater risk of dependency and smoke compounds are possibly worsening drug health impact. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Particle Release Experiment (PRex) Final Report

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

Keillor, Martin E.; Arrigo, Leah M.; Detwiler, Rebecca S.

2014-09-30

An experiment to release radioactive particles representative of small-scale venting from an underground nuclear test was conducted to gather data in support of treaty verification and monitoring activities. For this experiment, a CO 2-driven “air cannon” was used to release La-140 at ambient temperatures. Lanthanum-140 was chosen to represent the fission fragments because of its short half-life and prominent gamma-ray emissions; the choice was also influenced by the successful production and use of La-140 with low levels of radioactive contaminants in a Defence Research and Development Canada Field Trial. The source was created through activation of high-purity natural lanthanum oxidemore » at the reactor of Washington State University, Pullman, Washington. Multiple varieties of witness plates and air samplers were laid in an irregular grid covering the area over which the plume was modeled to deposit. Aerial survey, a NaI(Tl) mobile spectrometer, and handheld and backpack instruments ranging from polyvinyl toluene to high-purity germanium were used to survey the plume. Additionally, three varieties of soil sampling were investigated. The relative sensitivity and utility of sampling and survey methods are discussed in the context of On-Site Inspection. The measurements and samples show a high degree of correlation and form a valuable set of test data.« less

Purification of optical imaging ligand-Cybesin by high-speed counter-current chromatography

PubMed Central

Ma, Zhiyong; Ma, Ying; Sun, Xilin; Ye, Yunpeng; Shen, Baozhong; Chen, Xiaoyuan; Ito, Yoichiro

2010-01-01

Fluorescent Cybesin (Cypate-Bombesin Peptide Analogue Conjugate) was synthesized from Indocyanine Green (ICG) and the bombesin receptor ligand as a contrast agent for detecting pancreas tumors. However, the LC–MS analysis indicated that the target compound was only a minor component in the reaction mixture. Since preparative HPLC can hardly separate such a small amount of the target compound directly from the original crude reaction mixture without a considerable adsorptive loss onto the solid support, high-speed counter-current chromatography (HSCCC) was used for purification since the method uses no solid support and promises high sample recovery. A suitable two-phase solvent system composed of hexane/ethyl acetate/methanol/methyl t.-butyl ether/acetonitrile/water) at a volume ratio of 1:1:1:4:4:7 was selected based on the partition coefficient of Cybesin (K ≈ 0.9) determined by LC–MS. The separation was performed in two steps using the same solvent system with lower aqueous mobile phase. From 400 mg of the crude reaction mixture the first separation yielded 7.7 mg of fractions containing the target compound at 12.8% purity, and in the second run 1 mg of Cybesin was obtained at purity of 94.0% with a sample recovery rate of over 95% based on the LC–MS Analysis. PMID:20933483

Electrochemical characteristics of needle coke refined by molten caustic leaching as an anode material for a lithium-ion battery

NASA Astrophysics Data System (ADS)

Kang, Hyeong-Gon; Park, Jong-Kwang; Han, Byoung-Sung; Lee, Haeseong

Needle coke, the remaining material after refining petroleum, is used as an anode of a lithium-ion secondary battery. Sulfur is separated from the needle coke to below 0.1 wt.% using the molten caustic leaching (MCL) method developed at the Korea Institute of Energy Research. The needle coke with high-purity is carbonized at various temperatures, namely 0, 500, 700 and 900 °C. The coke treated at 700 °C gives a first and second discharge capacity of more than 560 and 460 mAh g -1, respectively, between 0 and 2.0 V. By contrast, the first and second discharge capacity of untreated coke is over 420 and 340 mAh g -1, respectively, between 0.05 and 2.0 V.The first discharge capacity of 560 mAh g -1 is beyond the theoretical maximum capacity of 372 mAh g -1 for LiC 6. Though the cycle efficiency is not consistent, the needle coke heat-treated at 700 °C persistently maintains an efficiency of over 90% until the 50th cycle, except on the first cycle. This study demonstrates that the needle coke with high-purity could be a good candidate for an anode material in fabricating high-capacity lithium-ion secondary batteries.

Halophilic viruses with varying biochemical and biophysical properties are amenable to purification with asymmetrical flow field-flow fractionation.

PubMed

Eskelin, Katri; Lampi, Mirka; Meier, Florian; Moldenhauer, Evelin; Bamford, Dennis H; Oksanen, Hanna M

2017-11-01

Viruses come in various shapes and sizes, and a number of viruses originate from extremities, e.g. high salinity or elevated temperature. One challenge for studying extreme viruses is to find efficient purification conditions where viruses maintain their infectivity. Asymmetrical flow field-flow fractionation (AF4) is a gentle native chromatography-like technique for size-based separation. It does not have solid stationary phase and the mobile phase composition is readily adjustable according to the sample needs. Due to the high separation power of specimens up to 50 µm, AF4 is suitable for virus purification. Here, we applied AF4 for extremophilic viruses representing four morphotypes: lemon-shaped, tailed and tailless icosahedral, as well as pleomorphic enveloped. AF4 was applied to input samples of different purity: crude supernatants of infected cultures, polyethylene glycol-precipitated viruses and viruses purified by ultracentrifugation. All four virus morphotypes were successfully purified by AF4. AF4 purification of culture supernatants or polyethylene glycol-precipitated viruses yielded high recoveries, and the purities were comparable to those obtained by the multistep ultracentrifugation purification methods. In addition, we also demonstrate that AF4 is a rapid monitoring tool for virus production in slowly growing host cells living in extreme conditions.

Size and Purity Control of HPHT Nanodiamonds down to 1 nm

PubMed Central

2015-01-01

High-pressure high-temperature (HPHT) nanodiamonds originate from grinding of diamond microcrystals obtained by HPHT synthesis. Here we report on a simple two-step approach to obtain as small as 1.1 nm HPHT nanodiamonds of excellent purity and crystallinity, which are among the smallest artificially prepared nanodiamonds ever shown and characterized. Moreover we provide experimental evidence of diamond stability down to 1 nm. Controlled annealing at 450 °C in air leads to efficient purification from the nondiamond carbon (shells and dots), as evidenced by X-ray photoelectron spectroscopy, Raman spectroscopy, photoluminescence spectroscopy, and scanning transmission electron microscopy. Annealing at 500 °C promotes, besides of purification, also size reduction of nanodiamonds down to ∼1 nm. Comparably short (1 h) centrifugation of the nanodiamonds aqueous colloidal solution ensures separation of the sub-10 nm fraction. Calculations show that an asymmetry of Raman diamond peak of sub-10 nm HPHT nanodiamonds can be well explained by modified phonon confinement model when the actual particle size distribution is taken into account. In contrast, larger Raman peak asymmetry commonly observed in Raman spectra of detonation nanodiamonds is mainly attributed to defects rather than to the phonon confinement. Thus, the obtained characteristics reflect high material quality including nanoscale effects in sub-10 nm HPHT nanodiamonds prepared by the presented method. PMID:26691647

Carbothermal reduction of Ti-modified IRMOF-3: an adaptable synthetic method to support catalytic nanoparticles on carbon.

PubMed

Kim, Jongsik; McNamara, Nicholas D; Her, Theresa H; Hicks, Jason C

2013-11-13

This work describes a novel method for the preparation of titanium oxide nanoparticles supported on amorphous carbon with nanoporosity (Ti/NC) via the post-synthetic modification of a Zn-based MOF with an amine functionality, IRMOF-3, with titanium isopropoxide followed by its carbothermal pyrolysis. This material exhibited high purity, high surface area (>1000 m(2)/g), and a high dispersion of metal oxide nanoparticles while maintaining a small particle size (~4 nm). The material was shown to be a promising catalyst for oxidative desulfurization of diesel using dibenzothiophene as a model compound as it exhibited enhanced catalytic activity as compared with titanium oxide supported on activated carbon via the conventional incipient wetness impregnation method. The formation mechanism of Ti/NC was also proposed based on results obtained when the carbothermal reduction temperature was varied.

Purity assessment of recombinant human granulocyte colony-stimulating factor in finished drug product by capillary zone electrophoresis.

PubMed

Benković, Goran; Skrlin, Ana; Madić, Tomislav; Debeljak, Zeljko; Medić-Šarić, Marica

2014-09-01

Current methods for determination of impurities with different charge-to-volume ratio are limited especially in terms of sensitivity and precision. The main goal of this research was to establish a quantitative method for determination of impurities with charges differing from that of recombinant human granulocyte colony-stimulating factor (rhG-CSF, filgrastim) with superior precision and sensitivity compared to existing methods. A CZE method has been developed, optimized, and validated for a purity assessment of filgrastim in liquid pharmaceutical formulations. Optimal separation of filgrastim from the related impurities with different charges was achieved on a 50 μm id fused-silica capillary of a total length of 80.5 cm. A BGE that contains 100 mM phosphoric acid adjusted to pH 7.0 with triethanolamine was used. The applied voltage was 20 kV while the temperature was maintained at 25°C. UV detection was set to 200 nm. Method was validated in terms of selectivity/specificity, linearity, precision, LOD, LOQ, stability, and robustness. Linearity was observed in the concentration range of 6-600 μg/mL and the LOQ was determined to be 0.3% relative to the concentration of filgrastim of 0.6 mg/mL. Other validation parameters were also found to be acceptable; thus the method was successfully applied for a quantitative purity assessment of filgrastim in a finished drug product. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A purity monitor for the KEDR liquid krypton calorimeter

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

Evtushenko, P. N.; Kotov, K. Yu.; Maslennikov, A. L.

We present a purity monitor for the KEDR liquid krypton calorimeter. A new method is suggested based on the usage of a short pulse of a gas discharge as a source of ultraviolet radiation for the photoproduction of electrons in a drift cell of the monitor. This paper describes the design of the monitor, the results of experiments with gaseous and liquid krypton, as well as the experience of using the developed device in the process of krypton purification for the KEDR liquid krypton calorimeter.

METHOD OF TESTING THERMAL NEUTRON FISSIONABLE MATERIAL FOR PURITY

DOEpatents

Fermi, E.; Anderson, H.L.

1961-01-24

A process is given for determining the neutronic purity of fissionable material by the so-called shotgun test. The effect of a standard neutron absorber of known characteristics and amounts on a neutronic field also of known characteristics is measured and compared with the effect which the impurities derived from a known quantity of fissionable material has on the same neutronic field. The two readings are then made the basis of calculation from which the amount of impurities can be computed.

TIGRESS highly-segmented high-purity germanium clover detector

NASA Astrophysics Data System (ADS)

Scraggs, H. C.; Pearson, C. J.; Hackman, G.; Smith, M. B.; Austin, R. A. E.; Ball, G. C.; Boston, A. J.; Bricault, P.; Chakrawarthy, R. S.; Churchman, R.; Cowan, N.; Cronkhite, G.; Cunningham, E. S.; Drake, T. E.; Finlay, P.; Garrett, P. E.; Grinyer, G. F.; Hyland, B.; Jones, B.; Leslie, J. R.; Martin, J.-P.; Morris, D.; Morton, A. C.; Phillips, A. A.; Sarazin, F.; Schumaker, M. A.; Svensson, C. E.; Valiente-Dobón, J. J.; Waddington, J. C.; Watters, L. M.; Zimmerman, L.

2005-05-01

The TRIUMF-ISAC Gamma-Ray Escape-Suppressed Spectrometer (TIGRESS) will consist of twelve units of four high-purity germanium (HPGe) crystals in a common cryostat. The outer contacts of each crystal will be divided into four quadrants and two lateral segments for a total of eight outer contacts. The performance of a prototype HPGe four-crystal unit has been investigated. Integrated noise spectra for all contacts were measured. Energy resolutions, relative efficiencies for both individual crystals and for the entire unit, and peak-to-total ratios were measured with point-like sources. Position-dependent performance was measured by moving a collimated source across the face of the detector.

Rapid and Convenient Separation of Chitooligosaccharides by Ion-Exchange Chromatography

NASA Astrophysics Data System (ADS)

Wu, Yuxiao; Lu, Wei-Peng; Wang, Jianing; Gao, Yunhua; Guo, Yanchuan

2017-12-01

Pervious methods for separation of highly purified chitooligosaccharides was time-consuming and labor-intensive, which limited the large-scale production. This study developed a convenient ion-exchange chromatography using the ÄKTA™ avant 150 chromatographic system. Five fractions were automatically collected under detecting the absorption at 210 nm. The fractions were analyzed by high-performance liquid chromatography. It proved that they primarily comprised chitobiose, chitotriose, chitotetraose, chitopentaose, and chitohexaose, respectively, with chromatographic purities over 90%. The separation process was rapid, convenient and could be monitored on-line, which would be benefit for the mass production of chitooligosaccharides.