Sample records for high purity samples

  1. Application of Digital Image Analysis to Determine Pancreatic Islet Mass and Purity in Clinical Islet Isolation and Transplantation

    PubMed Central

    Wang, Ling-jia; Kissler, Hermann J; Wang, Xiaojun; Cochet, Olivia; Krzystyniak, Adam; Misawa, Ryosuke; Golab, Karolina; Tibudan, Martin; Grzanka, Jakub; Savari, Omid; Grose, Randall; Kaufman, Dixon B; Millis, Michael; Witkowski, Piotr

    2015-01-01

    Pancreatic islet mass, represented by islet equivalent (IEQ), is the most important parameter in decision making for clinical islet transplantation. To obtain IEQ, the sample of islets is routinely counted manually under a microscope and discarded thereafter. Islet purity, another parameter in islet processing, is routinely acquired by estimation only. In this study, we validated our digital image analysis (DIA) system developed using the software of Image Pro Plus for islet mass and purity assessment. Application of the DIA allows to better comply with current good manufacturing practice (cGMP) standards. Human islet samples were captured as calibrated digital images for the permanent record. Five trained technicians participated in determination of IEQ and purity by manual counting method and DIA. IEQ count showed statistically significant correlations between the manual method and DIA in all sample comparisons (r >0.819 and p < 0.0001). Statistically significant difference in IEQ between both methods was found only in High purity 100μL sample group (p = 0.029). As far as purity determination, statistically significant differences between manual assessment and DIA measurement was found in High and Low purity 100μL samples (p<0.005), In addition, islet particle number (IPN) and the IEQ/IPN ratio did not differ statistically between manual counting method and DIA. In conclusion, the DIA used in this study is a reliable technique in determination of IEQ and purity. Islet sample preserved as a digital image and results produced by DIA can be permanently stored for verification, technical training and islet information exchange between different islet centers. Therefore, DIA complies better with cGMP requirements than the manual counting method. We propose DIA as a quality control tool to supplement the established standard manual method for islets counting and purity estimation. PMID:24806436

  2. 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.

  3. Frequency optimization in the eddy current test for high purity niobium

    NASA Astrophysics Data System (ADS)

    Joung, Mijoung; Jung, Yoochul; Kim, Hyungjin

    2017-01-01

    The eddy current test (ECT) is frequently used as a non-destructive method to check for the defects of high purity niobium (RRR300, Residual Resistivity Ratio) in a superconducting radio frequency (SRF) cavity. Determining an optimal frequency corresponding to specific material properties and probe specification is a very important step. The ECT experiments for high purity Nb were performed to determine the optimal frequency using the standard sample of high purity Nb having artificial defects. The target depth was considered with the treatment step that the niobium receives as the SRF cavity material. The results were analysed via the selectivity that led to a specific result, depending on the size of the defects. According to the results, the optimal frequency was determined to be 200 kHz, and a few features of the ECT for the high purity Nb were observed.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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

  10. 7 CFR 201.52 - Noxious-weed seeds.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... the bulk examined for noxious-weed seeds need not be noted: 1/2-gram purity working sample, 16 or more seeds; 1-gram purity working sample, 23 or more seeds; 2-gram purity working sample or larger, 30 or...

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. Precipitation of hydrides in high purity niobium after different treatments

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

    Barkov, F.; Romanenko, A.; Trenikhina, Y.

    Precipitation of lossy non-superconducting niobium hydrides represents a known problem for high purity niobium in superconducting applications. Using cryogenic optical and laser confocal scanning microscopy we have directly observed surface precipitation and evolution of niobium hydrides in samples after different treatments used for superconducting RF cavities for particle acceleration. Precipitation is shown to occur throughout the sample volume, and the growth of hydrides is well described by the fast diffusion-controlled process in which almost all hydrogen is precipitated atmore » $T=140$~K within $$\\sim30$$~min. 120$$^{\\circ}$$C baking and mechanical deformation are found to affect hydride precipitation through their influence on the number of nucleation and trapping centers.« less

  17. Results of an international drug testing service for cryptomarket users.

    PubMed

    Caudevilla, Fernando; Ventura, Mireia; Fornís, Iván; Barratt, Monica J; Vidal, Claudio; Lladanosa, Cristina Gil; Quintana, Pol; Muñoz, Ana; Calzada, Nuria

    2016-09-01

    User surveys indicate that expectations of higher drug purity are a key reason for cryptomarket use. In 2014-2015, Spain's NGO Energy Control conducted a 1-year pilot project to provide a testing service to cryptomarket drug users using the Transnational European Drug Information (TEDI) guidelines. In this paper, we present content and purity data from the trial. 219 samples were analyzed by gas chromatography associated with mass spectrometry (GC/MS). Users were asked to report what substance they allegedly purchased. 40 different advertised substances were reported, although 77.6% were common recreational drugs (cocaine, MDMA, amphetamines, LSD, ketamine, cannabis). In 200 samples (91.3%), the main result of analysis matched the advertised substance. Where the advertised compound was detected, purity levels (m±SD) were: cocaine 71.6±19.4%; MDMA (crystal) 88.3±1.4%; MDMA (pills) 133.3±38.4mg; Amphetamine (speed) 51.3±33.9%; LSD 123.6±40.5μg; Cannabis resin THC: 16.5±7.5% CBD: 3.4±1.5%; Ketamine 71.3±38.4%. 39.8% of cocaine samples contained the adulterant levamisole (11.6±8%). No adulterants were found in MDMA and LSD samples. The largest collection of test results from drug samples delivered from cryptomarkets are reported in this study. Most substances contained the advertised ingredient and most samples were of high purity. The representativeness of these results is unknown. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. 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.

  19. 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.

  20. 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.

  1. Characterization of ingot material for SRF cavity production

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

    Mondal, Jayanta; Ciovati, Gianluigi; Kneisel, Peter K.

    In recent years, large-grain/single-crystal niobium has become a viable alternative to the standard fine grain (ASTM grain size>6), high purity (RRR ) niobium for the fabrication of high-performance SRF cavities for particle accelerators. In this contribution we present the results of a systematic study of the superconducting properties of samples obtained from four Niobium ingots (from CBMM, Brazil) of different purity. Measurements of bulk magnetization, surface pinning, critical temperature and thermal conductivity have been carried out on the samples subjected to different surface treatments such as buffered chemical polishing (BCP), 6000C heat treatment, and low temperature baking (LTB). A correlationmore » has been established between the LTB and the ratio . In addition, the phonon peak in the thermal conductivity data is suppressed by the presence of trapped magnetic vortices in the samples.« less

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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

  7. Hydrogen, lithium, and lithium hydride production

    DOEpatents

    Brown, Sam W; Spencer, Larry S; Phillips, Michael R; Powell, G. Louis; Campbell, Peggy J

    2014-03-25

    A method of producing high purity lithium metal is provided, where gaseous-phase lithium metal is extracted from lithium hydride and condensed to form solid high purity lithium metal. The high purity lithium metal may be hydrided to provide high purity lithium hydride.

  8. A combined arc-melting and tilt-casting furnace for the manufacture of high-purity bulk metallic glass materials.

    PubMed

    Soinila, E; Pihlajamäki, T; Bossuyt, S; Hänninen, H

    2011-07-01

    An arc-melting furnace which includes a tilt-casting facility was designed and built, for the purpose of producing bulk metallic glass specimens. Tilt-casting was chosen because reportedly, in combination with high-purity processing, it produces the best fatigue endurance in Zr-based bulk metallic glasses. Incorporating the alloying and casting facilities in a single piece of equipment reduces the amount of laboratory space and capital investment needed. Eliminating the sample transfer step from the production process also saves time and reduces sample contamination. This is important because the glass forming ability in many alloy systems, such as Zr-based glass-forming alloys, deteriorates rapidly with increasing oxygen content of the specimen. The challenge was to create a versatile instrument, in which high purity conditions can be maintained throughout the process, even when melting alloys with high affinity for oxygen. Therefore, the design provides a high-vacuum chamber to be filled with a low-oxygen inert atmosphere, and takes special care to keep the system hermetically sealed throughout the process. In particular, movements of the arc-melting electrode and sample manipulator arm are accommodated by deformable metal bellows, rather than sliding O-ring seals, and the whole furnace is tilted for tilt-casting. This performance of the furnace is demonstrated by alloying and casting Zr(55)Cu(30)Al(10)Ni(5) directly into rods up to ø 10 mm which are verified to be amorphous by x-ray diffraction and differential scanning calorimetry, and to exhibit locally ductile fracture at liquid nitrogen temperature.

  9. Spallation studies on shock loaded uranium

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

    Tonks, D.L.; Hixson, R.; Gustavsen, R.L.

    1997-12-31

    Uranium samples at two different purity levels were used for spall strength measurements at three different stress levels. A 50 mm single-stage gas-gun was used to produce planar impact conditions using Z-cut quartz impactors. Samples of depleted uranium were taken from very high purity material and from material that had 300 ppm of carbon added. A pair of shots was done for each impact strength, one member of the pair with VISAR diagnostics and the second with soft recovery for metallographical examination. A series of increasing final stress states were chosen to effectively freeze the microstructural damage at three placesmore » in the development to full spall separation. This allowed determination of the dependence of spall mechanisms on stress level and sample purity. This report will discuss both the results of the metallurgical examination of soft recovered samples and the modeling of the free surface VISAR data. The micrographs taken from the recovered samples show brittle cracking as the spallation failure mechanism. Deformation induced twins are plentiful and obviously play a role in the spallation process. The twins are produced in the initial shock loading and, so, are present already before the fracture process begins. The 1 d characteristics code CHARADE has been used to model the free surface VISAR data.« less

  10. 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.

  11. Shock and Microstructural Characterization of the α-ω Phase Transition in Titanium Crystals

    NASA Astrophysics Data System (ADS)

    Morrow, Benjamin M.; Rigg, Paulo A.; Jones, David R.; Addessio, Francis L.; Trujillo, Carl P.; Saavedra, Ramon A.; Martinez, Daniel T.; Cerreta, Ellen K.

    2017-12-01

    A multicrystal comprised of a small number of large crystals of high-purity titanium and a [0001] oriented high-purity single crystal titanium sample were shock loaded using gas gun plate impact experiments. Tests were performed at stresses above the α {-}ω phase transition stress (for high-purity polycrystalline specimens) to observe the behavior of oriented crystals under similar conditions. Post-mortem characterization of the shocked microstructure was conducted on the single crystal sample to measure textures, and quantify phases and twinning. The apparent activation of plastic and transformation mechanisms was dependent upon crystal orientation. Specifically, the [0001] crystal showed a higher Hugoniot elastic limit than the [10\\bar{1}0] or [3\\bar{1}\\bar{4}4] orientations. The slope of velocity as a function of time was lower in the [0001] orientation than the other orientations during plastic deformation, indicating sluggish transformation kinetics for the α to ω phase transition for the [0001] oriented crystal. Microtexture measurements of a recovered [0001] oriented single crystal revealed the presence of retained ω phase after unloading, with orientations of the constituent phase fractions indicative of the forward α → ω transition, rather than the reverse ω → α transition, suggesting that the material never achieved a state of 100% ω phase.

  12. Linalool from Lippia alba: study of the reproducibility of the essential oil profile and the enantiomeric purity.

    PubMed

    Siani, Antonio C; Tappin, Marcelo R R; Ramos, Mônica F S; Mazzei, José L; Ramos, Maria Conceição K V; De Aquino Neto, Francisco R; Frighetto, Nélson

    2002-06-05

    A new chemotype of the aromatic Verbenaceae species Lippia alba Mill. N. E. Br. from southeastern Brazil has recently been shown to have a high content of linalool in the leaf essential oil. Vegetative propagation of this chemotype was conducted at six different locations in Brazil, and the variation of the content and the optical purity of linalool in the oils were verified. Yields (0.6-0.9%, hydrodistillation), chemical composition, linalool content, and optical purity of the oils from all the plants were compared, using GC-FID, GC-MS, chiral chromatography, and retention index calculation. No plant exceeded the matrix in linalool content (46.5 to 90.7%), and the chemical profile of the oils was the same for all the samples. Purification of linalool to a content close to 100% was effected by vacuum distillation of the crude oil. Chiral analysis showed exclusively the presence of S-linalool in all the crude oils and in the distilled samples.

  13. Long-term purity assessment in succinonitrile

    NASA Astrophysics Data System (ADS)

    Rubinstein, E. R.; Tirmizi, S. H.; Glicksman, M. E.

    1990-11-01

    Container materials for crystal growth chambers must be carefully selected in order to prevent sample contamination. To address the issue of contamination, high purity SCN was exposed to a variety of potential chamber construction materials, e.g., metal alloys, soldering materials, and sealants, at a temperature approximately 25 K above the melting point of SCN (58°C), over periods of up to one year. Acceptability, or lack thereof, of candidate chamber materials was determined by performing periodic melting point checks of the exposed samples. Those materials which did not measurably affect the melting point of SCN over a one-year period were considered to be chemically compatible and therefore eligible for use in constructing the flight chamber. A growth chamber constructed from compatible materials (304 SS and borosilicate glass) was filled with pure SCN. A thermistor probe placed within the chamber permitted in situ measurement of the melting point and, indirectly, of the purity of the SCN. Melting point plateaus were then determined, to assess the actual chamber performance.

  14. Heterogeneous nucleation in a glass-forming alloy

    NASA Astrophysics Data System (ADS)

    Wall, J. J.; Liu, C. T.; Rhim, W.-K.; Li, J. J. Z.; Liaw, P. K.; Choo, H.; Johnson, W. L.

    2008-06-01

    Nucleation in the undercooled liquid state in the bulk metallic glass-forming composition Zr52.5Cu17.9Ni14.6Al10Ti5 (VIT-105), produced using high purity (PA) and commercial purity (CA) raw materials was investigated using electrostatic levitation and ex situ neutron diffraction. The CA material was observed to have a lower density than the PA sample and crystallized at relatively shallow undercooling. The densities of the samples at temperatures above the solidus showed an oxygen-dependent hysteresis associated with the state change, indicating the presence of oxygen-stabilized intermetallics. The PA alloy exhibited three distinct crystallization modes dependent on the thermal history of the melt, one of which showed a net volume expansion.

  15. 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

  16. 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.

  17. Anomalous B-field Dependence of Spin-flip Time in High Purity InP

    NASA Astrophysics Data System (ADS)

    Linpeng, Xiayu; Karin, Todd; Barbour, Russell; Glazov, Mikhail; Fu, Kai-Mei

    2015-03-01

    We observe an anomalous B-field dependence of the spin-flip time (T1) of electrons bound to shallow donors which cannot be explained by current spin-relaxation theories. We conduct resonant pump-probe measurements in high-purity InP from the low to high magnetic field regimes, with a maximum T1 (400 μs) observed near the turning point gμB B ~=kB T . At low B, the T1 dependence on B is consistent with an electron correlation time (τc) in the tens of nanoseconds. The physical mechanism for the short τc in this high-purity sample (n ~= 2 ×1014 cm-3) is unclear, but a strong temperature (T) dependence indicates T1 can be further increased by lowering T below the 1.5 K experimental temperature. At high B, a B-3 dependence is observed, in contrast to the expected B-5 predicted by single-phonon spin-orbit mediated interactions. An understanding of the anomalous B-field dependence is expected to elucidate the effect of electron transport (low-field) and phonons (high-field) on T1 for shallow donors, which is of interest for both ensemble and single-spin quantum information applications. This material is based upon work supported by the National Science Foundation under Grant No. 1150647, DGE-0718124 and DGE-1256082. InP samples were graciously provided by Simon Watkins at Simon Fraser University.

  18. Shrink-induced sorting using integrated nanoscale magnetic traps.

    PubMed

    Nawarathna, Dharmakeerthi; Norouzi, Nazila; McLane, Jolie; Sharma, Himanshu; Sharac, Nicholas; Grant, Ted; Chen, Aaron; Strayer, Scott; Ragan, Regina; Khine, Michelle

    2013-02-11

    We present a plastic microfluidic device with integrated nanoscale magnetic traps (NSMTs) that separates magnetic from non-magnetic beads with high purity and throughput, and unprecedented enrichments. Numerical simulations indicate significantly higher localized magnetic field gradients than previously reported. We demonstrated >20 000-fold enrichment for 0.001% magnetic bead mixtures. Since we achieve high purity at all flow-rates tested, this is a robust, rapid, portable, and simple solution to sort target species from small volumes amenable for point-of-care applications. We used the NSMT in a 96 well format to extract DNA from small sample volumes for quantitative polymerase chain reaction (qPCR).

  19. Corrosion behavior of surface films on boron-implanted high purity iron and stainless steels

    NASA Technical Reports Server (NTRS)

    Kim, H. J.; Carter, W. B.; Hochman, R. F.; Meletis, E. I.

    1985-01-01

    Boron (dose, 2 x 10 to the 17th ions/sq cm) was implanted into high purity iron, AISI 316 austenitic stainless steel, and AISI 440C martensitic stainless steel, at 40 keV. The film structure of implanted samples was examined and characterized by contrast and diffraction analyses utilizing transmission electron microscopy. The effect of B(+) ion implantation on the corrosion behavior was studied using the potentiodynamic polarization technique. Tests were performed in deaerated 1 N H2SO4 and 0.1 M NaCl solutions. Scanning electron microscopy was used to examine the morphology of the corroded surfaces after testing.

  20. Effect of Electropolishing and Low-Temperature Baking on the Superconducting Properties of Large-Grain Niobium

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

    A. S. Dhavale, G. Ciovati, G. R. Myneni

    Measurements of superconducting properties such as bulk and surface critical fields and thermal conductivity have been carried out in the temperature range from 2 K to 8 K on large-grain samples of different purity and on a high-purity fine-grain sample, for comparison. The samples were treated by electropolishing and low temperature baking (120° C, 48 h). While the residual resistivity ratio changed by a factor of ~3 among the samples, no significant variation was found in their superconducting properties. The onset field for flux penetration at 2 K, Hffp, measured within a ~30 µm depth from the surface, was ~160more » mT, close to the bulk value. The baking effect was mainly to increase the field range up to which a coherent superconducting phase persists on the surface, above the upper critical field.« less

  1. 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.

  2. 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.

  3. 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).

  4. 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.

  5. [Purity Detection Model Update of Maize Seeds Based on Active Learning].

    PubMed

    Tang, Jin-ya; Huang, Min; Zhu, Qi-bing

    2015-08-01

    Seed purity reflects the degree of seed varieties in typical consistent characteristics, so it is great important to improve the reliability and accuracy of seed purity detection to guarantee the quality of seeds. Hyperspectral imaging can reflect the internal and external characteristics of seeds at the same time, which has been widely used in nondestructive detection of agricultural products. The essence of nondestructive detection of agricultural products using hyperspectral imaging technique is to establish the mathematical model between the spectral information and the quality of agricultural products. Since the spectral information is easily affected by the sample growth environment, the stability and generalization of model would weaken when the test samples harvested from different origin and year. Active learning algorithm was investigated to add representative samples to expand the sample space for the original model, so as to implement the rapid update of the model's ability. Random selection (RS) and Kennard-Stone algorithm (KS) were performed to compare the model update effect with active learning algorithm. The experimental results indicated that in the division of different proportion of sample set (1:1, 3:1, 4:1), the updated purity detection model for maize seeds from 2010 year which was added 40 samples selected by active learning algorithm from 2011 year increased the prediction accuracy for 2011 new samples from 47%, 33.75%, 49% to 98.89%, 98.33%, 98.33%. For the updated purity detection model of 2011 year, its prediction accuracy for 2010 new samples increased by 50.83%, 54.58%, 53.75% to 94.57%, 94.02%, 94.57% after adding 56 new samples from 2010 year. Meanwhile the effect of model updated by active learning algorithm was better than that of RS and KS. Therefore, the update for purity detection model of maize seeds is feasible by active learning algorithm.

  6. Measurements of Dendritic Growth Velocities in Undercooled Melts of Pure Nickel Under Static Magnetic Fields

    NASA Technical Reports Server (NTRS)

    Gao, Jianrong; Zhang, Zongning; Zhang, Yingjie

    2012-01-01

    Dendritic growth velocities in undercooled melts of pure Ni have been intensively studied over the past fifty years. However, the literature data are at marked variance with the prediction of the widely accepted model for rapid dendritic growth both at small and at large undercoolings. In the present work, bulk melts of pure Ni samples of high purity were undercooled by glass fluxing treatment under a static magnetic field. The recalescence processes of the samples at different undercoolings were recorded using a high-speed camera, and were modeled using a software to determine the dendritic growth velocities. The present data confirmed the effect of melt flow on dendritic growth velocities at undercoolings below 100 K. A comparison of the present data with previous measurements on a lower purity material suggested an effect of impurities on dendritic growth velocities at undercoolings larger than 200 K as well.

  7. Electrical conductivity of high-purity germanium crystals at low temperature

    NASA Astrophysics Data System (ADS)

    Yang, Gang; Kooi, Kyler; Wang, Guojian; Mei, Hao; Li, Yangyang; Mei, Dongming

    2018-05-01

    The temperature dependence of electrical conductivity of single-crystal and polycrystalline high-purity germanium (HPGe) samples has been investigated in the temperature range from 7 to 100 K. The conductivity versus inverse of temperature curves for three single-crystal samples consist of two distinct temperature ranges: a high-temperature range where the conductivity increases to a maximum with decreasing temperature, and a low-temperature range where the conductivity continues decreasing slowly with decreasing temperature. In contrast, the conductivity versus inverse of temperature curves for three polycrystalline samples, in addition to a high- and a low-temperature range where a similar conductive behavior is shown, have a medium-temperature range where the conductivity decreases dramatically with decreasing temperature. The turning point temperature ({Tm}) which corresponds to the maximum values of the conductivity on the conductivity versus inverse of temperature curves are higher for the polycrystalline samples than for the single-crystal samples. Additionally, the net carrier concentrations of all samples have been calculated based on measured conductivity in the whole measurement temperature range. The calculated results show that the ionized carrier concentration increases with increasing temperature due to thermal excitation, but it reaches saturation around 40 K for the single-crystal samples and 70 K for the polycrystalline samples. All these differences between the single-crystal samples and the polycrystalline samples could be attributed to trapping and scattering effects of the grain boundaries on the charge carriers. The relevant physical models have been proposed to explain these differences in the conductive behaviors between two kinds of samples.

  8. Purity, adulteration and price of drugs bought on-line versus off-line in the Netherlands.

    PubMed

    van der Gouwe, Daan; Brunt, Tibor M; van Laar, Margriet; van der Pol, Peggy

    2017-04-01

    On-line drug markets flourish and consumers have high expectations of on-line quality and drug value. The aim of this study was to (i) describe on-line drug purchases and (ii) compare on-line with off-line purchased drugs regarding purity, adulteration and price. Comparison of laboratory analyses of 32 663 drug consumer samples (stimulants and hallucinogens) purchased between January 2013 and January 2016, 928 of which were bought on-line. The Netherlands. Primary outcome measures were (i) the percentage of samples purchased on-line and (ii) the chemical purity of powders (or dosage per tablet); adulteration; and the price per gram, blotter or tablet of drugs bought on-line compared with drugs bought off-line. The proportion of drug samples purchased on-line increased from 1.4% in 2013 to 4.1% in 2015. The frequency varied widely, from a maximum of 6% for controlled, traditional substances [ecstasy tablets, 3,4-methylenedioxy-methamphetamine (MDMA) powder, amphetamine powder, cocaine powder, 4-bromo-2,5-dimethoxyphenethylamine (2C-B) and lysergic acid diethylamide (LSD)] to more than a third for new psychoactive substances (NPS) [4-fluoroamphetamine (4-FA), 5/6-(2-aminopropyl)benzofuran (5/6-APB) and methoxetamine (MXE)]. There were no large differences in drug purity, yet small but statistically significant differences were found for 4-FA (on-line 59% versus off-line 52% purity for 4-FA on average, P = 0.001), MDMA powders (45 versus 61% purity for MDMA, P = 0.02), 2C-B tablets (21 versus 10 mg 2C-B/tablet dosage, P = 0.49) and ecstasy tablets (131 versus 121 mg MDMA/tablet dosage, P = 0.05). The proportion of adulterated samples purchased on-line and off-line did not differ, except for 4-FA powder, being less adulterated on-line (χ 2  = 8.3; P < 0.02). Drug prices were mainly higher on-line, ranging for various drugs from 10 to 23% higher than that of drugs purchased off-line (six of 10 substances: P < 0.05). Dutch drug users increasingly purchase drugs on-line: new psychoactive substances in particular. Purity and adulteration do not vary considerably between drugs purchased on-line and off-line for most substances, while on-line prices are mostly higher than off-line prices. © 2016 Society for the Study of Addiction.

  9. 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.

  10. Boson Sampling with Single-Photon Fock States from a Bright Solid-State Source.

    PubMed

    Loredo, J C; Broome, M A; Hilaire, P; Gazzano, O; Sagnes, I; Lemaitre, A; Almeida, M P; Senellart, P; White, A G

    2017-03-31

    A boson-sampling device is a quantum machine expected to perform tasks intractable for a classical computer, yet requiring minimal nonclassical resources as compared to full-scale quantum computers. Photonic implementations to date employed sources based on inefficient processes that only simulate heralded single-photon statistics when strongly reducing emission probabilities. Boson sampling with only single-photon input has thus never been realized. Here, we report on a boson-sampling device operated with a bright solid-state source of single-photon Fock states with high photon-number purity: the emission from an efficient and deterministic quantum dot-micropillar system is demultiplexed into three partially indistinguishable single photons, with a single-photon purity 1-g^{(2)}(0) of 0.990±0.001, interfering in a linear optics network. Our demultiplexed source is between 1 and 2 orders of magnitude more efficient than current heralded multiphoton sources based on spontaneous parametric down-conversion, allowing us to complete the boson-sampling experiment faster than previous equivalent implementations.

  11. 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.

  12. 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.

  13. 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.

  14. GIS-NaP1 zeolite microspheres as potential water adsorption material: Influence of initial silica concentration on adsorptive and physical/topological properties

    PubMed Central

    Sharma, Pankaj; Song, Ju-Sub; Han, Moon Hee; Cho, Churl-Hee

    2016-01-01

    GIS-NaP1 zeolite samples were synthesized using seven different Si/Al ratios (5–11) of the hydrothermal reaction mixtures having chemical composition Al2O3:xSiO2:14Na2O:840H2O to study the impact of Si/Al molar ratio on the water vapour adsorption potential, phase purity, morphology and crystal size of as-synthesized GIS-NaP1 zeolite crystals. The X-ray diffraction (XRD) observations reveal that Si/Al ratio does not affect the phase purity of GIS-NaP1 zeolite samples as high purity GIS-NaP1 zeolite crystals were obtained from all Si/Al ratios. Contrary, Si/Al ratios have remarkable effect on the morphology, crystal size and porosity of GIS-NaP1 zeolite microspheres. Transmission electron microscopy (TEM) evaluations of individual GIS-NaP1 zeolite microsphere demonstrate the characteristic changes in the packaging/arrangement, shape and size of primary nano crystallites. Textural characterisation using water vapour adsorption/desorption, and nitrogen adsorption/desorption data of as-synthesized GIS-NaP1 zeolite predicts the existence of mix-pores i.e., microporous as well as mesoporous character. High water storage capacity 1727.5 cm3 g−1 (138.9 wt.%) has been found for as-synthesized GIS-NaP1 zeolite microsphere samples during water vapour adsorption studies. Further, the total water adsorption capacity values for P6 (1299.4 mg g−1) and P7 (1388.8 mg g−1) samples reveal that these two particular samples can absorb even more water than their own weights. PMID:26964638

  15. GIS-NaP1 zeolite microspheres as potential water adsorption material: Influence of initial silica concentration on adsorptive and physical/topological properties.

    PubMed

    Sharma, Pankaj; Song, Ju-Sub; Han, Moon Hee; Cho, Churl-Hee

    2016-03-11

    GIS-NaP1 zeolite samples were synthesized using seven different Si/Al ratios (5-11) of the hydrothermal reaction mixtures having chemical composition Al2O3:xSiO2:14Na2O:840H2O to study the impact of Si/Al molar ratio on the water vapour adsorption potential, phase purity, morphology and crystal size of as-synthesized GIS-NaP1 zeolite crystals. The X-ray diffraction (XRD) observations reveal that Si/Al ratio does not affect the phase purity of GIS-NaP1 zeolite samples as high purity GIS-NaP1 zeolite crystals were obtained from all Si/Al ratios. Contrary, Si/Al ratios have remarkable effect on the morphology, crystal size and porosity of GIS-NaP1 zeolite microspheres. Transmission electron microscopy (TEM) evaluations of individual GIS-NaP1 zeolite microsphere demonstrate the characteristic changes in the packaging/arrangement, shape and size of primary nano crystallites. Textural characterisation using water vapour adsorption/desorption, and nitrogen adsorption/desorption data of as-synthesized GIS-NaP1 zeolite predicts the existence of mix-pores i.e., microporous as well as mesoporous character. High water storage capacity 1727.5 cm(3) g(-1) (138.9 wt.%) has been found for as-synthesized GIS-NaP1 zeolite microsphere samples during water vapour adsorption studies. Further, the total water adsorption capacity values for P6 (1299.4 mg g(-1)) and P7 (1388.8 mg g(-1)) samples reveal that these two particular samples can absorb even more water than their own weights.

  16. Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

    PubMed

    Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

    2017-05-15

    A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. 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.

  18. 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

  19. Elution-extrusion counter-current chromatography for the separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix.

    PubMed

    Chu, Chu; Zhang, Shidi; Tong, Shengqiang; Li, Xingnuo; Li, Qingyong; Yan, Jizhong

    2015-09-01

    In this work, a simple and efficient protocol for the rapid separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix was developed by combining macroporous resin and elution-extrusion counter-current chromatography. The crude extract was firstly subjected to a D101 macroporous resin column eluted with water and a series of different concentrations of ethanol. Then, effluents of 30 and 95% ethanol were collected as sample 1 and sample 2 for further counter-current chromatography purification. Finally, a pair of isomers, 96 mg of compound 1 and 48 mg of compound 2 with purities of 91.1 and 96.2%, respectively, was isolated from 200 mg of sample 1. The other pair of isomers, 14 mg of compound 3 and 8 mg of compound 4 with purities of 93.6 and 88.9%, respectively, was isolated from 48 mg of sample 2. Their purities were analyzed by high-performance liquid chromatography, and their chemical structures were identified by mass spectrometry and (1) H NMR spectroscopy. Compared to a normal counter-current chromatography separation, the separation time and solvent consumption of elution-extrusion counter-current chromatography were reduced while the resolutions were still good. The established protocol is promising for the separation of natural products with great disparity of content in herbal medicines. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Heterogeneous nucleation in a glass-forming alloy

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

    Wall, J. J.; Liu, Chain T; Rhim, W. K.

    Nucleation in the undercooled liquid state in the bulk metallic glass-forming composition Zr{sub 52.5}Cu{sub 17.9}Ni{sub 14.6}Al{sub 10}Ti{sub 5} (VIT-105), produced using high purity (PA) and commercial purity (CA) raw materials was investigated using electrostatic levitation and ex situ neutron diffraction. The CA material was observed to have a lower density than the PA sample and crystallized at relatively shallow undercooling. The densities of the samples at temperatures above the solidus showed an oxygen-dependent hysteresis associated with the state change, indicating the presence of oxygen-stabilized intermetallics. The PA alloy exhibited three distinct crystallization modes dependent on the thermal history of themore » melt, one of which showed a net volume expansion.« less

  1. 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

  2. Grain Refining and Microstructural Modification during Solidification.

    DTIC Science & Technology

    1983-10-01

    was found to be insensitive to the iron concentration in the samples solidified in the levitated state but not in samples quenched from the liquid . The... liquid . The preliminary * results with niobium additions indicate that no appreciable grain refinement * is achieved when the samples are levitated in an...to the critical examination of the Cr-Ni phase diagram, by using high purity starting materials, and a containerless electromagnetic levitation

  3. 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.

  4. 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.

  5. Experimental study of UC polycrystals in the prospect of improving the as-fabricated sample purity

    NASA Astrophysics Data System (ADS)

    Raveu, Gaëlle; Martin, Guillaume; Fiquet, Olivier; Garcia, Philippe; Carlot, Gaëlle; Palancher, Hervé; Bonnin, Anne; Khodja, Hicham; Raepsaet, Caroline; Sauvage, Thierry; Barthe, Marie-France

    2014-12-01

    Uranium and plutonium carbides are candidate fuels for Generation IV nuclear reactors. This study is focused on the characterization of uranium monocarbide samples. The successive fabrication steps were carried out under atmospheres containing low oxygen and moisture concentrations (typically less than 100 ppm) but sample transfers occurred in air. Six samples were sliced from four pellets elaborated by carbothermic reaction under vacuum. Little presence of UC2 is expected in these samples. The α-UC2 phase was indeed detected within one of these UC samples during an XRD experiment performed with synchrotron radiation. Moreover, oxygen content at the surface of these samples was depth profiled using a recently developed nuclear reaction analysis method. Large oxygen concentrations were measured in the first micron below the sample surface and particularly in the first 100-150 nm. UC2 inclusions were found to be more oxidized than the surrounding matrix. This work points out to the fact that more care must be given at each step of UC fabrication since the material readily reacts with oxygen and moisture. A new glovebox facility using a highly purified atmosphere is currently being built in order to obtain single phase UC samples of better purity.

  6. Methodology Used for Gas Analysis and Control of Trace Chemical Contaminants at a Hyperbaric Facility. 1. Gas Sampling

    DTIC Science & Technology

    1988-12-01

    made using a gas sampling valve. All instruments were calibrated using gravimetric standards certified to t 1-2% relative of stated value ( Air Products and Chemicals , Inc ., Allentown...cannister - 985410 7. High Purity Gas Cylinder Regulators - several sources Air Products and Chemicals , Inc . P.O. Box 1536 Washington, DC 20013 (301

  7. 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.

  8. 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).

  9. High temperature (1200 C) ceramic-to-metal seal development

    NASA Technical Reports Server (NTRS)

    Mckisson, R. L.; Ervin, G., Jr.

    1972-01-01

    Two phases have been completed, of a program whose ultimate objective is the development of an alkali metal resistant, thermal shock resistant, leak-tight, and neutron radiation resistant ceramic-to-metal seal capable of operation at 1200 C for three to five years. The first phase involved the screening of platinum-base, vanadium-base and vanadium-niobium base brazes for the joining of Cb-1Zr or T-111 alloys to high purity alumina. The second phase involved studies of the performance of sealed capsule samples during 5000-hour aging tests at 800, 1000, and 1200 C in high vacuum. Sealed capsules which were made using pure vanadium braze, and were brazed at 1850 C for one minute, survived 64 thermal cycles to 1200 C at the heating/cooling rate of 100 C/minute. Vanadium braze samples survived 5000-hour aging tests at 800, 1000, and 1200 C. One thermally cycled sample survived a subsequent 5000-hour aging period at 1000 C, but another, at 1200 C, did not survive. It was concluded that a pure vanadium braze used to bond high purity alumina to Cb-1Zr alloy is the best of the systems studied, but that additional studies must be performed to establish its service temperature limitations for the desired three to five years' service.

  10. 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.

  11. 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.

  12. Thin Film Electrodes for Rare Event Detectors

    NASA Astrophysics Data System (ADS)

    Odgers, Kelly; Brown, Ethan; Lewis, Kim; Giordano, Mike; Freedberg, Jennifer

    2017-01-01

    In detectors for rare physics processes, such as neutrinoless double beta decay and dark matter, high sensitivity requires careful reduction of backgrounds due to radioimpurities in detector components. Ultra pure cylindrical resistors are being created through thin film depositions onto high purity substrates, such as quartz glass or sapphire. By using ultra clean materials and depositing very small quantities in the films, low radioactivity electrodes are produced. A new characterization process for cylindrical film resistors has been developed through analytic construction of an analogue to the Van Der Pauw technique commonly used for determining sheet resistance on a planar sample. This technique has been used to characterize high purity cylindrical resistors ranging from several ohms to several tera-ohms for applications in rare event detectors. The technique and results of cylindrical thin film resistor characterization will be presented.

  13. Production and Characterization of Bulk MgB2 Material made by the Combination of Crystalline and Carbon Coated Amorphous Boron Powders

    NASA Astrophysics Data System (ADS)

    Hiroki, K.; Muralidhar, M.; Koblischka, M. R.; Murakami, M.

    2017-07-01

    The object of this investigation is to reduce the cost of bulk production and in the same time to increase the critical current performance of bulk MgB2 material. High-purity commercial powders of Mg metal (99.9% purity) and two types of crystalline (99% purity) and 16.5 wt% carbon-coated, nanometer-sized amorphous boron powders (98.5% purity) were mixed in a nominal composition of MgB2 to reduce the boron cost and to see the effect on the superconducting and magnetic properties. Several samples were produced mixing the crystalline boron and carbon-coated, nanometer-sized amorphous boron powders in varying ratios (50:50, 60:40, 70:30, 80:20, 90:10) and synthesized using a single-step process using the solid state reaction around 800 °C for 3 h in pure argon atmosphere. The magnetization measurements exhibited a sharp superconducting transition temperature with T c, onset around 38.6 K to 37.2 K for the bulk samples prepared utilizing the mixture of crystalline boron and 16.5% carbon-coated amorphous boron. The critical current density at higher magnetic field was improved with addition of carbon-coated boron to crystalline boron in a ratio of 80:20. The highest self-field Jc around 215,000 A/cm2 and 37,000 A/cm2 were recorded at 20 K, self-field and 2 T for the sample with a ratio of 80:10. The present results clearly demonstrate that the bulk MgB2 performance can be improved by adding carbon-coated nano boron to crystalline boron, which will be attractive to reduce the cost of bulk MgB2 material for several industrial applications.

  14. 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.

  15. Chemical Characterization and Thermal Stressing Studies of Perfluorohexane Fluids for Space-Based Applications

    NASA Technical Reports Server (NTRS)

    Arnold, William A.; Hartman, Thomas G.; McQuillen, John

    2006-01-01

    Perfluorohexane (PFH), C6F14, is a perfluorocarbon fluid. Several PFH fluids with different isomer concentrations were evaluated for use in an upcoming NASA space experiment. Samples tested included two commercially obtained high-purity n-perfluorohexane (n-PFH) fluids and a technical grade mixture of C6F14 branched and linear isomers (FC-72(TradeMark)). These fluids were evaluated for exact chemical composition, impurity purity and high temperature degradation behavior (pyrolysis). Our investigation involved simulated thermal stressing studies of PFH fluids under conditions likely to occur in the event of an atmospheric breach within the International Space Station (ISS) and subsequent exposure of the vapors to the high temperature and catalyst present in its Trace Contaminant Control Subsystem (TCCS). Exposure to temperatures in the temperature range of 200-450 C in an inert or oxidizing atmosphere, with and without the presence of catalyst was investigated. The most aggressive conditions studied were exposure of PFH vapors to 450 C in air and in the presence of TCCS (palladium) catalyst. Gas chromatography-mass spectrometry (GC-MS) and gas chromatography (GC) analyses were conducted on the perfluorohexane samples before and after pyrolysis. The FC-72 and n-PFH samples showed no significant degradation following pyrolysis even under the most aggressive study conditions. Some trace level impurities associated with the PFH samples such as linear perfluorocarbon monohydrides or monoiodides were destroyed by pyrolysis at the upper limit. Other trace level impurities such as olefinic or cycloolefinic perfluorocarbons were converted into oxidation products by pyrolysis. The purity of PFH following pyrolysis actually increased slightly as a consequence since these trace contaminants were effectively scrubbed from the samples. However, since the initial concentrations of the thermally-impacted impurities were so low, the net effect was trivial. A potential byproduct of exposure of perfluorohexane fluids to high temperatures is the production of perfluoroisobutene (PFiB), which is extremely toxic. An ultra-high sensitivity PFiB-specific analysis based on GC-MS with negative ion chemical ionization (NICI) detection was used to evaluate the samples following thermal stressing. The perfluorohexanes examined here under conditions reflective of the ISS TCCS environment showed no signs of PFiB production with an analytical detection limit of 10 part per billion (ppb v/v).

  16. Two-photon absorption measurements of deep UV transmissible materials at 213 nm

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

    Patankar, S.; Yang, S. T.; Moody, J. D.

    We report on two photon absorption measurements at 213nm of deep UV transmissible media including LiF, MgF 2, CaF 2, BaF 2, Sapphire (Al 2O 3) and high purity grades of fused-silica (SiO 2). A high stability 24ps Nd:YAG laser operating at the 5th harmonic (213nm) was used to generate a high intensity, long Rayleigh length Gaussian focus inside the samples. The measurements of the Fluoride crystals and Sapphire indicate two photon absorption coefficients between 0.004 and 0.82 cm/GW. We find that different grades of fused silica performed near identically for two photon absorption, however, there are differences in linearmore » losses associated with purity. A low two photon absorption cross section is measured for MgF 2 making it an ideal material for the propagation of high intensity deep UV lasers.« less

  17. Two-photon absorption measurements of deep UV transmissible materials at 213 nm

    DOE PAGES

    Patankar, S.; Yang, S. T.; Moody, J. D.; ...

    2017-09-19

    We report on two photon absorption measurements at 213nm of deep UV transmissible media including LiF, MgF 2, CaF 2, BaF 2, Sapphire (Al 2O 3) and high purity grades of fused-silica (SiO 2). A high stability 24ps Nd:YAG laser operating at the 5th harmonic (213nm) was used to generate a high intensity, long Rayleigh length Gaussian focus inside the samples. The measurements of the Fluoride crystals and Sapphire indicate two photon absorption coefficients between 0.004 and 0.82 cm/GW. We find that different grades of fused silica performed near identically for two photon absorption, however, there are differences in linearmore » losses associated with purity. A low two photon absorption cross section is measured for MgF 2 making it an ideal material for the propagation of high intensity deep UV lasers.« less

  18. Two-photon absorption measurements of deep UV transmissible materials at 213  nm.

    PubMed

    Patankar, S; Yang, S T; Moody, J D; Swadling, G F; Erlandson, A C; Bayramian, A J; Barker, D; Datte, P; Acree, R L; Pepmeier, B; Madden, R E; Borden, M R; Ross, J S

    2017-10-20

    We report on two-photon absorption measurements at 213 nm of deep UV transmissible media, including LiF, MgF 2 , CaF 2 , BaF 2 , sapphire (Al 2 O 3 ), and high-purity grades of fused-silica (SiO 2 ). A high-stability 24 ps Nd:YAG laser operating at the 5th harmonic (213 nm) was used to generate a high-intensity, long-Rayleigh-length Gaussian focus inside the samples. The measurements of the fluoride crystals and sapphire indicate two-photon absorption coefficients between 0.004 and 0.82 cm/GW. We find that different grades of fused silica performed near identically for two-photon absorption; however, there are differences in linear losses associated with purity. A low two-photon absorption cross section is measured for MgF 2 , making it an ideal material for the propagation of high-intensity deep UV lasers.

  19. 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

  20. 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.

  1. 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.

  2. Volatility Characteristics of MIL-L-7808 Turbine Lubricants

    DTIC Science & Technology

    1975-06-01

    test measurements. Total acid numbers and gas chromatograms were obtained for selected residual evaporation samples which provided information on the...ethylhexyl) adipate, purity 99% E-109 Di()2-ethylhexyl azelate , purity 84% E-120 2,2-Dimethyltrimethylene nonanoate, purity - 89% E-129...gave slightly lower evaporation values along with a noticeable decrease in lubricant degradation as shown by the total acid members obtained on the

  3. 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.

  4. 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.

  5. 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

  6. Mechanical properties of niobium radio-frequency cavities

    DOE PAGES

    Ciovati, Gianluigi; Dhakal, Pashupati; Matalevich, Joseph R.; ...

    2015-07-02

    Radio-frequency cavities made of bulk niobium are one of the components used in modern particle accelerators. The mechanical stability is an important aspect of cavity design, which typically relies on finite-element analysis simulations using material properties from tensile tests on sample. This contribution presents the results of strain and resonant frequency measurements as a function of a uniform pressure up to 722 kPa, applied to single-cell niobium cavities with different crystallographic structure, purity and treatments. In addition, burst tests of high-purity multi-cell cavities with different crystallographic structure have been conducted up to the tensile strength of the material. Finite-element analysismore » of the single-cell cavity geometry is in good agreement with the observed behavior in the elastic regime assuming a Young's modulus value of 88.5 GPa and a Poisson's ratio of 0.4, regardless of crystallographic structure, purity or treatment. However, the measured yield strength and tensile strength depend on crystallographic structure, material purity and treatment. In particular, the results from this study show that the mechanical properties of niobium cavities with large crystals are comparable to those of cavities made of fine-grain niobium.« less

  7. 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.

  8. 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

  9. 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

  10. Biaxial deformation in high purity aluminum

    DOE PAGES

    Livescu, V.; Bingert, J. F.; Liu, C.; ...

    2015-09-25

    The convergence of multiple characterization tools has been applied to investigate the relationship of microstructure on damage evolution in high purity aluminum. The extremely coarse grain size of the disc-shaped sample provided a quasi-two dimensional structure from which the location of surface-measured features could be inferred. In particular, the role of pre-existing defects on damage growth was accessible due to the presence of casting porosity in the aluminum. Micro tomography, electron backscatter diffraction, and digital image correlation were applied to interrogate the sample in three dimensions. Recently micro-bulge testing apparatus was used to deform the pre-characterized disc of aluminum inmore » biaxial tension, and related analysis techniques were applied to map local strain fields. Subsequent post-mortem characterization of the failed sample was performed to correlate structure to damaged regions. We determined that strain localization and associated damage was most strongly correlated with grain boundary intersections and plastic anisotropy gradients between grains. Pre-existing voids played less of an apparent role than was perhaps initially expected. Finally, these combined techniques provide insight to the mechanism of damage initiation, propagation, and failure, along with a test bed for predictive damage models incorporating anisotropic microstructural effects.« less

  11. Pore structure of raw and purified HiPco single-walled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Cinke, Martin; Li, Jing; Chen, Bin; Cassell, Alan; Delzeit, Lance; Han, Jie; Meyyappan, M.

    2002-10-01

    Very high purity single-walled carbon nanotubes (SWNTs) were obtained from HiPco SWNT samples containing Fe particles by a two-step purification process. The raw and purified samples were characterized using high resolution transmission electron microscopy (HRTEM), Raman spectroscopy and thermogravimetric analysis (TGA). The purified sample consists of ˜0.4% Fe and the process does not seem to introduce any additional defects. The N 2 adsorption isotherm studies at 77 K reveal that the total surface area of the purified sample increases to 1587 m 2/g from 567 m 2/g for the raw material, which is the highest value reported for SWNTs.

  12. 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.

  13. Color display and encryption with a plasmonic polarizing metamirror

    NASA Astrophysics Data System (ADS)

    Song, Maowen; Li, Xiong; Pu, Mingbo; Guo, Yinghui; Liu, Kaipeng; Yu, Honglin; Ma, Xiaoliang; Luo, Xiangang

    2018-01-01

    Structural colors emerge when a particular wavelength range is filtered out from a broadband light source. It is regarded as a valuable platform for color display and digital imaging due to the benefits of environmental friendliness, higher visibility, and durability. However, current devices capable of generating colors are all based on direct transmission or reflection. Material loss, thick configuration, and the lack of tunability hinder their transition to practical applications. In this paper, a novel mechanism that generates high-purity colors by photon spin restoration on ultrashallow plasmonic grating is proposed. We fabricated the sample by interference lithography and experimentally observed full color display, tunable color logo imaging, and chromatic sensing. The unique combination of high efficiency, high-purity colors, tunable chromatic display, ultrathin structure, and friendliness for fabrication makes this design an easy way to bridge the gap between theoretical investigations and daily-life applications.

  14. 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.

  15. Effect of natural flocculants on purity and properties of β-glucan extracted from barley and oat.

    PubMed

    Kurek, Marcin Andrzej; Karp, Sabina; Stelmasiak, Adrian; Pieczykolan, Ewelina; Juszczyk, Karolina; Rieder, Anne

    2018-05-15

    In this study, β-glucan was extracted from wholegrain oat and barley flours by a novel extraction and purification method employing natural flocculants (chitosan, guar gum and gelatin). The use of flocculants decreased the total amount of extracted gum, which was highest in control samples (9.07 and 7.9% for oat and barley, respectively). The β-glucan specific yield, however, increased with the use of chitosan and guar gum, which were able to remove protein and ash impurities resulting in gums with a higher purity.The highest concentration of chitosan (0.6 %) resulted in gums with the highest β-glucan content (82.0 ± 0.23 and 79.0 ± 0.19 for barley and oat, respectively) and highest β-glucan specific yield (96.9 and 93.3 % for oat and barley, respectively). Explanation is in R&D section. The use of gelatin was not successful. All gum samples had a high content of total dietary fiber (>74%) and a high water holding capacity (4.6-7.4 g/g), but differed in apparent viscosity, which was highest for the oat sample extracted with 0.6% chitosan. This sample also showed the highest β-glucan molecular weight among the oat samples, which were in general 10-fold higher than for the barley samples. Among the barley samples, β-glucan molecular weight was highest for the control. Copyright © 2018 Elsevier Ltd. All rights reserved.

  16. A gas-loading system for LANL two-stage gas guns

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

    Gibson, Lloyd Lee; Bartram, Brian Douglas; Dattelbaum, Dana Mcgraw

    A novel gas loading system was designed for the specific application of remotely loading high purity gases into targets for gas-gun driven plate impact experiments. The high purity gases are loaded into well-defined target configurations to obtain Hugoniot states in the gas phase at greater than ambient pressures.The small volume of the gas samples is challenging, as slight changing in the ambient temperature result in measurable pressure changes. Therefore, the ability to load a gas gun target and continually monitor the sample pressure prior to firing provides the most stable and reliable target fielding approach. We present the design andmore » evaluation of a gas loading system built for the LANL 50 mm bore two-stage light gas gun. Targets for the gun are made of 6061 Al or OFHC Cu, and assembled to form a gas containment cell with a volume of approximately 1.38 cc. The compatibility of materials was a major consideration in the design of the system, particularly for its use with corrosive gases. Piping and valves are stainless steel with wetted seals made from Kalrez® and Teflon®. Preliminary testing was completed to ensure proper flow rate and that the proper safety controls were in place. The system has been used to successfully load Ar, Kr, Xe, and anhydrous ammonia with purities of up to 99.999 percent. The design of the system and example data from the plate impact experiments will be shown.« less

  17. A gas-loading system for LANL two-stage gas guns

    NASA Astrophysics Data System (ADS)

    Gibson, L. L.; Bartram, B. D.; Dattelbaum, D. M.; Lang, J. M.; Morris, J. S.

    2017-01-01

    A novel gas loading system was designed for the specific application of remotely loading high purity gases into targets for gas-gun driven plate impact experiments. The high purity gases are loaded into well-defined target configurations to obtain Hugoniot states in the gas phase at greater than ambient pressures. The small volume of the gas samples is challenging, as slight changing in the ambient temperature result in measurable pressure changes. Therefore, the ability to load a gas gun target and continually monitor the sample pressure prior to firing provides the most stable and reliable target fielding approach. We present the design and evaluation of a gas loading system built for the LANL 50 mm bore two-stage light gas gun. Targets for the gun are made of 6061 Al or OFHC Cu, and assembled to form a gas containment cell with a volume of approximately 1.38 cc. The compatibility of materials was a major consideration in the design of the system, particularly for its use with corrosive gases. Piping and valves are stainless steel with wetted seals made from Kalrez® and Teflon®. Preliminary testing was completed to ensure proper flow rate and that the proper safety controls were in place. The system has been used to successfully load Ar, Kr, Xe, and anhydrous ammonia with purities of up to 99.999 percent. The design of the system and example data from the plate impact experiments will be shown.

  18. 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

  19. SEPARATION AND PURIFICATION OF TWO MINOR COMPOUNDS FROM RADIX ISATIDIS BY INTEGRATIVE MPLC AND HSCCC WITH PREPARATIVE HPLC.

    PubMed

    Liang, Zhenjie; Li, Bin; Liang, Yong; Su, Yaping; Ito, Yoichiro

    2015-01-01

    Radix isatidis has been widely used as a Chinese traditional medicine for its anti-virus and anticancer activities where the minor components may contribute to these beneficial pharmaceutical effects. In order to enrich the target minor compounds effectively and rapidly, extraction, medium-pressure liquid chromatography (MPLC), high-speed countercurrent chromatography (HSCCC) and preparative high-performance liquid chromatography (pre-HPLC) were integratively used for separation and purification of two target minor compounds indole-3-acetonitrile-6-O-β-D-glucopyranoside (target 1) and clemastanin B (target 2) in the present study. Radix isatidis was dried, pulverized and extracted with 50% methanol at room temperature, then concentrated and subjected to pretreatment with D-101 macroporous resin chromatography and extraction by MPLC. The first target compound was separated by MPLC at the purity raised to 70-80%, but without the second minor compounds which were irreversibly adsorbed by C18 solid support. Therefore, the second target compound in the crude extract was directly separated by HSCCC at purity of 80-90%. Finally these refined samples were further separated by pre-HPLC to obtain a high purity at 98-99%. The chemical structure identification of each target compound was carried out by IR, ESI-MS and 1 H NMR.

  20. Radionuclidic purity measurements for cyclotron-produced 99mTc via 100Mo(p,2n) at 18 MeV

    NASA Astrophysics Data System (ADS)

    Buckley, K.; Tanguay, J.; Hou, X.; Stothers, L.; Vuckovic, M.; Frantzen, K.; Cockburn, N.; Corsaut, J.; Dodd, M.; Goodbody, A.; Hanemaayer, V.; Hook, B.; Klug, J.; Kovacs, M.; Kumlin, J.; McDiarmid, S.; McEwan, J.; Prato, F.; Ruddock, P.; Valiant, J.; Zeisler, S.; Ruth, T.; Celler, A.; Benard, F.; Schaffer, P.

    2017-05-01

    The radionuclidic purity of cyclotron-produced 99mTc has been measured by gamma ray spectroscopy and compared to the results of a quick release test modeled after the molybdenum breakthrough test performed on generator-derived 99mTc. Excellent radionuclidic purity is reported for samples produced at BCCA during our clinical trial. The quick release test results agree well with the gamma ray analysis.

  1. 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.

  2. 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.

  3. 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

  4. MIS High-Purity Plutonium Oxide Hydride Product 5501579 (SSR124): Final Report

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

    Veirs, Douglas Kirk; Stroud, Mary Ann; Berg, John M.

    A high-purity plutonium dioxide material from the Material Identification and Surveillance (MIS) Program inventory has been studied with regard to gas generation and corrosion in a storage environment. Sample 5501579 represents process plutonium oxides from hydride oxide from Rocky Flats that are currently stored in 3013 containers. After calcination to 950°C, the material contained 87.42% plutonium with no major impurities. This study followed over time, the gas pressure of a sample with nominally 0.5 wt% water in a sealed container with an internal volume scaled to 1/500th of the volume of a 3013 container. Gas compositions were measured periodically overmore » a six year period. The maximum observed gas pressure was 124 kPa. The increase over the initial pressure of 70 kPa was primarily due to generation of nitrogen and carbon dioxide gas. Hydrogen and oxygen were minor components of the headspace gas. At the completion of the study, the internal components of the sealed container showed signs of corrosion.« less

  5. 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.

  6. Processing and Fabrication of High Temperature Oxide Superconductors

    DTIC Science & Technology

    1992-11-30

    I. Gusman and S. M. Johnson, "Cryochemical Method of Preparing Ultrafine Particles of High-Purity Superconducting Oxides," U.S. Patent 4,975,415...Supercon- PREPARING ULTRAFINE PARTICLES OF ducting-MRS EA 11, Apr. 1987, pp. 265-267. HIGH-PURITY SUPERCONDUCTING Materials and Processing Report vol. 2, No... ULTRAFINE PARTICLES OF HIGH-PURITY A. W. Sleight in U.S. Pa&. No. 3,932.315 discloses SUPERCONDUCTING OXIDES superconductive barium-lead-bismuth oxides of

  7. 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.

  8. 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

  9. A simple fabrication of CH3NH3PbI3 perovskite for solar cells using low-purity PbI2

    NASA Astrophysics Data System (ADS)

    Guo, Nanjie; Zhang, Taiyang; Li, Ge; Xu, Feng; Qian, Xufang; Zhao, Yixin

    2017-01-01

    The CH3NH3PbI3 (MAPbI3) perovskite was usually prepared by high-purity PbI2 with high cost. The low cost and low-purity PbI2 was seldom reported for fabrication of MAPbI3 because it cannot even dissolve well in widely adopted solvent of DMF. We developed an easy method to adapt low-purity PbI2 for fabrication of high quality MAPbI3 just by the simple addition of some hydrochloric acid into the mixture of low-purity PbI2, MAI and DMF. This straightforward method can not only help dissolve the low quality PbI2 by reacting with some impurities in DMF, but also lead to a successful fabrication of high-quality perovskite solar cells with up to 14.80% efficiency comparable to the high quality PbI2 precursors. Project supported by the National Natural Science Foundation of China (Nos. 51372151, 21303103) and Houyingdong Grant (No. 151046).

  10. Nuclear Resonance Fluorescence Measurements of High Explosives

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

    Caggiano, Joseph A.; Warren, Glen A.; Korbly, Steve

    Pacific Northwest National Laboratory and Passport Systems have collaborated to perform Nuclear Resonance Fluorescence experiments using several high quality high-explosive simulant samples. These measurements were conducted to determine the feasibility of finding and characterizing high explosive material by NRF interrogation. Electron beams of 5.1, 5.3, 8, and 10 MeV were used to produce bremsstrahlung photon beams, which irradiated the samples. The gamma-ray spectra were collected using high-purity germanium detectors. Nitrogen-to-carbon ratios of the high-explosive simulants were extracted from the 5.1 and 5.3 MeV data and compare favorably with accepted values. Analysis of the 8 and 10 MeV data is inmore » progress; preliminary isotopic comparisons within the samples are consistent with the expected results.« less

  11. Ion implantation system and process for ultrasensitive determination of target isotopes

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

    Farmer, III, Orville T.; Liezers, Martin

    2016-09-13

    A system and process are disclosed for ultrasensitive determination of target isotopes of analytical interest in a sample. Target isotopes may be implanted in an implant area on a high-purity substrate to pre-concentrate the target isotopes free of contaminants. A known quantity of a tracer isotope may also be implanted. Target isotopes and tracer isotopes may be determined in a mass spectrometer. The present invention provides ultrasensitive determination of target isotopes in the sample.

  12. 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.

  13. [Simultaneously preparation of grams of high purity tyrosol, crenulatin and salidroside from Rhodiola crenulata].

    PubMed

    Luo, Xin; Wang, Xue-jing; Li, Shi-ping; Zhang, Qiao; Zhao, Yi-wu; Huang Wen-zhe; Wang, Zhen-zhong; Xiao, Wei

    2015-04-01

    Tyrosol, crenulatin and salidroside are the main active constituents of Rhodiola crenulata, with extensive pharmacological activities. In the study, grams of high purity tyrosol, crenulatin and salidroside were simultaneously separated from R. crenulata by the first time. Firstly, R. crenulata was extracted by 70% alcohol. Then, with the yields of three compounds as the index, the macroporous resin was optimized. At last, grams of high purity tyrosol, crenulatin and salidroside were isolated by D-101 macroporousresin, purified by column chromatography. Detected by HPLC, the purity of three compounds were higher than 98%. This method has the advantages of simple process and operation, less dosage of organic solvent, highly yield and reproducibility, suitable for the simultaneously preparation of tyrosol, crenulatin and salidroside.

  14. 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.

  15. Determination of NIST-Traceable Quantitative Weight Percentage Purity for G Agent Standards

    DTIC Science & Technology

    Nuclear magnetic resonance (NMR) with phosphorus -31 detection is described to determine the weight percent purity of feedstock samples of agents GA...and GD in a way that is National Institute of Standards and Technology (NIST)-traceable. A Precision and Accuracy test is described.

  16. 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

  17. Selection of polymer binders and fabrication of SiC fiber-reinforced reaction-bonded silicon nitride matrix composites

    NASA Technical Reports Server (NTRS)

    Haggerty, John S.; Lightfoot, A.; Sigalovsky, J.

    1993-01-01

    The topics discussed include the following: effects of solvent and polymer exposures on nitriding kinetics of high purity Si powders and on resulting phase distributions; effects of solvent and polymer exposures on Si Surface Chemistry; effects of solvent and polymeric exposures on nitriding kinetics; and fabrication of flexural test samples.

  18. Preparative isolation and purification of anti-tumor agent ansamitocin P-3 from fermentation broth of Actinosynnema pretiosum using high-performance counter-current chromatography.

    PubMed

    Yao, Yuqin; Cheng, Zhihui; Ye, Haoyu; Xie, Yongmei; He, Jing; Tang, Minghai; Shen, Tao; Wang, Jiangman; Zhou, Yan; Lu, Zejun; Luo, Feng; Chen, Lijuan; Yu, Luoting; Yang, Jin-Liang; Peng, Aihua; Wei, Yuquan

    2010-05-01

    Ansamitocin P-3 is a potent anti-tumor maytansinoid found in Actinosynnema pretiosum. However, due to the complexity of the fermentation broth of Actinomycete, how to effectively separate ansamitocin P-3 is still a challenge. In this study, both analytical and preparative high-performance counter-current chromatography were successfully used to separate and purify ansamitocin P-3 from fermentation broth. A total of 28.8 mg ansamitocin P-3 with purity of 98.4% was separated from 160 mg crude sample of fermentation broth in less than 80 min with the two-phase solvent system of hexane-ethyl acetate-methanol-water (0.6:1:0.6:1, v/v/v/v). The purity and structural identification were determined by HPLC, (1)H NMR, (13)C NMR and mass spectroscopy.

  19. Synthesis and characterization of Mn-Bi alloy

    NASA Astrophysics Data System (ADS)

    Mishra, Ashutosh; Patil, Harsha; Jain, G.; Mishra, N.

    2012-06-01

    High purity MnBi low temperature phase has been prepared and analyzed using X-ray diffraction, Lorentz-Polarization Factor and Fourier transforms infrared measurement. After synthesis of samples structural characterization has done on samples by X-ray diffraction, which shows that after making the bulk sample is in no single phase MnBi has been prepared by sintering Mn and Bi powders. By Lorentz-Polarization Factor is affecting the relative intensity of diffraction lines on a powder form. And by FTIR which shows absorption peaks of MnBi alloys.

  20. High-efficiency multiphoton boson sampling

    NASA Astrophysics Data System (ADS)

    Wang, Hui; He, Yu; Li, Yu-Huai; Su, Zu-En; Li, Bo; Huang, He-Liang; Ding, Xing; Chen, Ming-Cheng; Liu, Chang; Qin, Jian; Li, Jin-Peng; He, Yu-Ming; Schneider, Christian; Kamp, Martin; Peng, Cheng-Zhi; Höfling, Sven; Lu, Chao-Yang; Pan, Jian-Wei

    2017-06-01

    Boson sampling is considered as a strong candidate to demonstrate 'quantum computational supremacy' over classical computers. However, previous proof-of-principle experiments suffered from small photon number and low sampling rates owing to the inefficiencies of the single-photon sources and multiport optical interferometers. Here, we develop two central components for high-performance boson sampling: robust multiphoton interferometers with 99% transmission rate and actively demultiplexed single-photon sources based on a quantum dot-micropillar with simultaneously high efficiency, purity and indistinguishability. We implement and validate three-, four- and five-photon boson sampling, and achieve sampling rates of 4.96 kHz, 151 Hz and 4 Hz, respectively, which are over 24,000 times faster than previous experiments. Our architecture can be scaled up for a larger number of photons and with higher sampling rates to compete with classical computers, and might provide experimental evidence against the extended Church-Turing thesis.

  1. 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

  2. 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

  3. 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.

  4. 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.

  5. Sample preservation, transport and processing strategies for honeybee RNA extraction: Influence on RNA yield, quality, target quantification and data normalization.

    PubMed

    Forsgren, Eva; Locke, Barbara; Semberg, Emilia; Laugen, Ane T; Miranda, Joachim R de

    2017-08-01

    Viral infections in managed honey bees are numerous, and most of them are caused by viruses with an RNA genome. Since RNA degrades rapidly, appropriate sample management and RNA extraction methods are imperative to get high quality RNA for downstream assays. This study evaluated the effect of various sampling-transport scenarios (combinations of temperature, RNA stabilizers, and duration) of transport on six RNA quality parameters; yield, purity, integrity, cDNA synthesis efficiency, target detection and quantification. The use of water and extraction buffer were also compared for a primary bee tissue homogenate prior to RNA extraction. The strategy least affected by time was preservation of samples at -80°C. All other regimens turned out to be poor alternatives unless the samples were frozen or processed within 24h. Chemical stabilizers have the greatest impact on RNA quality and adding an extra homogenization step (a QIAshredder™ homogenizer) to the extraction protocol significantly improves the RNA yield and chemical purity. This study confirms that RIN values (RNA Integrity Number), should be used cautiously with bee RNA. Using water for the primary homogenate has no negative effect on RNA quality as long as this step is no longer than 15min. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. High-brightness and high-color purity red-emitting Ca3Lu(AlO)3(BO3)4:Eu3+ phosphors with internal quantum efficiency close to unity for near-ultraviolet-based white-light-emitting diodes.

    PubMed

    Huang, Xiaoyong; Wang, Shaoying; Li, Bin; Sun, Qi; Guo, Heng

    2018-03-15

    In this work, we reported on high-brightness Eu 3+ -activated Ca 3 Lu(AlO) 3 (BO 3 ) 4 (CLAB) red-emitting phosphors. Under 397 nm excitation, the CLAB:Eu 3+ phosphors showed intense red emissions at around 621 nm with CIE coordinates of (0.657, 0.343). The optimal doping concentration of Eu 3+ ions was found to be 30 mol. %, and the CLAB:0.3Eu 3+ sample possessed high-color purity of 93% and ultra-high internal quantum efficiency as great as 98.5%. Importantly, the CLAB:0.3Eu 3+ also had good thermal stability. Finally, a white-light-emitting diode (WLED) lamp with good color-rendering index was fabricated by using a 365 nm ultraviolet chip and the phosphor blends of CLAB:0.3Eu 3+ red-emitting phosphors, (Ba,Sr) 2 SiO 4 :Eu 2+ green-emitting phosphors, and BaMgAl 10 O 7 :Eu 2+ blue-emitting phosphors.

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

    Kristo, Michael Joseph; Keegan, Elizabeth; Colella, Michael

    Nuclear forensic analysis was conducted on two uranium samples confiscated during a police investigation in Victoria, Australia. The first sample, designated NSR-F-270409-1, was a depleted uranium powder of moderate purity (~1000 μg/g total elemental impurities). The chemical form of the uranium was a compound similar to K 2(UO 2) 3O 4·4H 2O. While aliquoting NSR-F-270409-1 for analysis, the body and head of a Tineid moth was discovered in the sample. The second sample, designated NSR-F-270409-2, was also a depleted uranium powder. It was of reasonably high purity (~380 μg/g total elemental impurities). The chemical form of the uranium was primarilymore » UO 3·2H 2O, with minor phases of U 3O 8 and UO 2. While aliquoting NSR-F-270409-2 for analysis, a metal staple of unknown origin was discovered in the sample. The presence of 236U and 232U in both samples indicates that the uranium feed stocks for these samples experienced a neutron flux at some point in their history. The reactor burn-up calculated from the isotopic composition of the uranium is consistent with that of spent fuel from natural uranium (NU) fueled Pu production. These nuclear forensic conclusions allow us to categorically exclude Australia as the origin of the material and greatly reduce the number of candidate sources.« less

  8. 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.

  9. On-chip cell sorting via patterned magnetic traps

    NASA Astrophysics Data System (ADS)

    Byvank, Tom; Prikockis, Michael; Chen, Aaron; Miller, Brandon; Chalmers, Jeffrey; Sooryakumar, Ratnasingham

    2015-03-01

    Due to their importance in research for the diagnosis and treatment of cancer, numerous schemes have been developed to sort rare cell populations, e.g., circulating tumor cells (CTCs), from a larger ensemble of cells. Here, we improve upon a previously developed microfluidic device (Lab Chip 13, 1172, (2013)) to increase throughput and sorting purity of magnetically labeled cells. The separation mechanism involves controlling magnetic forces by manipulating the magnetic domain structures of embedded permalloy microdisks with weak external fields. These forces move labeled cells from the input flow stream into an adjacent buffer flow stream. Such magnetically activated transfer separates the magnetic entities from their non-magnetic counterparts as the two flow streams split apart and move toward their respective outputs. Purity of the magnetic output is modulated by the withdrawal rate of the non-magnetic output relative to the inputs. A proof of concept shows that CTCs from metastatic breast cancer patients can be sorted, recovered from the device, and confirmed as CTCs using separate immunofluorescence staining and analysis. With further optimizations, the channel could become a useful device for high purity final sorting of enriched patient cell samples.

  10. Piezoelectric and Electrostrictive Materials for Transducer Applications. Volume 3.

    DTIC Science & Technology

    1988-03-01

    the preparation and characterization of these required compositions. High-purity lead acetate, titanium isopropoxide , and zirconium n-propoxide were...method was similar to the procedure used in Reference 4 to prepare PbTiO 3. High-purity lead acetate [Pb(C2 H3 0 2 )2 -3H-2Oj, titanium isopropoxide [Ti(OC...dielectric constant as shown in Figure 14(A). P.𔃿 8 IV. CONCLUSION High-purity lead acetate, titanium isopropoxide and zirconium n-propoxide were used as

  11. 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.

  12. Human parvovirus B19 infection in hemophiliacs first infused with two high-purity, virally attenuated factor VIII concentrates.

    PubMed

    Azzi, A; Ciappi, S; Zakvrzewska, K; Morfini, M; Mariani, G; Mannucci, P M

    1992-03-01

    Human parvovirus B19 can be transmitted by coagulation factor concentrates and is highly resistant to virucidal methods. To evaluate whether the additional removal of virus by chromatographic methods during the manufacture of high-purity concentrates reduces the risk of B19 transmission, we have prospectively evaluated the rate of anti-B19 seroconversion in two groups of susceptible (anti-B19 negative) hemophiliacs infused with high-purity, heated (pasteurized) or solvent-detergent-treated factor VIII concentrates. Both products infected a relatively high proportion of patients (nine of 20).

  13. Analysis of heterogeneities in strain and microstructure in aluminum alloy and magnesium processed by high-pressure torsion

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

    Panda, Subrata, E-mail: subrata.panda@univ-lorrain

    2017-01-15

    Two distinct bulk light metals were opted to study the shear strain evolution and associated heterogeneities in texture/microstructure development during torsional straining by high pressure torsion (HPT): a face centered cubic Al alloy (A5086) and a hexagonal commercial purity Mg. Relatively thick disk samples - four times thicker than usually employed in HPT process - were processed to 180° and 270° rotations. With the help of X-ray tomography, the shear strain gradients were examined in the axial direction. The results showed strongly localized shear deformation in the middle plane of the disks in both materials. These gradients involved strong heterogeneitiesmore » in texture, microstructure and associated hardness, in particular through the thickness direction at the periphery of the disk where the interplay between significant strain hardening and possible dynamic recrystallization could occur. - Highlights: •HPT processing was conducted on bulk specimens thicker than the usual thin-disks. •The Al alloy (A5086) and commercial purity magnesium samples were compared. •Distributions of strain and microhardness were evaluated in the radial and axial direction. •Plastic deformation is highly localized in the middle plane at outer edge in both materials. •Different DRX rates governed the differences in microstructure and hardening behavior.« less

  14. 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

  15. Synthesis of Reduced Graphene Oxide-Modified LiMn0.75Fe0.25PO4 Microspheres by Salt-Assisted Spray Drying for High-Performance Lithium-Ion Batteries

    PubMed Central

    Kim, Myeong-Seong; Kim, Hyun-Kyung; Lee, Suk-Woo; Kim, Dong-Hyun; Ruan, Dianbo; Chung, Kyung Yoon; Lee, Sang Hyun; Roh, Kwang Chul; Kim, Kwang-Bum

    2016-01-01

    Microsized, spherical, three-dimensional (3D) graphene-based composites as electrode materials exhibit improved tap density and electrochemical properties. In this study, we report 3D LiMn0.75Fe0.25PO4/reduced graphene oxide microspheres synthesized by one-step salt-assisted spray drying using a mixed solution containing a precursor salt and graphene oxide and a subsequent heat treatment. During this process, it was found that the type of metal salt used has significant effects on the morphology, phase purity, and electrochemical properties of the synthesized samples. Furthermore, the amount of the chelating agent used also affects the phase purity and electrochemical properties of the samples. The composite exhibited a high tap density (1.1 g cm−3) as well as a gravimetric capacity of 161 mA h g−1 and volumetric capacity of 281 mA h cm−3 at 0.05 C-rate. It also exhibited excellent rate capability, delivering a discharge capacity of 90 mA h g−1 at 60 C-rate. Furthermore, the microspheres exhibited high energy efficiency and good cyclability, showing a capacity retention rate of 93% after 1000 cycles at 10 C-rate. PMID:27220812

  16. 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.

  17. Toward Better Personal Ballistic Protection

    DTIC Science & Technology

    2014-03-04

    nanotube-reinforced zirconia-toughened alumina composites prepared by spark plasma sintering , Carbon, Vol 50, Iss 2 (2012), 706-717. [4] Bolduc M...attempt to optimize mechanical properties. The processing approaches investigated were pressureless sintering , hot pressing and hot isostatic...pressing (CIP) and pressureless sintering (PS). Test samples were made with high purity commercially available ceramic powder (over 99.5% for Al2O3). For

  18. MIS High-Purity Plutonium Oxide Metal Oxidation Product TS707001 (SSR123): Final Report

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

    Veirs, Douglas Kirk; Stroud, Mary Ann; Berg, John M.

    A high-purity plutonium dioxide material from the Material Identification and Surveillance (MIS) Program inventory has been studied with regard to gas generation and corrosion in a storage environment. Sample TS707001 represents process plutonium oxides from several metal oxidation operations as well as impure and scrap plutonium from Hanford that are currently stored in 3013 containers. After calcination to 950°C, the material contained 86.98% plutonium with no major impurities. This study followed over time, the gas pressure of a sample with nominally 0.5 wt% water in a sealed container with an internal volume scaled to 1/500th of the volume of amore » 3013 container. Gas compositions were measured periodically over a six year period. The maximum observed gas pressure was 138 kPa. The increase over the initial pressure of 80 kPa was primarily due to generation of nitrogen and carbon dioxide gas in the first six months. Hydrogen and oxygen were minor components of the headspace gas. At the completion of the study, the internal components of the sealed container showed signs of corrosion, including pitting.« less

  19. 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

  20. 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

  1. 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

  2. Measurements of induced radioactivity in some LDEF samples

    NASA Technical Reports Server (NTRS)

    Moss, C. E.; Reedy, R. C.

    1992-01-01

    Twenty-six stainless steel trunnion samples, five aluminum end support retainer plate samples, two aluminum keel plate samples, and two titanium clips were analyzed. The shielded high purity germanium detectors used had efficiencies of 33, 54, and 80 percent at 1332 keV. Detector efficiencies as a function of energy and corrections for self-absorption in the samples were determined with calibrated sources and unactivated control samples. Several measurements were made on most samples. In the trunnion samples, Mn-54 and Co-57 were seen and limits were obtained for other isotopes. The results agree well with 1-D activation calculations for an anisotropic trapped proton model. In the aluminum and titanium samples, Na-22 was detected. Other results are presented.

  3. Measurements of induced radioactivity in some LDEF samples

    NASA Technical Reports Server (NTRS)

    Moss, C. E.; Reedy, R. C.

    1991-01-01

    Twenty-six stainless steel trunnion samples, five aluminum end support retainer plate samples, two aluminum keel plate samples, and two titanium clips were analyzed. The shielded high purity germanium detectors used had efficiencies of 33, 54, and 80 pcts. at 1332 keV. Detector efficiencies as a function of energy and corrections for self absorption in the samples were determined with calibrated sources, unactivated control samples, and calculations. Several measurements were made on most samples. In the trunnion samples, Mn-54 and Co-57 were seen and limits were obtained for other isotopes. The results agree well with 1-D activation calculations for an anisotropic trapped proton model. In the aluminum samples, Na-22 and Be-7 were seen. Other results are presented.

  4. Fractography of the high temperature hydrogen attack of a medium carbon steel

    NASA Technical Reports Server (NTRS)

    Nelson, H. G.; Moorhead, R. D.

    1976-01-01

    Results are reported for an experimental study of the microscopic fracture processes associated with hydrogen attack of a commercially produced plain carbon steel in a well-controlled high-temperature hydrogen environment of high purity. In the experiments, sheet samples were exposed to laboratory-grade hydrogen at a pressure of 3.5 MN/sq m and a temperature of 575 C. The fractography of gas-filled fissures and failed tension specimens is analyzed in an effort to identify any predominant microstructural defect associated with fissure formation, the prevalent modes of fracture, and the contribution of gas-filled fissures to the overall failure process. It is found that the tensile properties of the examined steel were significantly degraded after as few as 136 hr of exposure to a high-purity hydrogen atmosphere at 575 C; that the yield strength, ultimate strength, and elongation at fracture were all reduced progressively with increasing exposure time; and that the yield and ultimate strengths were reduced more than 40% after 408 hr while elongation was reduced to less than 2%.

  5. Label-free isolation of prostate circulating tumor cells using Vortex microfluidic technology.

    PubMed

    Renier, Corinne; Pao, Edward; Che, James; Liu, Haiyan E; Lemaire, Clementine A; Matsumoto, Melissa; Triboulet, Melanie; Srivinas, Sandy; Jeffrey, Stefanie S; Rettig, Matthew; Kulkarni, Rajan P; Di Carlo, Dino; Sollier-Christen, Elodie

    2017-01-01

    There has been increased interest in utilizing non-invasive "liquid biopsies" to identify biomarkers for cancer prognosis and monitoring, and to isolate genetic material that can predict response to targeted therapies. Circulating tumor cells (CTCs) have emerged as such a biomarker providing both genetic and phenotypic information about tumor evolution, potentially from both primary and metastatic sites. Currently, available CTC isolation approaches, including immunoaffinity and size-based filtration, have focused on high capture efficiency but with lower purity and often long and manual sample preparation, which limits the use of captured CTCs for downstream analyses. Here, we describe the use of the microfluidic Vortex Chip for size-based isolation of CTCs from 22 patients with advanced prostate cancer and, from an enumeration study on 18 of these patients, find that we can capture CTCs with high purity (from 1.74 to 37.59%) and efficiency (from 1.88 to 93.75 CTCs/7.5 mL) in less than 1 h. Interestingly, more atypical large circulating cells were identified in five age-matched healthy donors (46-77 years old; 1.25-2.50 CTCs/7.5 mL) than in five healthy donors <30 years old (21-27 years old; 0.00 CTC/7.5 mL). Using a threshold calculated from the five age-matched healthy donors (3.37 CTCs/mL), we identified CTCs in 80% of the prostate cancer patients. We also found that a fraction of the cells collected (11.5%) did not express epithelial prostate markers (cytokeratin and/or prostate-specific antigen) and that some instead expressed markers of epithelial-mesenchymal transition, i.e., vimentin and N-cadherin. We also show that the purity and DNA yield of isolated cells is amenable to targeted amplification and next-generation sequencing, without whole genome amplification, identifying unique mutations in 10 of 15 samples and 0 of 4 healthy samples.

  6. High carrier mobility in ultrapure diamond measured by time-resolved cyclotron resonance

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

    Akimoto, Ikuko, E-mail: akimoto@sys.wakayama-u.ac.jp; Handa, Yushi; Fukai, Katsuyuki

    2014-07-21

    We have performed time-resolved cyclotron resonance measurements in ultrapure diamond crystals for the temperature range of T=7.3–40 K and obtained the temperature-dependent momentum relaxation times based on the cyclotron resonance widths for optically generated electrons and holes. The relaxation time follows a T{sup −3/2} law down to 12 K, which is expected for acoustic-phonon scattering without impurity effect because of the high purity of our samples. The deviation from the law at lower temperatures is explained by the impurity scattering and the breakdown of the high-temperature approximation for the phonon scattering. We extract the carrier drift mobility by using the directly measuredmore » effective masses and the relaxation times. The mobility at 10 K for 600 ns delay time after optical injection is found to be μ{sub e}=1.5×10{sup 6} cm{sup 2}/V s for the electrons, and μ{sub lh}=2.3×10{sup 6} cm{sup 2}/V s and  μ{sub hh}=2.4×10{sup 5} cm{sup 2}/V s for the light and heavy holes, respectively. These high values are achieved by our high-sensitivity detection for low-density carriers (at <10{sup 11} cm{sup −3}) free from the carrier-carrier scattering as well as by the suppression of the impurity scattering in the high-purity samples.« less

  7. Quality control of commercial bovine lactoferrin.

    PubMed

    Wakabayashi, Hiroyuki; Yamauchi, Koji; Abe, Fumiaki

    2018-06-01

    Herein we review commercial bovine lactoferrin quality issues by describing an example of industrial production, the current status of global quality standardization, and quality-activity concerns for further discussion. Morinaga Milk Industry has been industrially producing bovine lactoferrin in Milei GmbH, Germany, since 1989. We delineate its production and quality as an example of safe and high-quality manufacturing. Currently, global standardization in the quality of bovine lactoferrin is progressing through Novel Food and GRAS in the EU and USA, respectively. Novel Food was applied or notified to seven lactoferrin manufacturers and GRAS was notified to three manufacturers, two of which are for infant use and one is for adult use, by the end of 2017. The specifications of these regulations are relatively high, including more than 95% lactoferrin purity in protein, which means that such companies can supply relatively high-grade lactoferrin. There appear to be several concerns regarding lactoferrin quality affecting activities, including contamination of lipopolysaccharide (LPS) and angiogenin, purity, and degradation of lactoferrin sample. Although LPS is immunologically toxic when invading the body, it is distributed normally in foods and the gut. However, an industrial lactoferrin sample may contain LPS at a maximum LPS/lactoferrin molecule ratio = 1/1724, which means 99.9% of the lactoferrin molecule is LPS-free. It is difficult to speculate that LPS contained in a lactoferrin sample affects its activities. Finally in order to achieve good and reproducible results, we make proposals to researchers a use of high-grade lactoferrin, careful storage, and indication the manufacturers' names and specifications in the paper.

  8. Preparation of High Purity Crystalline Silicon by Electro-Catalytic Reduction of Sodium Hexafluorosilicate with Sodium below 180°C

    PubMed Central

    Chen, Yuan; Liu, Yang; Wang, Xin; Li, Kai; Chen, Pu

    2014-01-01

    The growing field of silicon solar cells requires a substantial reduction in the cost of semiconductor grade silicon, which has been mainly produced by the rod-based Siemens method. Because silicon can react with almost all of the elements and form a number of alloys at high temperatures, it is highly desired to obtain high purity crystalline silicon at relatively low temperatures through low cost process. Here we report a fast, complete and inexpensive reduction method for converting sodium hexafluorosilicate into silicon at a relatively low reaction temperature (∼200°C). This temperature could be further decreased to less than 180°C in combination with an electrochemical approach. The residue sodium fluoride is dissolved away by pure water and hydrochloric acid solution in later purifying processes below 15°C. High purity silicon in particle form can be obtained. The relative simplicity of this method might lead to a low cost process in producing high purity silicon. PMID:25153509

  9. 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.

  10. Enhanced Uranium Ore Concentrate Analysis by Handheld Raman Sensor: FY15 Status Report

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

    Bryan, Samuel A.; Johnson, Timothy J.; Orton, Christopher R.

    2015-11-11

    High-purity uranium ore concentrates (UOC) represent a potential proliferation concern. A cost-effective, “point and shoot” in-field analysis capability to identify ore types, phases of materials present, and impurities, as well as estimate the overall purity would be prudent. Handheld, Raman-based sensor systems are capable of identifying chemical properties of liquid and solid materials. While handheld Raman systems have been extensively applied to many other applications, they have not been broadly studied for application to UOC, nor have they been optimized for this class of chemical compounds. PNNL was tasked in Fiscal Year 2015 by the Office of International Safeguards (NA-241)more » to explore the use of Raman for UOC analysis and characterization. This report summarizes the activities in FY15 related to this project. The following tasks were included: creation of an expanded library of Raman spectra of a UOC sample set, creation of optimal chemometric analysis methods to classify UOC samples by their type and level of impurities, and exploration of the various Raman wavelengths to identify the ideal instrument settings for UOC sample interrogation.« less

  11. 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.

  12. 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.

  13. Growth and characterization of high-purity SiC single crystals

    NASA Astrophysics Data System (ADS)

    Augustine, G.; Balakrishna, V.; Brandt, C. D.

    2000-04-01

    High-purity SiC single crystals with diameter up to 50 mm have been grown by the physical vapor transport method. Finite element analysis was used for thermal modeling of the crystal growth cavity in order to reduce stress in the grown crystal. Crystals are grown in high-purity growth ambient using purified graphite furniture and high-purity SiC sublimation sources. Undoped crystals up to 50 mm in diameter with micropipe density less than 100 cm -2 have been grown using this method. These undoped crystals exhibit resistivities in the 10 3 Ω cm range and are p-type due to the presence of residual acceptor impurities, mainly boron. Semi-insulating SiC material is obtained by doping the crystal with vanadium. Vanadium has a deep donor level located near the middle of the band gap, which compensates the residual acceptor resulting in semi-insulating behavior.

  14. A new method to process testicular sperm: combining enzymatic digestion, accumulation of spermatozoa, and stimulation of motility.

    PubMed

    Wöber, Martina; Ebner, Thomas; Steiner, Sarah L; Strohmer, Heinz; Oppelt, Peter; Plas, Eugen; Obruca, Andreas

    2015-03-01

    In azoospermia processing of the TESE material often results in a sample of reduced purity. This prospective study was set up to clarify whether a combination of enzymatic digestion, density gradient centrifugation and stimulation of motility (where indicated) is a feasible option in TESE patients. A total of 63 samples (showing spermatozoa) were processed by the present tripartite processing method. The resulting sperm sample of high purity was directly used for ICSI and subsequent cryopreservation when quality of the accumulated sperm sample allowed for it (n = 39 cycles). Compared to the control group blastocyst formation rate in the present tripartite processing technique was significantly (P < 0.01) higher (55.2 vs. 43.7%). Fertilization rates differed significantly (P < 0.001) between cases in which motile sperm could be used (58.4%) compared to ICSI with immotile sperm (45.0%). Clinical pregnancy rate per transfer was 40.0% (24/60) using fresh and 21.6% (8/37) with cryopreserved TESE material. The calculated live birth rates were 31.7 and 21.6%, respectively. Thirty-five healthy children were born. A comparison with a control group suggests that the present approach using standardized ready-to-use products is efficient and reliable. Presumably healthy live births further indicate the safety of the procedure.

  15. Recovery and Determination of Adsorbed Technetium on Savannah River Site Charcoal Stack Samples

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

    Lahoda, Kristy G.; Engelmann, Mark D.; Farmer, Orville T.

    2008-03-01

    Experimental results are provided for the sample analyses for technetium (Tc) in charcoal samples placed in-line with a Savannah River Site (SRS) processing stack effluent stream as a part of an environmental surveillance program. The method for Tc removal from charcoal was based on that originally developed with high purity charcoal. Presented is the process that allowed for the quantitative analysis of 99Tc in SRS charcoal stack samples with and without 97Tc as a tracer. The results obtained with the method using the 97Tc tracer quantitatively confirm the results obtained with no tracer added. All samples contain 99Tc at themore » pg g-1 level.« less

  16. Development of a gas-pressurized high-pressure μSR setup at the RIKEN-RAL Muon Facility

    NASA Astrophysics Data System (ADS)

    Watanabe, I.; Ishii, Y.; Kawamata, T.; Suzuki, T.; Pratt, F. L.; Done, R.; Chowdhury, M.; Goodway, C.; Dreyer, J.; Smith, C.; Southern, M.

    2009-04-01

    The development and testing of a gas-pressurized μSR setup for the RIKEN-RAL Muon Facility is reported. In collaboration with the high-pressure group of the ISIS Facility at the Rutherford Appleton Laboratory, a gas-pressurized setup for a pulsed muon beam at the RIKEN-RAL Muon Facility has been constructed in 2008. The sample is pressurized by helium gas and the designed maximum pressure is 6.4 kbar. The high-pressure cell can be cooled down to 2 K using an existing cryostat. Tests were made injecting the double-pulsed muon beam into a high-purity sample of Sn powder, which confirmed that the maximum pressure achieved at 2 K was close to the designed pressure.

  17. 3D modeling of unconstrained HPT process: role of strain gradient on high deformed microstructure formation

    NASA Astrophysics Data System (ADS)

    Ben Kaabar, A.; Aoufi, A.; Descartes, S.; Desrayaud, C.

    2017-05-01

    During tribological contact’s life, different deformation paths lead to the formation of high deformed microstructure, in the near-surface layers of the bodies. The mechanical conditions (high pressure, shear) occurring under contact, are reproduced through unconstrained High Pressure Torsion configuration. A 3D finite element model of this HPT test is developed to study the local deformation history leading to high deformed microstructure with nominal pressure and friction coefficient. For the present numerical study the friction coefficient at the interface sample/anvils is kept constant at 0.3; the material used is high purity iron. The strain distribution in the sample bulk, as well as the main components of the strain gradients according to the spatial coordinates are investigated, with rotation angle of the anvil.

  18. Research and preparation of ultra purity silicon tetrachloride

    NASA Astrophysics Data System (ADS)

    Wan, Ye; Zhao, Xiong; Yan, Dazhou; Yang, Dian; Li, Yunhao; Guo, Shuhu

    2017-10-01

    This article demonstrated a technology for producing ultra-purity silicon tetrachloride, which using the high purity SiCl4 as raw material through the method of combination ray reaction with purification. This technology could remove metal impurities and compounds impurities contained hydrogen effectively. The purity of product prepared by this technology can reach at 99.9999%, content of metal impurities can be low at 0.3PPb, meeting the requirement of industry easily. This technology has the advantages of simple process, continuous operation, and stable performance.

  19. Nuclear forensic analysis of uranium oxide powders interdicted in Victoria, Australia

    DOE PAGES

    Kristo, Michael Joseph; Keegan, Elizabeth; Colella, Michael; ...

    2015-04-13

    Nuclear forensic analysis was conducted on two uranium samples confiscated during a police investigation in Victoria, Australia. The first sample, designated NSR-F-270409-1, was a depleted uranium powder of moderate purity (~1000 μg/g total elemental impurities). The chemical form of the uranium was a compound similar to K 2(UO 2) 3O 4·4H 2O. While aliquoting NSR-F-270409-1 for analysis, the body and head of a Tineid moth was discovered in the sample. The second sample, designated NSR-F-270409-2, was also a depleted uranium powder. It was of reasonably high purity (~380 μg/g total elemental impurities). The chemical form of the uranium was primarilymore » UO 3·2H 2O, with minor phases of U 3O 8 and UO 2. While aliquoting NSR-F-270409-2 for analysis, a metal staple of unknown origin was discovered in the sample. The presence of 236U and 232U in both samples indicates that the uranium feed stocks for these samples experienced a neutron flux at some point in their history. The reactor burn-up calculated from the isotopic composition of the uranium is consistent with that of spent fuel from natural uranium (NU) fueled Pu production. These nuclear forensic conclusions allow us to categorically exclude Australia as the origin of the material and greatly reduce the number of candidate sources.« less

  20. 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

  1. Low cycle fatigue of PM/HIP astroloy

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

    Choe, S.J.; Stoloff, N.S.; Duquette, D.J.

    Low cycle fatigue and creep-fatigue-environment interactions of PM/HIP Astrology were studied at 650 C and 725 C. Total strain range was varied from 1.5% to 2.7% at a frequency of 0.3Hz. Creep-fatigue tests were performed with 2 min. or 5 min. tensile hold times. All tests were run in high purity argon in an attempt to minimize environmental effects. Employing a tensile hold was more damaging than raising temperature by 75 C. Slopes of Coffin-Manson plots were nearly independent of temperature and hold time. Raising temperature from 650 C to 725 C did not change the transgranular (TG) crack propagationmore » mode, whereas employing hold times caused TG+IG propagation. All samples displayed multiple fracture origins associated with inclusions located at the specimen surface; pre-existing pores did not affect fatigue crack initiation. Examination of secondary cracks showed no apparent creep damage. Oxidation in high purity argon appeared to be the major factor in LCF life degradation due to hold times.« less

  2. 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.

  3. The Physics and Chemistry of carbides, Nitrides and Borides. Volume 185

    DTIC Science & Technology

    1990-01-01

    and C-B-C chains [15,17]. Clearly, the use of boron-rich solids as electronic materials will place new demands on the quality of materials. In this...first heated in a pyrolytic boron nitride (PBN) crucible ( Union Carbide Corp.) under high vacuum (< 50 mTorr) to 1900°C. This removed surface...contamination of the sample. The powders were loaded into a graphite die with a high-purity BN die liner ( Union Carbide Grade HBC) with inner diameter of 3/8

  4. Crystalline nucleation in undercooled liquids: a Bayesian data-analysis approach for a nonhomogeneous Poisson process.

    PubMed

    Filipponi, A; Di Cicco, A; Principi, E

    2012-12-01

    A Bayesian data-analysis approach to data sets of maximum undercooling temperatures recorded in repeated melting-cooling cycles of high-purity samples is proposed. The crystallization phenomenon is described in terms of a nonhomogeneous Poisson process driven by a temperature-dependent sample nucleation rate J(T). The method was extensively tested by computer simulations and applied to real data for undercooled liquid Ge. It proved to be particularly useful in the case of scarce data sets where the usage of binned data would degrade the available experimental information.

  5. Continuous Ultra-Thin MOS2 Films Grown by Low-Temperature Physical Vapor Deposition (Postprint)

    DTIC Science & Technology

    2014-07-01

    MoS2 target of 99.95% purity. The SiO2 and highly oriented pyrolitic graphite (HOPG) substrates were intro- duced via a vacuum load- lock and mounted on...im- mediately prior insertion into a sample vacuum load- lock . In this work, the samples were heated to 350 C and allowed to rotate at approximately...136805 (2010). 6H. Terrones, F. Lopez-Urias, and M. Terrones, Sci. Rep. 3(203), 1549 (2013). 7H. Li, Q. Zhang, C. C. R. Yap, B. K. Tay, T. H. T. Edwin

  6. 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.

  7. 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.

  8. Isolation and purification of series bioactive components from Hypericum Perforatum L. by high-speed counter-current chromatography

    PubMed Central

    Cao, Xueli; Wang, Qiaoe; Li, Yan; Bai, Ge; Ren, Hong; Ito, Yiochiro

    2011-01-01

    High-speed counter-current chromatography (HSCCC) combined with pre-separation by ultrasonic solvent extraction was successively used for the separation of series bioactive compounds from the crude extract of Hypericum perforatum L. The petroleum ether extract was separated by the solvent system of n-heptane-methanol-acetonitrile (1.5:0.5:0.5, v/v) and n-heptane-methanol (1.5:1, v/v) in gradient elution, yielding a phloroglucinol compound, hyperforin with HPLC purity over 98%. The ethyl acetate extract was separated by using the solvent system composed of hexane-ethyl acetate-methanol-water (1:1:1:1 and 1:3:1:3, v/v) in gradient through both reverse phase and normal phase elution mode, yielding a naphthodianthrone compound, hypericin with HPLC purity about 95%. The n-butanol extract was separated with the solvent system composed of n-butanol-ethyl acetate–water (1:4:5 and 1.5:3.5:5, v/v) in elution and back-extrusion mode, yielding two of flavones, rutin and hyperoside, with HPLC purity over 95%. HPLC-MS, reference sample and UV spectrum were selectively used in separation to search for target compounds from HPLC-DAD profiles of different sub-extracts. The structures of isolated compounds were further identified by ESI-MS, 1HNMR and 13CNMR. PMID:21306961

  9. Procedure for chromatography involving sample solvent with higher elution strength than the mobile phase.

    PubMed

    Patil, Nitin S; Mendhe, Rakesh B; Sankar, Ajeet A; Iyer, Harish

    2008-01-11

    In preparative chromatography, often the solubility of the sample in the mobile phase is limited, making the mobile phase unsuitable as a solvent for preparation of load. Generally, solvents that have high solubility for the sample also have higher elution strengths than the mobile phase. Additionally, at high loading volumes, these strong sample solvents are known to adversely affect the band profiles leading to poor chromatographic performance. Here, we show that controlling the mobile phase strength during loading and post-load elution resulted in improved band profiles when the sample solvent was stronger than the mobile phase. Such an approach improves performance in preparative chromatography by allowing either higher sample loading or higher organic content in mobile phase (without loss of yield). Alternately, the approach can be used for improvement in performance by increase in yield or product purity.

  10. 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.

  11. Characteristics of high-purity Teflon vial for 14C measurement in old tree rings

    NASA Astrophysics Data System (ADS)

    Sakurai, H.; Saswaki, Y.; Matsumoto, T.; Aoki, T.; Kato, W.; Gandou, T.; Gunji, S.; Tokanai, F.

    2003-06-01

    14C concentration in single-year tree rings of an old cedar of ca. 2500 years ago is measured to investigate the 11-yr periodicity of solar activity. Our highly accurate 14C measuring system is composed of a benzene synthesizer capable of producing a large quantity (10 g) of benzene and a Quantulus 1220™ liquid scintillation counting system. The accuracy is less than 0.2% for measurements of 14C concentration. The benzene sample is contained in a high-purity Teflon/copper-counting vial (20 ml) manufactured by Wallac Oy Company. We found a vial with an irregular copper cap for the measurements of 11 tree rings. The behavior of the vial with the irregular cap was investigated. The Teflon sheet inside the cap plays an important role in achieving stable measurement. The rate of volatilization of the benzene was less than 0.35 mg/day for vials with ordinary caps. This results in the volatilization rate of 0.003% for 10.5 g of benzene and hence guarantees measurement at an accuracy of 0.2% for 70 days.

  12. Indices of polarimetric purity for biological tissues inspection

    NASA Astrophysics Data System (ADS)

    Van Eeckhout, Albert; Lizana, Angel; Garcia-Caurel, Enric; Gil, José J.; Sansa, Adrià; Rodríguez, Carla; Estévez, Irene; González, Emilio; Escalera, Juan C.; Moreno, Ignacio; Campos, Juan

    2018-02-01

    We highlight the interest of using the Indices of Polarimetric Purity (IPPs) for the biological tissue inspection. These are three polarimetric metrics focused on the study of the depolarizing behaviour of the sample. The IPPs have been recently proposed in the literature and provide different and synthetized information than the commonly used depolarizing indices, as depolarization index (PΔ) or depolarization power (Δ). Compared with the standard polarimetric images of biological samples, IPPs enhance the contrast between different tissues of the sample and show differences between similar tissues which are not observed using the other standard techniques. Moreover, they present further physical information related to the depolarization mechanisms inherent to different tissues. In addition, the algorithm does not require advanced calculations (as in the case of polar decompositions), being the indices of polarimetric purity fast and easy to implement. We also propose a pseudo-coloured image method which encodes the sample information as a function of the different indices weights. These images allow us to customize the visualization of samples and to highlight certain of their constitutive structures. The interest and potential of the IPP approach are experimentally illustrated throughout the manuscript by comparing polarimetric images of different ex-vivo samples obtained with standard polarimetric methods with those obtained from the IPPs analysis. Enhanced contrast and retrieval of new information are experimentally obtained from the different IPP based images.

  13. Design of Experiment Analysis of the Sulzer Metco DJ High Velocity Oxy-Fuel Coating of Hydroxyapatite for Orthopedic Applications

    NASA Astrophysics Data System (ADS)

    Hasan, S.; Stokes, J.

    2011-01-01

    High Velocity Oxy-Fuel (HVOF) has the potential to produce hydroxyapatite (HA; Bio-ceramic) coatings based on its experience with other sprayed ceramic materials. This technique should offer mechanical and biological results comparable to other thermal spraying processes, such as atmospheric plasma thermal spray, currently FDA approved for HA deposition. Deposition of HA via HVOF is a new venture especially using the Sulzer Metco Diamond Jet (DJ) process, and the aim of this article was to establish this technique's potential in providing superior HA coating results compared to the FDA-approved plasma spray technique. In this research, a Design of Experiment (DOE) model was developed to optimize the Sulzer Metco DJ HVOF process for the deposition of HA. In order to select suitable ranges for the production of HA coatings, the parameters were first investigated. Five parameters (factors) were researched over two levels namely: oxygen flow rate, propylene flow rate, air flow rate, spray distance, and powder flow rate. Coating crystallinity and purity were measured at the surface of each sample as the responses to the factors used. The research showed that propylene, air flow rate, spray distance, and powder feed rate had the largest effect on the responses, and the study aimed to find the preferred optimized settings to achieve high crystallinity and purity of percentages of up to 95%. This research found crystallinity and purity values of 93.8 and 99.8%, respectively, for a set of HVOF parameters which showed improvement compared to the crystallinity and purity values of 87.6 and 99.4%, respectively, found using the FDA-approved Sulzer Metco Atmospheric Plasma thermal spray process. Hence, a new technique for HA deposition now exists using the DJ HVOF facility; however, other mechanical and biorelated properties must also be assessed.

  14. Synthesis and characterization of CMC from water hyacinth for lithium-ion battery applications

    NASA Astrophysics Data System (ADS)

    Hidayat, Sahrul; Susanty, Riveli, Nowo; Suroto, Bambang Joko; Rahayu, Iman

    2018-02-01

    Recently, the most dominating power supply on the mobile electronics market are rechargeable Lithium-ion batteries. This is because of a higher energy density and longer lifetime compared to similar rechargeable battery systems. One of the components that determine the performance of a lithium ion battery is the binder material, whether at the anode or the cathode. In commercial batteries, the material used as the binder is Polyvinylidene Difluoride (PVDF), with n-methyl-2-phyrrolidone (NMP) as the solvent. Both are synthetic materials that are expensive, toxic and harmful to the environment. An alternative binder material for lithium-ion battery electrodes is CMC (carboxymethyl cellulose) in a water solvent. CMC is cheaper than PVDF, non-toxic and more environmental friendly. CMC can be synthesized from several types of plants, such as water hyacinth, which is a weed plant with high cellulose content. The synthesis of CMC consists of three main steps, namely 1) the isolation process from water hyacinth, 2) the alkalization and carboxymethylation process and 3) the purification process to obtain CMC in high purity. FTIR characterization of the CMC shows five region of absorption bands. The bands in the region 1330-1400 cm-1 are due to symmetrical deformations of CH2 and OH groups. The ether bonds in CMC occur in the fingerprint region of 1250-1060 cm-1. The presence of new and strong absorption band around 1600 cm-1 is confirmed to the stretching vibration of the carboxyl group (COO-), while the one around 1415 cm-1 is assigned to carboxyl groups as it salts. The broad absorption band above 3400 cm-1 is due to the stretching frequency of the hydroxyl group (-OH). Purity test on three samples (CMC mesh-100, CMC mesh-60 and CMC, mesh-40) gives purity values of 99.89%, 99.99% and 99.89%, respectively. This proves that CMC have actually been formed with high purity.

  15. Micro and Nano Laser Pulses for Melting and Surface Alloying of Aluminum with Copper

    NASA Astrophysics Data System (ADS)

    Hamoudi, Walid K.; Ismail, Raid A.; Sultan, Fatima I.; Jaleel, Summayah

    2017-03-01

    In the present work, the use of microsecond and nanosecond laser pulses to alloy copper in aluminum is presented. In the first run, high purity (99.999%) copper thin film was thermally evaporated over (99.9%) purity, 300 μm aluminum sheet. Thereafter, surface alloying was performed using (1-3) 500 μs, (0.1-1.5) Joule Nd: YAG laser pulses; operating at 1060 nm wavelength. Hard homogeneous alloyed zone was obtained at depths between 60 and 110 μm below the surface. In the second run, 9 ns laser pulses from Q-switched Nd: YAG laser operating at 1060 nm was employed to melt/alloy Al-Cu sheets. The resulted alloyed depth, after using 20 laser pulses, was 199.22 μm for Al over Cu samples and 419.61 μm for Cu over Al samples. X-ray diffraction and fluorescence analysis revealed the formation of Cu2Al2, CuAl2 and δ- Al4Cu9 phases with percentage depended on laser energy and copper layer thicknesses.

  16. Optimizing the multicycle subrotational internal cooling of diatomic molecules

    NASA Astrophysics Data System (ADS)

    Aroch, A.; Kallush, S.; Kosloff, R.

    2018-05-01

    Subrotational cooling of the AlH+ ion to the miliKelvin regime, using optimally shaped pulses, is computed. The coherent electromagnetic fields induce purity-conserved transformations and do not change the sample temperature. A decrease in a sample temperature, manifested by an increase of purity, is achieved by the complementary uncontrolled spontaneous emission which changes the entropy of the system. We employ optimal control theory to find a pulse that stirs the system into a population configuration that will result in cooling, upon multicycle excitation-emission steps. The obtained optimal transformation was shown capable to cool molecular ions to the subkelvins regime.

  17. 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.

  18. PRex: An Experiment to Investigate Detection of Near-field Particulate Deposition from a Simulated Underground Nuclear Weapons Test Vent

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

    Keillor, Martin E.; Arrigo, Leah M.; Baciak, James E.

    2016-01-01

    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 capability development activities. For this experiment, a CO2-driven “air cannon” was used to release lanthanum-140 at ambient temperatures. The radioisotope 140La was chosen as a representative fission fragment with a short half-life and prominent gamma-ray emissions; the choice was also influenced by the successful production and use of 140La with low levels of radioactive contaminants in the Defence Research and Development Canada Field Trials. The source was created through activation of high-purity lanthanum oxide at themore » TRIGA research reactor of Washington State University, Pullman, Washington. Witness plates and air samplers were laid out in an irregular grid covering the area for which the plume was anticipated to deposit based on climatological wind records. A vehicle-mounted spectrometer, and handheld and backpack instruments ranging from polyvinyl toluene to high purity germanium, were used to survey the plume. Additionally, three soil sampling techniques were investigated. The relative sensitivity and utility of sampling and survey methods are discussed in the context of On-Site Inspection.« less

  19. Rmax: A systematic approach to evaluate instrument sort performance using center stream catch☆

    PubMed Central

    Riddell, Andrew; Gardner, Rui; Perez-Gonzalez, Alexis; Lopes, Telma; Martinez, Lola

    2015-01-01

    Sorting performance can be evaluated with regard to Purity, Yield and/or Recovery of the sorted fraction. Purity is a check on the quality of the sample and the sort decisions made by the instrument. Recovery and Yield definitions vary with some authors regarding both as how efficient the instrument is at sorting the target particles from the original sample, others distinguishing Recovery from Yield, where the former is used to describe the accuracy of the instrument’s sort count. Yield and Recovery are often neglected, mostly due to difficulties in their measurement. Purity of the sort product is often cited alone but is not sufficient to evaluate sorting performance. All of these three performance metrics require re-sampling of the sorted fraction. But, unlike Purity, calculating Yield and/or Recovery calls for the absolute counting of particles in the sorted fraction, which may not be feasible, particularly when dealing with rare populations and precious samples. In addition, the counting process itself involves large errors. Here we describe a new metric for evaluating instrument sort Recovery, defined as the number of particles sorted relative to the number of original particles to be sorted. This calculation requires only measuring the ratios of target and non-target populations in the original pre-sort sample and in the waste stream or center stream catch (CSC), avoiding re-sampling the sorted fraction and absolute counting. We called this new metric Rmax, since it corresponds to the maximum expected Recovery for a particular set of instrument parameters. Rmax is ideal to evaluate and troubleshoot the optimum drop-charge delay of the sorter, or any instrument related failures that will affect sort performance. It can be used as a daily quality control check but can be particularly useful to assess instrument performance before single-cell sorting experiments. Because we do not perturb the sort fraction we can calculate Rmax during the sort process, being especially valuable to check instrument performance during rare population sorts. PMID:25747337

  20. Size dependent exchange bias in single-phase Zn0.3Ni0.7Fe2O4 ferrite nanoparticles

    NASA Astrophysics Data System (ADS)

    Mohan, Rajendra; Ghosh, Mritunjoy Prasad; Mukherjee, Samrat

    2018-07-01

    We report the microstructural and magnetic characterization of single phase nanocrystalline partially inverted Zn0.3Ni0.7Fe2O4 mixed spinel ferrite. The samples were annealed at 200 °C, 400 °C, 600 °C, 800 °C and 1000 °C. X-ray diffraction results indicate phase purity of all the samples and application of Debye- Scherrer yielded a crystallite size variation from 5 nm to 33 nm for the different samples. Magnetic measurements have revealed the freezing of interfacial spins which were the cause of the large horizontal M-H loop shift causing large exchange bias with high anisotropy. The magnetic measurements show a hysteresis loop with high effective anisotropy constant due to highly magnetically disordered surface spin at 5 K.

  1. Synthesis and characterization of Zn-Mg ferrite

    NASA Astrophysics Data System (ADS)

    Singh, Shailndra; Barbar, S. K.; Ram, Sahi

    2018-05-01

    The Zn-Mg ferrite sample of general formula Zn0.5Mg0.5Fe2O4 have been prepared by standard solid state reaction technique using high purity oxides. X-ray diffraction analysis shows the formation of a zinc-magnesium ferrite cubic phase at room temperature with space group Fd3m. FTIR spectra show two significant absorption bands first at 665.15 cm-1 corresponding to tetrahedral (A) and second band at 434 cm-1 corresponding to octahedral (B) sites of the spinel. Morphology of the sample determined by the SEM measurement and EDS analysis has confirmed the composition of atoms in the sample.

  2. CMV-specific T cell isolation from G-CSF mobilized peripheral blood: depletion of myeloid progenitors eliminates non-specific binding of MHC-multimers.

    PubMed

    Beloki, Lorea; Ciaurriz, Miriam; Mansilla, Cristina; Zabalza, Amaya; Perez-Valderrama, Estela; Samuel, Edward R; Lowdell, Mark W; Ramirez, Natalia; Olavarria, Eduardo

    2014-11-19

    Cytomegalovirus (CMV)-specific T cell infusion to immunocompromised patients following allogeneic Hematopoietic Stem Cell Transplantation (allo-HSCT) is able to induce a successful anti-viral response. These cells have classically been manufactured from steady-state apheresis samples collected from the donor in an additional harvest prior to G-CSF mobilization, treatment that induces hematopoietic stem cell (HSC) mobilization to the periphery. However, two closely-timed cellular collections are not usually available in the unrelated donor setting, which limits the accessibility of anti-viral cells for adoptive immunotherapy. CMV-specific cytotoxic T cell (CTL) manufacture from the same G-CSF mobilized donor stem cell harvest offers great regulatory advantages, but the isolation using MHC-multimers is hampered by the high non-specific binding to myeloid progenitors, which reduces the purity of the cellular product. In the present study we describe an easy and fast method based on plastic adherence to remove myeloid cell subsets from 11 G-CSF mobilized donor samples. CMV-specific CTLs were isolated from the non-adherent fraction using pentamers and purity and yield of the process were compared to products obtained from unmanipulated samples. After the elimination of unwanted cell subtypes, non-specific binding of pentamers was notably reduced. Accordingly, following the isolation process the purity of the obtained cellular product was significantly improved. G-CSF mobilized leukapheresis samples can successfully be used to isolate antigen-specific T cells with MHC-multimers to be adoptively transferred following allo-HSCT, widening the accessibility of this therapy in the unrelated donor setting. The combination of the clinically translatable plastic adherence process to the antigen-specific cell isolation using MHC-multimers improves the quality of the therapeutic cellular product, thereby reducing the clinical negative effects associated with undesired alloreactive cell infusion.

  3. 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

  4. 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.

  5. Analysis of cocaine and its adulterants in drugs for international trafficking seized by the Brazilian Federal Police.

    PubMed

    Lapachinske, Silvio Fernandes; Okai, Guilherme Gonçalves; dos Santos, Ariana; de Bairros, André Valle; Yonamine, Mauricio

    2015-02-01

    Here, gas chromatography with nitrogen phosphorous detector (GC-NPD) method was developed and validated for the quantification of cocaine and adulterants (caffeine, 4-dimethylaminoantipyrine, levamisole, lidocaine and phenacetin) in illicit samples. The method was based on direct dilution of samples in methanol, sonication for 5 min and centrifugation. After appropriate dilution, an aliquot was injected into GC-MS in order to identify the active compounds and into GC-NPD for the analytes quantification. Bupivacaine was used as an internal standard. The method showed to be precise, accurate and linear over a range of 0.5-100% (weight/weight percentages) for all analytes, except phenacetin which showed a linear range between 2% and 100%. The method was successfully applied to 54 samples seized by the Brazilian Federal Police in the International Airport of Sao Paulo and mailing services during the year 2011. All the samples were associated with international trafficking and were apprehended while leaving the country. The purity of cocaine ranged from 16.5% to 91.4%. Cocaine was the only detected active compound in 29.6% of total samples. Among the identified cutting agents, levamisole was the most abundant (55.6% of the total samples) and relative concentrations (weight/weight percentages) ranged from 0.7% to 23%. Lidocaine, caffeine, phenacetin and 4-dimethylaminoantipyrine were also identified in these samples in minor concentrations. In contrast with what we initially hypothesized, drugs intended to international trafficking did not present high cocaine purity and most of the samples were laced with adulterants before leaving Brazil. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  6. 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

  7. Microfluidic device with integrated microfilter of conical-shaped holes for high efficiency and high purity capture of circulating tumor cells

    NASA Astrophysics Data System (ADS)

    Tang, Yadong; Shi, Jian; Li, Sisi; Wang, Li; Cayre, Yvon E.; Chen, Yong

    2014-08-01

    Capture of circulating tumor cells (CTCs) from peripheral blood of cancer patients has major implications for metastatic detection and therapy analyses. Here we demonstrated a microfluidic device for high efficiency and high purity capture of CTCs. The key novelty of this approach lies on the integration of a microfilter with conical-shaped holes and a micro-injector with cross-flow components for size dependent capture of tumor cells without significant retention of non-tumor cells. Under conditions of constant flow rate, tumor cells spiked into phosphate buffered saline could be recovered and then cultured for further analyses. When tumor cells were spiked in blood of healthy donors, they could also be recovered at high efficiency and high clearance efficiency of white blood cells. When the same device was used for clinical validation, CTCs could be detected in blood samples of cancer patients but not in that of healthy donors. Finally, the capture efficiency of tumor cells is cell-type dependent but the hole size of the filter should be more closely correlated to the nuclei size of the tumor cells. Together with the advantage of easy operation, low-cost and high potential of integration, this approach offers unprecedented opportunities for metastatic detection and cancer treatment monitoring.

  8. An Efficient Protocol for Preparation of Gallic Acid from Terminalia bellirica (Gaertn.) Roxb by Combination of Macroporous Resin and Preparative High-Performance Liquid Chromatography.

    PubMed

    Zou, Denglang; Chen, Tao; Chen, Chen; Li, Hongmei; Liu, Yongling; Li, Yulin

    2016-08-01

    In this article, macroporous resin column chromatography and preparative high-performance liquid chromatography were applied for preparation of gallic acid from Terminalia bellirica (Gaertn.) Roxb. In the first step, six kinds of resins were investigated by adsorption and desorption tests and AB-8 macroporous resin was selected for the enrichment of gallic acid. As a result, 20 g of gallic acid at a purity of 71% could be separated from 100 g of crude extract in which the content of gallic acid was 16.7% and the recovery of gallic acid reached 85.0%. In the second step, preparative high-performance liquid chromatography was selected to purify gallic acid. As a result, 640 mg of gallic acid at a purity of 99.1% was obtained from 1 g of sample in 35 min. The results demonstrated that macroporous resin coupled with preparative high-performance liquid chromatography was suitable for preparation of gallic acid from T. bellirica (Gaertn.) Roxb. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. DMS cyclone separation processes for optimization of plastic wastes recycling and their implications.

    PubMed

    Gent, Malcolm Richard; Menendez, Mario; Toraño, Javier; Torno, Susana

    2011-06-01

    It is demonstrated that substantial reductions in plastics presently disposed of in landfills can be achieved by cyclone density media separation (DMS). In comparison with the size fraction of plastics presently processed by industrial density separations (generally 6.4 to 9.5 mm), cyclone DMS methods are demonstrated to effectively process a substantially greater range of particle sizes (from 0.5 up to 120 mm). The purities of plastic products and recoveries obtained with a single stage separation using a cylindrical cyclone are shown to attain virtually 100% purity and recoveries >99% for high-density fractions and >98% purity and recoveries were obtained for low-density products. Four alternative schemas of multi-stage separations are presented and analyzed as proposed methods to obtain total low- and high-density plastics fraction recoveries while maintaining near 100% purities. The results of preliminary tests of two of these show that the potential for processing product purities and recoveries >99.98% of both density fractions are indicated. A preliminary economic comparison of capital costs of DMS systems suggests cyclone DMS methods to be comparable with other DMS processes even if the high volume capacity for recycling operations of these is not optimized.

  10. 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.

  11. 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.

  12. 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.

  13. A versatile design for resonant guided-wave parametric down-conversion sources for quantum repeaters

    NASA Astrophysics Data System (ADS)

    Brecht, Benjamin; Luo, Kai-Hong; Herrmann, Harald; Silberhorn, Christine

    2016-05-01

    Quantum repeaters—fundamental building blocks for long-distance quantum communication—are based on the interaction between photons and quantum memories. The photons must fulfil stringent requirements on central frequency, spectral bandwidth and purity in order for this interaction to be efficient. We present a design scheme for monolithically integrated resonant photon-pair sources based on parametric down-conversion in nonlinear waveguides, which facilitate the generation of such photons. We investigate the impact of different design parameters on the performance of our source. The generated photon spectral bandwidths can be varied between several tens of MHz up to around 1 GHz, facilitating an efficient coupling to different memories. The central frequency of the generated photons can be coarsely tuned by adjusting the pump frequency, poling period and sample temperature, and we identify stability requirements on the pump laser and sample temperature that can be readily fulfilled with off-the-shelf components. We find that our source is capable of generating high-purity photons over a wide range of photon bandwidths. Finally, the PDC emission can be frequency fine-tuned over several GHz by simultaneously adjusting the sample temperature and pump frequency. We conclude our study with demonstrating the adaptability of our source to different quantum memories.

  14. UPLC-MS/MS determination of ptaquiloside and pterosin B in preserved natural water.

    PubMed

    Clauson-Kaas, Frederik; Hansen, Hans Christian Bruun; Strobel, Bjarne W

    2016-11-01

    The naturally occurring carcinogen ptaquiloside and its degradation product pterosin B are found in water leaching from bracken stands. The objective of this work is to present a new sample preservation method and a fast UPLC-MS/MS method for quantification of ptaquiloside and pterosin B in environmental water samples, employing a novel internal standard. A faster, reliable, and efficient method was developed for isolation of high purity ptaquiloside and pterosin B from plant material for use as analytical standards, with purity verified by 1 H-NMR. The chemical analysis was performed by cleanup and preconcentration of samples with solid phase extraction, before analyte quantification with UPLC-MS/MS. By including gradient elution and optimizing the liquid chromatography mobile phase buffer system, a total run cycle of 5 min was achieved, with method detection limits, including preconcentration, of 8 and 4 ng/L for ptaquiloside and pterosin B, respectively. The use of loganin as internal standard improved repeatability of the determination of both analytes, though it could not be employed for sample preparation. Buffering raw water samples in situ with ammonium acetate to pH ∼5.5 decisively increased sample integrity at realistic transportation and storing conditions prior to extraction. Groundwater samples collected in November 2015 at the shallow water table below a Danish bracken stand were preserved and analyzed using the above methods, and PTA concentrations of 3.8 ± 0.24 μg/L (±sd, n = 3) were found, much higher than previously reported. Graphical abstract Workflow overview of ptaquiloside determination.

  15. 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.

  16. Purity and cleanness of aerogel as a cosmic dust capture medium

    NASA Technical Reports Server (NTRS)

    Tsou, P.; Fleming, R. H.; Lindley, P. M.; Craig, A. Y.; Blake, D.

    1994-01-01

    The capability for capturing micrometeoroids intact through laboratory simulations and in space in passive underdense silica aerogel offers a valuable tool for cosmic dust research. The integrity of the sample handling medium can substantially modify the integrity of the sample. Intact capture is a violent hypervelocity event: the integrity of the capturing medium can cause even greater modification of the sample. Doubts of the suitability of silica aerogel as a capture medium were raised at the 20th LPSC, and questions were raised again at the recent workshop on Particle Capture, Recovery, and Velocity Trajectory Measurement Technologies. Assessment of aerogel's volatile components and carbon contents have been made. We report the results of laboratory measurements of the purity and cleanliness of silica aerogel used for several Sample Return Experiments flown on the Get Away Special program.

  17. 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.

  18. Process Simulation and Modeling for Advanced Intermetallic Alloys.

    DTIC Science & Technology

    1994-06-01

    calorimetry, using a Stanton Redfera/Omnitherm DOC 1500 thermal analysis system, was the primary experimental tool for this investigation...samples during both heating and cooling in a high purity argon atmosphere at a rate of 20K/min. The DSC instrumental baseline was obtained using both empty...that is capable of fitting the observed data to given cell structures using a least squares procedure. RESULTS The results of the DOC observations are

  19. Development Of A Magnetic Directional-Solidification Furnace

    NASA Technical Reports Server (NTRS)

    Aldrich, Bill R.; Lehoczky, Sandor L.

    1996-01-01

    Report describes development of directional-solidification furnace in which axial magnetic field is imposed by surrounding ring permanent magnets and/or electromagnets and pole pieces. Furnace provides controlled axial temperature gradients in multiple zones, through which ampoule containing sample of material to be solidified is translated at controlled speed by low-vibration, lead-screw, stepping-motor-driven mechanism. Intended for use in low-gravity (spaceflight) experiments on melt growth of high-purity semiconductor crystals.

  20. Signal recognition efficiencies of artificial neural-network pulse-shape discrimination in HPGe -decay searches

    NASA Astrophysics Data System (ADS)

    Caldwell, A.; Cossavella, F.; Majorovits, B.; Palioselitis, D.; Volynets, O.

    2015-07-01

    A pulse-shape discrimination method based on artificial neural networks was applied to pulses simulated for different background, signal and signal-like interactions inside a germanium detector. The simulated pulses were used to investigate variations of efficiencies as a function of used training set. It is verified that neural networks are well-suited to identify background pulses in true-coaxial high-purity germanium detectors. The systematic uncertainty on the signal recognition efficiency derived using signal-like evaluation samples from calibration measurements is estimated to be 5 %. This uncertainty is due to differences between signal and calibration samples.

  1. 65Zn and 133Ba standardizing by photon-photon coincidence counting

    NASA Astrophysics Data System (ADS)

    Loureiro, Jamir S.; da Cruz, Paulo A. L.; Iwahara, Akira; Delgado, José U.; Lopes, Ricardo T.

    2018-03-01

    The LNMRI/Brazil has deployed a system using X-gamma coincidence technique for the standardizing radionuclide, which present simple and complex decay scheme with X-rays of energy below 100 keV. The work was carried on radionuclide metrology laboratory using a sodium iodide detector, for gamma photons, in combination with a high purity germanium detector for X-rays. Samples of 65Zn and 133Ba were standardized and the results for both radionuclides showed good precision and accuracy when compared with reference values. The standardization differences were 0.72 % for 65Zn and 0.48 % for 133Ba samples.

  2. Comparing the efficiency of digital and conventional soil mapping to predict soil types in a semi-arid region in Iran

    NASA Astrophysics Data System (ADS)

    Zeraatpisheh, Mojtaba; Ayoubi, Shamsollah; Jafari, Azam; Finke, Peter

    2017-05-01

    The efficiency of different digital and conventional soil mapping approaches to produce categorical maps of soil types is determined by cost, sample size, accuracy and the selected taxonomic level. The efficiency of digital and conventional soil mapping approaches was examined in the semi-arid region of Borujen, central Iran. This research aimed to (i) compare two digital soil mapping approaches including Multinomial logistic regression and random forest, with the conventional soil mapping approach at four soil taxonomic levels (order, suborder, great group and subgroup levels), (ii) validate the predicted soil maps by the same validation data set to determine the best method for producing the soil maps, and (iii) select the best soil taxonomic level by different approaches at three sample sizes (100, 80, and 60 point observations), in two scenarios with and without a geomorphology map as a spatial covariate. In most predicted maps, using both digital soil mapping approaches, the best results were obtained using the combination of terrain attributes and the geomorphology map, although differences between the scenarios with and without the geomorphology map were not significant. Employing the geomorphology map increased map purity and the Kappa index, and led to a decrease in the 'noisiness' of soil maps. Multinomial logistic regression had better performance at higher taxonomic levels (order and suborder levels); however, random forest showed better performance at lower taxonomic levels (great group and subgroup levels). Multinomial logistic regression was less sensitive than random forest to a decrease in the number of training observations. The conventional soil mapping method produced a map with larger minimum polygon size because of traditional cartographic criteria used to make the geological map 1:100,000 (on which the conventional soil mapping map was largely based). Likewise, conventional soil mapping map had also a larger average polygon size that resulted in a lower level of detail. Multinomial logistic regression at the order level (map purity of 0.80), random forest at the suborder (map purity of 0.72) and great group level (map purity of 0.60), and conventional soil mapping at the subgroup level (map purity of 0.48) produced the most accurate maps in the study area. The multinomial logistic regression method was identified as the most effective approach based on a combined index of map purity, map information content, and map production cost. The combined index also showed that smaller sample size led to a preference for the order level, while a larger sample size led to a preference for the great group level.

  3. 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.

  4. 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

  5. On evaluating clustering procedures for use in classification

    NASA Technical Reports Server (NTRS)

    Pore, M. D.; Moritz, T. E.; Register, D. T.; Yao, S. S.; Eppler, W. G. (Principal Investigator)

    1979-01-01

    The problem of evaluating clustering algorithms and their respective computer programs for use in a preprocessing step for classification is addressed. In clustering for classification the probability of correct classification is suggested as the ultimate measure of accuracy on training data. A means of implementing this criterion and a measure of cluster purity are discussed. Examples are given. A procedure for cluster labeling that is based on cluster purity and sample size is presented.

  6. Purity analyses of high-purity organic compounds with nitroxyl radicals based on the Curie–Weiss law

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

    Matsumoto, Nobuhiro, E-mail: nobu-matsumoto@aist.go.jp; Shimosaka, Takuya

    2015-05-07

    This work reports an attempt to quantify the purities of powders of high-purity organic compounds with stable nitroxyl radicals (namely, 2,2,6,6-tetramethylpiperidine 1-oxyl (TEMPO), 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine (TEMPOL), and 4-hydroxy-2,2,6,6-tetramethylpiperidine 1-oxyl benzoate (4-hydroxy-TEMPO benzoate)) in terms of mass fractions by using our “effective magnetic moment method,” which is based on both the Curie–Weiss law and a fundamental equation of electron paramagnetic resonance (ESR). The temperature dependence of the magnetic moment resulting from the radicals was measured with a superconducting quantum interference device magnetometer. The g value for each compound was measured with an X-band ESR spectrometer. The results of the purities were (0.998 ± 0.064) kg kg{supmore » −1} for TEMPO, (1.019 ± 0.040) kg kg{sup −1} for TEMPOL, and (1.001 ± 0.048) kg kg{sup −1} for 4-hydroxy-TEMPO benzoate. These results demonstrate that this analytical method as a future candidate of potential primary direct method can measure the purities with expanded uncertainties of approximately 5%.« less

  7. 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).

  8. 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.

  9. 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.

  10. Thin-Film Ceramic Thermocouples Fabricated and Tested

    NASA Technical Reports Server (NTRS)

    Wrbanek, John D.; Fralick, Gustave C.; Farmer, Serene C.; Sayir, Ali; Gregory, Otto J.; Blaha, Charles A.

    2004-01-01

    The Sensors and Electronics Technology Branch of the NASA Glenn Research Center is developing thin-film-based sensors for surface measurement in propulsion system research. Thin-film sensors do not require special machining of the components on which they are mounted, and they are considerably thinner than wire- or foil-based sensors. One type of sensor being advanced is the thin-film thermocouple, specifically for applications in high-temperature combustion environments. Ceramics are being demonstrated as having the potential to meet the demands of thin-film thermocouples in advanced aerospace environments. The maximum-use temperature of noble metal thin-film thermocouples, 1500 C (2700 F), may not be adequate for components used in the increasingly harsh conditions of advanced aircraft and next-generation launch vehicles. Ceramic-based thermocouples are known for their high stability and robustness at temperatures exceeding 1500 C, but are typically in the form of bulky rods or probes. As part of ASTP, Glenn's Sensors and Electronics Technology Branch is leading an in-house effort to apply ceramics as thin-film thermocouples for extremely high-temperature applications as part of ASTP. Since the purity of the ceramics is crucial for the stability of the thermocouples, Glenn's Ceramics Branch and Case Western Reserve University are developing high-purity ceramic sputtering targets for fabricating high-temperature sensors. Glenn's Microsystems Fabrication Laboratory, supported by the Akima Corporation, is using these targets to fabricate thermocouple samples for testing. The first of the materials used were chromium silicide (CrSi) and tantalum carbide (TaC). These refractory materials are expected to survive temperatures in excess of 1500 C. Preliminary results indicate that the thermoelectric voltage output of a thin-film CrSi versus TaC thermocouple is 15 times that of the standard type R (platinum-rhodium versus platinum) thermocouple, producing 20 mV with a 200 C temperature gradient. The photograph on the left shows the CrSi-TaC thermocouple in a test fixture at Glenn, and the resulting output signal is shown on the right. The temperature differential across the sample, from the center of the sample inside the oven to the sample mount outside the oven, is measured using a type R thermocouple on the sample.

  11. 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.

  12. Lithium1.3Aluminum0.3Titanium1.7Phosphate as a solid state Li-ion conductor: Issues with microcracking and stability in aqueous solutions

    NASA Astrophysics Data System (ADS)

    Jackman, Spencer D.

    Lithium aluminum titanium phosphate (LATP) with formula Li1.3Al0.3Ti1.7(PO4)3 was analyzed and tested to better understand its applicability as a solid state ion conducting ceramic material for electrochemical applications. Sintered samples were obtained from Ceramatec, Inc. in Salt Lake City and characterized in terms of density, phase-purity, fracture toughness, Young's modulus, thermal expansion behavior, mechanical strength, a.c. and d.c. ionic conductivity, and susceptibility to static and electrochemical corrosion in aqueous Li salt solutions. It was shown that LATP is prone to microcrack generation because of high thermal expansion anisotropy. A.c. impedance spectra of high-purity LATP of varying grain sizes showed that microcracking had a negative impact on the ionic conduction of Li along grain boundaries, with fine-grained (1.7±0.7 µm) LATP having twice the ionic conductivity of the same purity of coarse-grained (4.8±1.9 µm) LATP at 50°C. LATP with detectible secondary phases had lower ionic conductivity for similar grain sizes, as would be expected. The Young's modulus of fine-grained LATP was measured to be 115 GPa, and the highest biaxial strength was 191±11 MPa when tested in mineral oil, 144±13 MPa as measured in air, and 26±7 MPa after exposure to deionized water, suggesting that LATP undergoes stress-corrosion cracking. After exposure to LiOH, the strength was 76±19 MPa. This decrease in strength was observed despite there being no measureable change in a.c. impedance spectra, X-ray diffraction, or sample mass, suggesting phosphate glasses at grain boundaries. The chemical and electrochemical stability of high-purity LATP in aqueous electrochemical cells was evaluated using LiOH, LiCl, LiNO3, and LiCOOCH3 salts as the Li source. LATP was found to be most stable between pH 8-9, with the longest cell operating continuously at 25 mA cm-2 for 625 hours at 40°C in LiCOOCH3. At pH values outside of the 7-10 range, eventual membrane degradation was observed in all aqueous systems under electrochemical conditions. While LATP was surprisingly resistant to static corrosion in a hot, aqueous LiOH solution, electrochemical degradation was observed at the cathode due to subsurface pitting. Strength measurements were more instructive than impedance measurements in detecting this degradation.

  13. The development of an efficient mass balance approach for the purity assignment of organic calibration standards.

    PubMed

    Davies, Stephen R; Alamgir, Mahiuddin; Chan, Benjamin K H; Dang, Thao; Jones, Kai; Krishnaswami, Maya; Luo, Yawen; Mitchell, Peter S R; Moawad, Michael; Swan, Hilton; Tarrant, Greg J

    2015-10-01

    The purity determination of organic calibration standards using the traditional mass balance approach is described. Demonstrated examples highlight the potential for bias in each measurement and the need to implement an approach that provides a cross-check for each result, affording fit for purpose purity values in a timely and cost-effective manner. Chromatographic techniques such as gas chromatography with flame ionisation detection (GC-FID) and high-performance liquid chromatography with UV detection (HPLC-UV), combined with mass and NMR spectroscopy, provide a detailed impurity profile allowing an efficient conversion of chromatographic peak areas into relative mass fractions, generally avoiding the need to calibrate each impurity present. For samples analysed by GC-FID, a conservative measurement uncertainty budget is described, including a component to cover potential variations in the response of each unidentified impurity. An alternative approach is also detailed in which extensive purification eliminates the detector response factor issue, facilitating the certification of a super-pure calibration standard which can be used to quantify the main component in less-pure candidate materials. This latter approach is particularly useful when applying HPLC analysis with UV detection. Key to the success of this approach is the application of both qualitative and quantitative (1)H NMR spectroscopy.

  14. The Dynamic Nature of the Ligustilide Complex

    PubMed Central

    Schinkovitz, Andreas; Pro, Samuel M.; Main, Matthew; Chen, Shao-Nong; Jaki, Birgit U.; Lankin, David C.; Pauli, Guido F.

    2008-01-01

    Monomeric phthalides like Z-ligustilide (1) and Z-butylidenephthalide (2) are major constituents of medicinal plants of the Apiaceae family. While 1 has been associated with a variety of observed biological effects, it is also known for its instability and rapid chemical degradation. For the purpose of isolating pure 1 and 2, a gentle and rapid 2-step countercurrent isolation procedure was developed. From a supercritical CO2 fluid extract of Angelica sinensis roots, the phthalides were isolated with high GC-MS purities of 99.4 % for 1 and 98.9 % for 2, and consistently lower qHNMR purities of 98.1 % and 96.4 %, respectively. Taking advantage of molarity-based qHNMR methodology, a time-resolved study of the dynamic changes and residual complexity of pure 1 was conducted. GC-MS and (qH)NMR analysis of artificially degraded 1 provided evidence for the phthalide degradation pathways and optimized storing conditions. Parallel qHNMR analysis led to the recognition of variations in time- and process-dependant sample purity, and has impact on the overall assessment of time dependent changes in complex natural products systems. The study underscores the importance of independent quantitative monitoring as a prerequisite for the biological evaluation of labile natural products such as monomeric phthalides. PMID:18781813

  15. Facile Purification of Milligram to Gram Quantities of Condensed Tannins According to Mean Degree of Polymerization and Flavan-3-ol Subunit Composition.

    PubMed

    Brown, Ron H; Mueller-Harvey, Irene; Zeller, Wayne E; Reinhardt, Laurie; Stringano, Elisabetta; Gea, An; Drake, Christopher; Ropiak, Honorata M; Fryganas, Christos; Ramsay, Aina; Hardcastle, Emily E

    2017-09-13

    Unambiguous investigation of condensed tannin (CT) structure-activity relationships in biological systems requires well-characterized, high-purity CTs. Sephadex LH-20 and Toyopearl HW-50F resins were compared for separating CTs from acetone/water extracts, and column fractions analyzed for flavan-3-ol subunits, mean degree of polymerization (mDP), and purity. Toyopearl HW-50F generated fractions with higher mDP values and better separation of procyanidins (PC) and prodelphinidins (PD) but required a prepurification step, needed more time for large scale purifications, and gave poorer recoveries. Therefore, two gradient elution schemes were developed for CT purification on Sephadex LH-20 providing 146-2000 mg/fraction. Fractions were analyzed by thiolysis and NMR spectroscopy. In general, PC/PD ratios decreased and mDP increased during elution. 1 H NMR spectroscopy served as a rapid screening tool to qualitatively determine CT enrichment and carbohydrate impurities present, guiding fractionation toward repurification or 1 H- 13 C HSQC NMR spectroscopy and thiolysis. These protocols provide options for preparing highly pure CT samples.

  16. High Purity and Yield of Boron Nitride Nanotubes Using Amorphous Boron and a Nozzle-Type Reactor

    PubMed Central

    Kim, Jaewoo; Seo, Duckbong; Yoo, Jeseung; Jeong, Wanseop; Seo, Young-Soo; Kim, Jaeyong

    2014-01-01

    Enhancement of the production yield of boron nitride nanotubes (BNNTs) with high purity was achieved using an amorphous boron-based precursor and a nozzle-type reactor. Use of a mixture of amorphous boron and Fe decreases the milling time for the preparation of the precursor for BNNTs synthesis, as well as the Fe impurity contained in the B/Fe interdiffused precursor nanoparticles by using a simple purification process. We also explored a nozzle-type reactor that increased the production yield of BNNTs compared to a conventional flow-through reactor. By using a nozzle-type reactor with amorphous boron-based precursor, the weight of the BNNTs sample after annealing was increased as much as 2.5-times with much less impurities compared to the case for the flow-through reactor with the crystalline boron-based precursor. Under the same experimental conditions, the yield and quantity of BNNTs were estimated as much as ~70% and ~1.15 g/batch for the former, while they are ~54% and 0.78 g/batch for the latter. PMID:28788161

  17. High Purity and Yield of Boron Nitride Nanotubes Using Amorphous Boron and a Nozzle-Type Reactor.

    PubMed

    Kim, Jaewoo; Seo, Duckbong; Yoo, Jeseung; Jeong, Wanseop; Seo, Young-Soo; Kim, Jaeyong

    2014-08-11

    Enhancement of the production yield of boron nitride nanotubes (BNNTs) with high purity was achieved using an amorphous boron-based precursor and a nozzle-type reactor. Use of a mixture of amorphous boron and Fe decreases the milling time for the preparation of the precursor for BNNTs synthesis, as well as the Fe impurity contained in the B/Fe interdiffused precursor nanoparticles by using a simple purification process. We also explored a nozzle-type reactor that increased the production yield of BNNTs compared to a conventional flow-through reactor. By using a nozzle-type reactor with amorphous boron-based precursor, the weight of the BNNTs sample after annealing was increased as much as 2.5-times with much less impurities compared to the case for the flow-through reactor with the crystalline boron-based precursor. Under the same experimental conditions, the yield and quantity of BNNTs were estimated as much as ~70% and ~1.15 g/batch for the former, while they are ~54% and 0.78 g/batch for the latter.

  18. 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.

  19. Aqueous Two-Phase Systems at Large Scale: Challenges and Opportunities.

    PubMed

    Torres-Acosta, Mario A; Mayolo-Deloisa, Karla; González-Valdez, José; Rito-Palomares, Marco

    2018-06-07

    Aqueous two-phase systems (ATPS) have proved to be an efficient and integrative operation to enhance recovery of industrially relevant bioproducts. After ATPS discovery, a variety of works have been published regarding their scaling from 10 to 1000 L. Although ATPS have achieved high recovery and purity yields, there is still a gap between their bench-scale use and potential industrial applications. In this context, this review paper critically analyzes ATPS scale-up strategies to enhance the potential industrial adoption. In particular, large-scale operation considerations, different phase separation procedures, the available optimization techniques (univariate, response surface methodology, and genetic algorithms) to maximize recovery and purity and economic modeling to predict large-scale costs, are discussed. ATPS intensification to increase the amount of sample to process at each system, developing recycling strategies and creating highly efficient predictive models, are still areas of great significance that can be further exploited with the use of high-throughput techniques. Moreover, the development of novel ATPS can maximize their specificity increasing the possibilities for the future industry adoption of ATPS. This review work attempts to present the areas of opportunity to increase ATPS attractiveness at industrial levels. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. 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.

  1. Oxidation of TD nickel at 1050 C and 1200 C as compared with three grades of nickel of different purity

    NASA Technical Reports Server (NTRS)

    Lowell, C. E.; Grisaffe, S. J.; Deadmore, D. L.

    1972-01-01

    The isothermal oxidation of three nickels of different purity, Ni-200, Ni-270, and JM-Ni, was compared with that of TD-Ni in air at 1050 and 1200 C. The samples were oxidized as ground, as polished, or as annealed and polished. Weight change, metal loss, scale thickness, oxide morphology, and scale texture were determined. In degree of oxidation, TD-Ni was nearly the same as the higher purity materials, Ni-270 and JM-Ni; and less pure Ni-200 oxidized more than the others. However, in microstructure and scale texture the TD-Ni more closely resembled Ni-200. Grinding only charged the texture of the oxides of Ni_200 and TD-Ni.

  2. High-Purity Silicon Seeds for Silane Pyrolysis

    NASA Technical Reports Server (NTRS)

    Hsu, G. C.; Rohatgi, N. K.; Morrison, A.

    1985-01-01

    Seed particles for fluidized-bed production of silicon made by new contamination-free, economical method. In new method, large particles of semiconductor-grade silicon fired at each other by high-speed streams of gas and thereby break up into particles of suitable size for fluidized bed. No foreign materials introduced, and leaching unnecessary. Method used to feed fluidized-bed reactor for continuous production of high-purity silicon.

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

    PubMed

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

    2016-12-01

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

  4. 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.

  5. 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

  6. 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.

  7. Ultraviolet Shadowing of RNA Can Cause Significant Chemical Damage in Seconds

    PubMed Central

    Kladwang, Wipapat; Hum, Justine; Das, Rhiju

    2012-01-01

    Chemical purity of RNA samples is important for high-precision studies of RNA folding and catalytic behavior, but photodamage accrued during ultraviolet (UV) shadowing steps of sample preparation can reduce this purity. Here, we report the quantitation of UV-induced damage by using reverse transcription and single-nucleotide-resolution capillary electrophoresis. We found photolesions in a dozen natural and artificial RNAs; across multiple sequence contexts, dominantly at but not limited to pyrimidine doublets; and from multiple lamps recommended for UV shadowing. Irradiation time-courses revealed detectable damage within a few seconds of exposure for 254 nm lamps held at a distance of 5 to 10 cm from 0.5-mm thickness gels. Under these conditions, 200-nucleotide RNAs subjected to 20 seconds of UV shadowing incurred damage to 16-27% of molecules; and, due to a ‘skin effect’, the molecule-by-molecule distribution of lesions gave 4-fold higher variance than a Poisson distribution. Thicker gels, longer wavelength lamps, and shorter exposure times reduced but did not eliminate damage. These results suggest that RNA biophysical studies should report precautions taken to avoid artifactual heterogeneity from UV shadowing. PMID:22816040

  8. [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.

  9. Structural characterization and antioxidant activity evaluation of lignins from rice husk.

    PubMed

    Salanti, Anika; Zoia, Luca; Orlandi, Marco; Zanini, Fabiana; Elegir, Graziano

    2010-09-22

    In recent years, lignin and extractives from herbaceous plants and crops are receiving increasing attention for their renewability and large annual biomass stock. It is worth noting that only a few studies deal with the chemical characterization of rice husk, a side product of one of the most important crops with regard to human nutrition. Thus, in this study lignin from rice husk was isolated and characterized. Two different extraction procedures were optimized and tested: acidolysis and alkaline enzymatic (AE). The different lignins isolated were fully characterized by means of gravimetric, chromatographic (GPC), and spectroscopic (31P NMR, 2D-HSQC-NMR) analyses with the aim to compare yields, sample purity, and chemical properties, recognized as key parameters for future development. Notwithstanding the extraction procedure, the results highlighted that rice husk lignin is mainly formed by guaiacyl and p-hydroxyphenyl units. The acidolytic approach showed an appreciable lignin recovery and high purity, whereas the AE lignin sample was found to be rich in residual polysaccharides and oxidized functionalities. Moreover, different rice husk extracts, along with acidolysis lignin and AE lignin specimens, were assayed for their antioxidant activity by means of a DPPH radical scavenging test.

  10. A thermal desorption spectroscopy study of hydrogen trapping in polycrystalline α-uranium

    DOE PAGES

    Lillard, R. S.; Forsyth, R. T.

    2015-03-14

    The kinetics of hydrogen desorption from polycrystalline α-uranium (α-U) was examined using thermal desorption spectroscopy (TDS). The goal was to identify the major trap sites for hydrogen and their associated trap energies. In polycrystalline α-U six TDS adsorption peaks were observed at temperatures of 521 K, 556 K, 607 K, 681 K, 793 K and 905 K. In addition, the desorption was determined to be second order based on peak shape. The position of the first three peaks was consistent with desorption from UH3. To identify the trap site corresponding to the high temperature peaks the data were compared tomore » a plastically deformed sample and a high purity single crystal sample. The plastically deformed sample allowed the identification of trapping at dislocations while the single crystal sample allow for the identification of high angle boundaries and impurities. Thus, with respect to the desorption energy associated with each peak, values between 12.9 and 26.5 kJ/mole were measured.« less

  11. Enhancement of microfluidic particle separation using cross-flow filters with hydrodynamic focusing

    PubMed Central

    Chiu, Yun-Yen; Huang, Chen-Kang

    2016-01-01

    A microfluidic chip is proposed to separate microparticles using cross-flow filtration enhanced with hydrodynamic focusing. By exploiting a buffer flow from the side, the microparticles in the sample flow are pushed on one side of the microchannels, lining up to pass through the filters. Meanwhile a larger pressure gradient in the filters is obtained to enhance separation efficiency. Compared with the traditional cross-flow filtration, our proposed mechanism has the buffer flow to create a moving virtual boundary for the sample flow to actively push all the particles to reach the filters for separation. It further allows higher flow rates. The device only requires soft lithograph fabrication to create microchannels and a novel pressurized bonding technique to make high-aspect-ratio filtration structures. A mixture of polystyrene microparticles with 2.7 μm and 10.6 μm diameters are successfully separated. 96.2 ± 2.8% of the large particle are recovered with a purity of 97.9 ± 0.5%, while 97.5 ± 0.4% of the small particle are depleted with a purity of 99.2 ± 0.4% at a sample throughput of 10 μl/min. The experiment is also conducted to show the feasibility of this mechanism to separate biological cells with the sample solutions of spiked PC3 cells in whole blood. By virtue of its high separation efficiency, our device offers a label-free separation technique and potential integration with other components, thereby serving as a promising tool for continuous cell filtration and analysis applications. PMID:26858812

  12. An XPS study on the impact of relative humidity on the aging of UO 2 powders

    DOE PAGES

    Donald, Scott B.; Dai, Zurong R.; Davisson, M. Lee; ...

    2017-02-10

    High resolution x-ray photoemission spectroscopy (XPS) was used to characterize the chemical speciation of high purity uranium dioxide (UO 2) powder samples following aging for periods of up to one year under controlled conditions with relative humidity ranging from 34% to 98%. A systematic shift to higher uranium oxidation states, and thus an increase in the mean uranium valence, was found to directly correlate with the dose of water received (i.e. the product of exposure time and relative humidity). Exposure duration was found to have a greater impact on sample aging than relative humidity. Lastly, the sample aged at 98%more » relative humidity was found to have unique structural differences for exposure time beyond 180 days when observed by scanning electron microscopy (SEM).« less

  13. An XPS study on the impact of relative humidity on the aging of UO 2 powders

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

    Donald, Scott B.; Dai, Zurong R.; Davisson, M. Lee

    High resolution x-ray photoemission spectroscopy (XPS) was used to characterize the chemical speciation of high purity uranium dioxide (UO 2) powder samples following aging for periods of up to one year under controlled conditions with relative humidity ranging from 34% to 98%. A systematic shift to higher uranium oxidation states, and thus an increase in the mean uranium valence, was found to directly correlate with the dose of water received (i.e. the product of exposure time and relative humidity). Exposure duration was found to have a greater impact on sample aging than relative humidity. Lastly, the sample aged at 98%more » relative humidity was found to have unique structural differences for exposure time beyond 180 days when observed by scanning electron microscopy (SEM).« less

  14. [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.

  15. Processing of laser formed SiC powder

    NASA Technical Reports Server (NTRS)

    Haggerty, J. S.; Bowen, H. K.

    1985-01-01

    Superior SiC characteristics can be achieved through the use of ideal constituent powders and careful post-synthesis processing steps. High purity SiC powders of approx. 1000 A uniform diameter, nonagglomerated and spherical were produced. This required major revision of the particle formation and growth model from one based on classical nucleation and growth to one based on collision and coalescence of Si particles followed by their carburization. Dispersions based on pure organic solvents as well as steric stabilization were investigated. Although stable dispersions were formed by both, subsequent part fabrication emphasized the pure solvents since fewer problems with drying and residuals of the high purity particles were anticipated. Test parts were made by the colloidal pressing technique; both liquid filtration and consolidation (rearrangement) stages were modeled. Green densities corresponding to a random close packed structure (approx. 63%) were achieved; this highly perfect structure has a high, uniform coordination number (greater than 11) approaching the quality of an ordered structure without introducing domain boundary effects. After drying, parts were densified at temperatures ranging from 1800 to 2100 C. Optimum densification temperatures will probably be in the 1900 to 2000 C range based on these preliminary results which showed that 2050 C samples had experienced substantial grain growth. Although overfired, the 2050 C samples exhibited excellent mechanical properties. Biaxial tensile strengths up to 714 MPa and Vickers hardness values of 2430 kg/sq mm 2 were both more typical of hot pressed than sintered SiC. Both result from the absence of large defects and the confinement of residual porosity (less than 2.5%) to small diameter, uniformly distributed pores.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. Comparison of DNA extraction methods used to detect bacterial and yeast DNA from spiked whole blood by real-time PCR.

    PubMed

    Dalla-Costa, Libera M; Morello, Luis G; Conte, Danieli; Pereira, Luciane A; Palmeiro, Jussara K; Ambrosio, Altair; Cardozo, Dayane; Krieger, Marco A; Raboni, Sonia M

    2017-09-01

    Sepsis is the leading cause of death in intensive care units (ICUs) worldwide and its diagnosis remains a challenge. Blood culturing is the gold standard technique for blood stream infection (BSI) identification. Molecular tests to detect pathogens in whole blood enable early use of antimicrobials and affect clinical outcomes. Here, using real-time PCR, we evaluated DNA extraction using seven manual and three automated commercially available systems with whole blood samples artificially contaminated with Escherichia coli, Staphylococcus aureus, and Candida albicans, microorganisms commonly associated with BSI. Overall, the commercial kits evaluated presented several technical limitations including long turnaround time and low DNA yield and purity. The performance of the kits was comparable for detection of high microorganism loads (10 6 CFU/mL). However, the detection of lower concentrations was variable, despite the addition of pre-processing treatment to kits without such steps. Of the evaluated kits, the UMD-Universal CE IVD kit generated a higher quantity of DNA with greater nucleic acid purity and afforded the detection of the lowest microbial load in the samples. The inclusion of pre-processing steps with the kit seems to be critical for the detection of microorganism DNA directly from whole blood. In conclusion, future application of molecular techniques will require overcoming major challenges such as the detection of low levels of microorganism nucleic acids amidst the large quantity of human DNA present in samples or differences in the cellular structures of etiological agents that can also prevent high-quality DNA yields. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. 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

  4. 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

  5. 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

  6. Monitoring xenon purity in the LUX detector with a mass spectrometry system

    NASA Astrophysics Data System (ADS)

    Balajthy, Jon; LUX Experiment Collaboration

    2015-04-01

    The LUX dark matter search experiment is a 350 kg two-phase liquid/gas xenon time projection chamber located at the 4850 ft level of the Sanford Underground Research Facility in Lead, SD. To monitor for radioactive impurities such as krypton and impurities which limit charge yield such as oxygen, LUX uses a xenon sampling system consisting of a mass spectrometer and a liquid nitrogen cold trap. The cold trap separates the gaseous impurities from a small sample of xenon and allows them to pass to the mass spectrometer for analysis. We report here on results from the LUX xenon sampling program. We also report on methods to enhance the sensitivity of the cold trap technique in preparation for the next-generation LUX-ZEPLIN experiment which will have even more stringent purity requirements.

  7. 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...

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. Luminescent Eu3+ doped Al6Ge2O13 crystalline compounds obtained by the sol gel process for photonics

    NASA Astrophysics Data System (ADS)

    Maia, Lauro J. Q.; Faria Filho, Fausto M.; Gonçalves, Rogéria R.; Ribeiro, Sidney J. L.

    2018-01-01

    We synthesized pure and Eu3+ doped Al6Ge2O13 samples by an easy and low-cost sol-gel route using the GeO2, Al(NO3)3·9H2O and Eu(NO3)3·6H2O as precursors, tetramethylammonium hydroxide and ethanol as solvents. The Al6Ge2O13 crystalline phase possesses orthorhombic structure and is a potential host for rare earth ions, especially due to high aluminum concentration. Homogeneous and transparent sols and gels were obtained. The samples containing 1 mol% of Eu3+ were heat-treated at 1000 °C to eliminate organic compounds, providing high optical quality and structural purity. All materials were characterized by thermogravimetric and differential thermal analysis, X-ray diffraction, Fourier transform infrared spectroscopy, high resolution transmission electron microscopy, selected area electron diffraction, diffuse reflectance spectra in the ultraviolet-visible-near infrared regions and photoluminescence measurements. High purity of Eu3+ doped Al6Ge2O13 orthorhombic phase and well crystallized grain dimensions of around 100 nm was obtained with high red photoluminescence emission. The decay lifetime of 5D0 level from Eu3+ (the emission at 612 nm) was determined, being between 0.97 and 2.12 ms, and an average quantum efficiency of 54% was determined (considering the average experimental lifetime of 1.77 ms). Moreover, it was calculated and analyzed some parameters of Judd-Ofelt theory applied to Eu3+ emissions from Al6Ge2O13 host. The results show that Eu3+ doped Al6Ge2O13 crystalline compounds have large potential to be used in displays and LED devices.

  15. 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.

  16. Agarose-gel electrophoresis for the quality assurance and purity of heparin formulations.

    PubMed

    Volpi, Nicola; Buzzega, Dania

    2012-01-01

    The adulteration of raw heparin (Hep) with a synthetic oversulfated chondroitin sulfate (OSCS) not found in nature produced in 2007-2008 a global crisis giving rise to the development of additional, new and specific methods for its quality assurance and purity. In this study, a simple and sensitive agarose-gel electrophoresis method has been developed for the visualization of OSCS in Hep samples along with other natural glycosaminoglycans possibly present as "process-related impurities", in particular dermatan sulfate (DS) and chondroitin sulfate (CS). Agarose-gel electrophoresis under non-conventional conditions is able to separate OSCS from Hep with its two components, the slow-moving and fast-moving species, DS and CS by performing separation for 15 h (overnight) and under high voltage (100 mA, ∼200 V). Densitometric scanning enabled us to calculate a limit of detection of ∼0.5 μg OSCS with a linear behaviour from 0.1 to 5 μg, comparable to CS/DS. Contaminated samples from Hep manufacturers were analyzed and quantitative data were found comparable to previous studies. Due to its capacity to process many samples in a single run and to the equipment commonly available in laboratories, this analytical method would be suitable for the identification and quantification of contamination by other polysaccharides, in particular OSCS and DS, within Hep preparations and formulations. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. 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.

  18. 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.

  19. Separation of Be and Al for AMS using single-step column chromatography

    NASA Astrophysics Data System (ADS)

    Binnie, Steven A.; Dunai, Tibor J.; Voronina, Elena; Goral, Tomasz; Heinze, Stefan; Dewald, Alfred

    2015-10-01

    With the aim of simplifying AMS target preparation procedures for TCN measurements we tested a new extraction chromatography approach which couples an anion exchange resin (WBEC) to a chelating resin (Beryllium resin) to separate Be and Al from dissolved quartz samples. Results show that WBEC-Beryllium resin stacks can be used to provide high purity Be and Al separations using a combination of hydrochloric/oxalic and nitric acid elutions. 10Be and 26Al concentrations from quartz samples prepared using more standard procedures are compared with results from replicate samples prepared using the coupled WBEC-Beryllium resin approach and show good agreement. The new column procedure is performed in a single step, reducing sample preparation times relative to more traditional methods of TCN target production.

  20. Towards well-defined gold nanomaterials via diafiltration and aptamer mediated synthesis

    NASA Astrophysics Data System (ADS)

    Sweeney, Scott Francis

    Gold nanoparticles have garnered recent attention due to their intriguing size- and shape-dependent properties. Routine access to well-defined gold nanoparticle samples in terms of core diameter, shape, peripheral functionality and purity is required in order to carry out fundamental studies of their properties and to utilize these properties in future applications. For this reason, the development of methods for preparing well-defined gold nanoparticle samples remains an area of active research in materials science. In this dissertation, two methods, diafiltration and aptamer mediated synthesis, are explored as possible routes towards well-defined gold nanoparticle samples. It is shown that diafiltration has considerable potential for the efficient and convenient purification and size separation of water-soluble nanoparticles. The suitability of diafiltration for (i) the purification of water-soluble gold nanoparticles, (ii) the separation of a bimodal distribution of nanoparticles into fractions, (iii) the fractionation of a polydisperse sample and (iv) the isolation of [rimers from monomers and aggregates is studied. NMR, thermogravimetric analysis (TGA), and X-ray photoelectron spectroscopy (XPS) measurements demonstrate that diafiltration produces highly pure nanoparticles. UV-visible spectroscopic and transmission electron microscopic analyses show that diafiltration offers the ability to separate nanoparticles of disparate core size, including linked nanoparticles. These results demonstrate the applicability of diafiltration for the rapid and green preparation of high-purity gold nanoparticle samples and the size separation of heterogeneous nanoparticle samples. In the second half of the dissertation, the identification of materials specific aptamers and their use to synthesize shaped gold nanoparticles is explored. The use of in vitro selection for identifying materials specific peptide and oligonucleotide aptamers is reviewed, outlining the specific requirements of in vitro selection for materials and the ways in which the field can be advanced. A promising new technique, in vitro selection on surfaces (ISOS), is developed and the discovery using ISOS of RNA aptamers that bind to evaporated gold is discussed. Analysis of the isolated gold binding RNA aptamers indicates that they are highly structured with single-stranded polyadenosine binding motifs. These aptamers, and similarly isolated peptide aptamers, are briefly explored for their ability to synthesize gold nanoparticles. This dissertation contains both previously published and unpublished co-authored material.

  1. 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.

  2. Pinning-to-barrier crossover in YBa2Cu3O7-δ single crystals

    NASA Astrophysics Data System (ADS)

    Indenbom, M. V.; van der Beek, C. J.; Berseth, V.; Konczykowski, M.; Holtzberg, F.; Benoit, W.

    1996-03-01

    The behaviour of magnetic flux in high purity untwinned YBa2Cu3O7-δ (YBCO) single crystals is visualised by means of the magneto-optical technique. It is observed that after zero field-cooling at high temperatures near T c , flux penetrates directly to the sample center over a flux free edge area, in contrast to the usual Bean-like flux penetration from the edges. This fact clearly shows that volume pinning becomes negligible compared with the edge barrier. The role of the recently rediscovered geometrical barrier in the crystal magnetisation is discussed.

  3. Characterization of Extracellular Vesicles by Size-Exclusion High-Performance Liquid Chromatography (HPLC).

    PubMed

    Huang, Tao; He, Jiang

    2017-01-01

    Extracellular vesicles (EVs) have recently attracted substantial attention due to the potential diagnostic and therapeutic relevance. Although a variety of techniques have been used to isolate and analyze EVs, it is still far away from satisfaction. Size-exclusion chromatography (SEC), which separates subjects by size, has been widely applied in protein purification and analysis. The purpose of this chapter is to show the applications of size-exclusion high-performance liquid chromatography (HPLC) as methods for EV characterization of impurities or contaminants of small size, and thus for quality assay for the purity of the samples of EVs.

  4. Human DNA extraction from whole saliva that was fresh or stored for 3, 6 or 12 months using five different protocols

    PubMed Central

    GARBIERI, Thais Francini; BROZOSKI, Daniel Thomas; DIONÍSIO, Thiago José; SANTOS, Carlos Ferreira; NEVES, Lucimara Teixeira das

    2017-01-01

    Abstract Saliva when compared to blood collection has the following advantages: it requires no specialized personnel for collection, allows for remote collection by the patient, is painless, well accepted by participants, has decreased risks of disease transmission, does not clot, can be frozen before DNA extraction and possibly has a longer storage time. Objective and Material and Methods This study aimed to compare the quantity and quality of human DNA extracted from saliva that was fresh or frozen for three, six and twelve months using five different DNA extraction protocols: protocol 1 – Oragene™ commercial kit, protocol 2 – QIAamp DNA mini kit, protocol 3 – DNA extraction using ammonium acetate, protocol 4 – Instagene™ Matrix and protocol 5 – Instagene™ Matrix diluted 1:1 using proteinase K and 1% SDS. Briefly, DNA was analyzed using spectrophotometry, electrophoresis and PCR. Results Results indicated that time spent in storage typically decreased the DNA quantity with the exception of protocol 1. The purity of DNA was generally not affected by storage times for the commercial based protocols, while the purity of the DNA samples extracted by the noncommercial protocols typically decreased when the saliva was stored longer. Only protocol 1 consistently extracted unfragmented DNA samples. In general, DNA samples extracted through protocols 1, 2, 3 and 4, regardless of storage time, were amplified by human specific primers whereas protocol 5 produced almost no samples that were able to be amplified by human specific primers. Depending on the protocol used, it was possible to extract DNA in high quantities and of good quality using whole saliva, and furthermore, for the purposes of DNA extraction, saliva can be reliably stored for relatively long time periods. Conclusions In summary, a complicated picture emerges when taking into account the extracted DNA’s quantity, purity and quality; depending on a given researchers needs, one protocol’s particular strengths and costs might be the deciding factor for its employment. PMID:28403355

  5. 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.

  6. 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

  7. 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.

  8. 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.

  9. 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...

  10. 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

  11. First result of deuterium retention in neutron-irradiated tungsten exposed to high flux plasma in TPE

    NASA Astrophysics Data System (ADS)

    Shimada, Masashi; Hatano, Y.; Calderoni, P.; Oda, T.; Oya, Y.; Sokolov, M.; Zhang, K.; Cao, G.; Kolasinski, R.; Sharpe, J. P.

    2011-08-01

    With the Japan-US joint research project Tritium, Irradiations, and Thermofluids for America and Nippon (TITAN), an initial set of tungsten samples (99.99% purity, A.L.M.T. Co.) were irradiated by high flux neutrons at 323 K to 0.025 dpa in High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL). Subsequently, one of the neutron-irradiated tungsten samples was exposed to a high-flux deuterium plasma (ion flux: 5 × 1021 m-2 s-1, ion fluence: 4 × 1025 m-2) in the Tritium Plasma Experiment (TPE) at Idaho National Laboratory (INL). The deuterium retention in the neutron-irradiated tungsten was 40% higher in comparison to the unirradiated tungsten. The observed broad desorption spectrum from neutron-irradiated tungsten and associated TMAP modeling of the deuterium release suggest that trapping occurs in the bulk material at more than three different energy sites.

  12. Method for growing low defect, high purity crystalline layers utilizing lateral overgrowth of a patterned mask

    NASA Technical Reports Server (NTRS)

    Morrison, Andrew D. (Inventor); Daud, Taher (Inventor)

    1986-01-01

    A method for growing a high purity, low defect layer of semiconductor is described. This method involves depositing a patterned mask of a material impervious to impurities of the semiconductor on a surface of a blank. When a layer of semiconductor is grown on the mask, the semiconductor will first grow from the surface portions exposed by the openings in the mask and will bridge the connecting portions of the mask to form a continuous layer having improved purity, since only the portions overlying the openings are exposed to defects and impurities. The process can be iterated and the mask translated to further improve the quality of grown layers.

  13. Electrical resistivity of La

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

    Legvold, S.; Burgardt, P.; Beaudry, B.J.

    1977-09-15

    The electrical resistivity of high-purity double hexagonal-close-packed (dhcp) ..cap alpha..-La from 5 to 300 K is reported. Measurements were made on small-grained samples prepared by heat treatment of cold-worked lanthanum. Measurements were also made on samples cut in different directions from an ingot slowly cooled from the molten state. The room-temperature results were all within 2% of the mean value. Chemically pure ..beta..-La (fcc) cannot be retained at room temperature, hence, measurements were made on an fcc sample of La containing 0.2-at. % Gd and approx. 0.8-at. % total interstitial nonmetallic impurities. The cubic form has almost the same typemore » of temperature dependence as the dhcp form, but has a 10% lower magnitude.« less

  14. Inorganic trace analysis by mass spectrometry

    NASA Astrophysics Data System (ADS)

    Becker, Johanna Sabine; Dietze, Hans-Joachim

    1998-10-01

    Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g -1 concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of high-purity materials and environmental samples) is used in order to improve the detection limits of trace elements. Furthermore, the determination of chemical elements in the trace and ultratrace concentration range is often difficult and can be disturbed through mass interferences of analyte ions by molecular ions at the same nominal mass. By applying double-focusing sector field mass spectrometry at the required mass resolution—by the mass spectrometric separation of molecular ions from the analyte ions—it is often possible to overcome these interference problems. Commercial instrumental equipment, the capability (detection limits, accuracy, precision) and the analytical application fields of mass spectrometric methods for the determination of trace and ultratrace elements and for surface analysis are discussed.

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

    PubMed Central

    2013-01-01

    Background 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. Results 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. Conclusions 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. PMID:23800080

  16. 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.

  17. 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.

  18. Silicon halide-alkali metal flames as a source of solar grade silicon

    NASA Technical Reports Server (NTRS)

    Olsen, D. B.; Miller, W. J.

    1979-01-01

    The feasibility of using alkali metal-silicon halide diffusion flames to produce solar-grade silicon in large quantities and at low cost is demonstrated. Prior work shows that these flames are stable and that relatively high purity silicon can be produced using Na + SiCl4 flames. Silicon of similar purity is obtained from Na + SiF4 flames although yields are lower and product separation and collection are less thermochemically favored. Continuous separation of silicon from the byproduct alkali salt was demonstrated in a heated graphite reactor. The process was scaled up to reduce heat losses and to produce larger samples of silicon. Reagent delivery systems, scaled by a factor of 25, were built and operated at a production rate of 0.5 kg Si/h. Very rapid reactor heating rates are observed with wall temperatures reaching greater than 2000 K. Heat release parameters were measured using a cooled stainless steel reactor tube. A new reactor was designed.

  19. 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.

  20. Nb-Based Nb-Al-Fe Alloys: Solidification Behavior and High-Temperature Phase Equilibria

    NASA Astrophysics Data System (ADS)

    Stein, Frank; Philips, Noah

    2018-03-01

    High-melting Nb-based alloys hold significant promise for the development of novel high-temperature materials for structural applications. In order to understand the effect of alloying elements Al and Fe, the Nb-rich part of the ternary Nb-Al-Fe system was investigated. A series of Nb-rich ternary alloys were synthesized from high-purity Nb, Al, and Fe metals by arc melting. Solidification paths were identified and the liquidus surface of the Nb corner of the ternary system was established by analysis of the as-melted microstructures and thermal analysis. Complementary analysis of heat-treated samples yielded isothermal sections at 1723 K and 1873 K (1450 °C and 1600 °C).

  1. The intensive DT neutron generator of TU Dresden

    NASA Astrophysics Data System (ADS)

    Klix, Axel; DÖring, Toralf; Domula, Alexander; Zuber, Kai

    2018-01-01

    TU Dresden operates an accelerator-based intensive DT neutron generator. Experimental activities comprise investigation into material activation and decay, neutron and photon transport in matter and R&D work on radiation detectors for harsh environments. The intense DT neutron generator is capable to produce a maximum of 1012 n/s. The neutron source is a solid-type water-cooled tritium target based on a titanium matrix on a copper carrier. The neutron yield at a typical deuteron beam current of 1 mA is of the order of 1011 n/s in 4Π. A pneumatic sample transport system is available for short-time irradiations and connected to wo high-purity germanium detector spectrometers for the measurement of induced activities. The overall design of the experimental hall with the neutron generator allows a flexible setup of experiments including the possibility of investigating larger structures and cooled samples or samples at high temperatures.

  2. Scintillation gamma spectrometer for analysis of hydraulic fracturing waste products.

    PubMed

    Ying, Leong; O'Connor, Frank; Stolz, John F

    2015-01-01

    Flowback and produced wastewaters from unconventional hydraulic fracturing during oil and gas explorations typically brings to the surface Naturally Occurring Radioactive Materials (NORM), predominantly radioisotopes from the U238 and Th232 decay chains. Traditionally, radiological sampling are performed by sending collected small samples for laboratory tests either by radiochemical analysis or measurements by a high-resolution High-Purity Germanium (HPGe) gamma spectrometer. One of the main isotopes of concern is Ra226 which requires an extended 21-days quantification period to allow for full secular equilibrium to be established for the alpha counting of its progeny daughter Rn222. Field trials of a sodium iodide (NaI) scintillation detector offers a more economic solution for rapid screenings of radiological samples. To achieve the quantification accuracy, this gamma spectrometer must be efficiency calibrated with known standard sources prior to field deployments to analyze the radioactivity concentrations in hydraulic fracturing waste products.

  3. High mobility high efficiency organic films based on pure organic materials

    DOEpatents

    Salzman, Rhonda F [Ann Arbor, MI; Forrest, Stephen R [Ann Arbor, MI

    2009-01-27

    A method of purifying small molecule organic material, performed as a series of operations beginning with a first sample of the organic small molecule material. The first step is to purify the organic small molecule material by thermal gradient sublimation. The second step is to test the purity of at least one sample from the purified organic small molecule material by spectroscopy. The third step is to repeat the first through third steps on the purified small molecule material if the spectroscopic testing reveals any peaks exceeding a threshold percentage of a magnitude of a characteristic peak of a target organic small molecule. The steps are performed at least twice. The threshold percentage is at most 10%. Preferably the threshold percentage is 5% and more preferably 2%. The threshold percentage may be selected based on the spectra of past samples that achieved target performance characteristics in finished devices.

  4. Semi-supervised learning for photometric supernova classification

    NASA Astrophysics Data System (ADS)

    Richards, Joseph W.; Homrighausen, Darren; Freeman, Peter E.; Schafer, Chad M.; Poznanski, Dovi

    2012-01-01

    We present a semi-supervised method for photometric supernova typing. Our approach is to first use the non-linear dimension reduction technique diffusion map to detect structure in a data base of supernova light curves and subsequently employ random forest classification on a spectroscopically confirmed training set to learn a model that can predict the type of each newly observed supernova. We demonstrate that this is an effective method for supernova typing. As supernova numbers increase, our semi-supervised method efficiently utilizes this information to improve classification, a property not enjoyed by template-based methods. Applied to supernova data simulated by Kessler et al. to mimic those of the Dark Energy Survey, our methods achieve (cross-validated) 95 per cent Type Ia purity and 87 per cent Type Ia efficiency on the spectroscopic sample, but only 50 per cent Type Ia purity and 50 per cent efficiency on the photometric sample due to their spectroscopic follow-up strategy. To improve the performance on the photometric sample, we search for better spectroscopic follow-up procedures by studying the sensitivity of our machine-learned supernova classification on the specific strategy used to obtain training sets. With a fixed amount of spectroscopic follow-up time, we find that, despite collecting data on a smaller number of supernovae, deeper magnitude-limited spectroscopic surveys are better for producing training sets. For supernova Ia (II-P) typing, we obtain a 44 per cent (1 per cent) increase in purity to 72 per cent (87 per cent) and 30 per cent (162 per cent) increase in efficiency to 65 per cent (84 per cent) of the sample using a 25th (24.5th) magnitude-limited survey instead of the shallower spectroscopic sample used in the original simulations. When redshift information is available, we incorporate it into our analysis using a novel method of altering the diffusion map representation of the supernovae. Incorporating host redshifts leads to a 5 per cent improvement in Type Ia purity and 13 per cent improvement in Type Ia efficiency. A web service for the supernova classification method used in this paper can be found at .

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. [Procedure of seed quality testing and seed grading standard of Prunus humilis].

    PubMed

    Wen, Hao; Ren, Guang-Xi; Gao, Ya; Luo, Jun; Liu, Chun-Sheng; Li, Wei-Dong

    2014-11-01

    So far there exists no corresponding quality test procedures and grading standards for the seed of Prunus humilis, which is one of the important source of base of semen pruni. Therefor we set up test procedures that are adapt to characteristics of the P. humilis seed through the study of the test of sampling, seed purity, thousand-grain weight, seed moisture, seed viability and germination percentage. 50 cases of seed specimens of P. humilis tested. The related data were analyzed by cluster analysis. Through this research, the seed quality test procedure was developed, and the seed quality grading standard was formulated. The seed quality of each grade should meet the following requirements: for first grade seeds, germination percentage ≥ 68%, thousand-grain weight 383 g, purity ≥ 93%, seed moisture ≤ 5%; for second grade seeds, germination percentage ≥ 26%, thousand-grain weight ≥ 266 g, purity ≥ 73%, seed moisture ≤9%; for third grade seeds, germination percentage ≥ 10%, purity ≥ 50%, thousand-grain weight ≥ 08 g, seed moisture ≤ 13%.

  11. 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.

  12. 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.

  13. 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…

  14. Controlling the Morphology and Oxidation Resistance of Boron Carbide Synthesized Via Carbothermic Reduction Reaction

    NASA Astrophysics Data System (ADS)

    Ahmed, Yasser M. Z.; El-Sheikh, Said M.; Ewais, Emad M. M.; Abd-Allah, Asmaa A.; Sayed, Said A.

    2017-03-01

    Boron carbide powder was synthesized from boric acid and lactose mixtures via easy procedure. Boric acid and lactose solution mixtures were roasted in stainless steel pot at 280 °C for 24 h. Boron carbide was obtained by heating the roasted samples under flowing of industrial argon gas at 1500 °C for 3 h. The amount of borate ester compound in the roasted samples was highly influenced by the boron/carbon ratio in the starting mixtures and plays a versatile role in the produced boron carbide. The high-purity boron carbide powder was produced with a sample composed of lowest boron/carbon ratio of 1:1 without calcination step. Particle morphology was changed from nano-needles like structure of 8-10 nm size with highest carbon ratio mixture to spherical shape of >150 nm size with lowest one. The oxidation resistance performance of boron carbide is highly dependent on the morphology and grain size of the synthesized powder.

  15. 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

  16. 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.

  17. 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.

  18. Self- and Air-Broadened Line Shapes in the 2v3 P and R Branches of 12CH4

    NASA Technical Reports Server (NTRS)

    Devi, V. Malathy; Benner, D. Chris; Sung, Keeyoon; Crawford, Timothy J.; Yu, Shanshan; Brown, Linda R.; Smith, Mary Ann H.; Mantz, Arlan W.; Boudon, Vincent; Ismail, Syed

    2015-01-01

    In this paper we report line shape parameters of 12CH4 for several hundred 2V(sub 3) transitions in the spectral regions 5891-5996 cm( exp -1) (P branch) and 6015-6115 cm(exp -1) (R branch). Air- and self-broadening coefficients were measured as a function of temperature; line mixing via off-diagonal relaxation matrix element coefficients was also obtained for 47 transition pairs. In total, nearly 1517 positions and intensities were retrieved, but many transitions were too weak for the line shape study. For this analysis, we used 25 high-resolution (0.0056 and 0.0067 cm(ex[ -1) and high signal-to-noise (S/N) spectra of high-purity 12CH4 and the same high-purity 12CH4 broadened by dry air recorded at different sample temperatures between 130 K and 295 K with the Bruker IFS 125HR Fourier transform spectrometer at JPL. Three different absorption cells were used (1) a White cell set to a path length of 13.09 m for room temperature data, (2) a single-pass 0.2038 m long coolable cell (for self-broadening) and (3) a multipass cell with 20.941 m total path coolable Herriott cell (for air-broadening). In total there were 13 spectra with pure 12CH4 (0.27-599 Torr) and 12 air-broadened spectra with total sample pressures of 80-805 Torr and volume mixing ratios (VMR) of methane between 0.18 and 1.0. An interactive multispectrum nonlinear least-squares technique was employed to fit the individual P10-P1 and R0-R10 manifolds in all the spectra simultaneously. Results obtained from the present analysis are compared to other recent measurements.

  19. Production of Ultrafine, High-purity Ceramic Powders Using the US Bureau of Mines Developed Turbomill

    NASA Technical Reports Server (NTRS)

    Hoyer, Jesse L.

    1993-01-01

    Turbomilling, an innovative grinding technology developed by the U.S. Bureau of Mines in the early 1960's for delaminating filler-grade kaolinitic clays, has been expanded into the areas of particle size reduction, material mixing, and process reaction kinetics. The turbomill, originally called an attrition grinder, has been used for particle size reduction of many minerals, including natural and synthetic mica, pyrophyllite, talc, and marble. In recent years, an all-polymer version of the turbomill has been used to produce ultrafine, high-purity, advanced ceramic powders such as SiC, Si3N4, TiB2, and ZrO2. In addition to particle size reduction, the turbomill has been used to produce intimate mixtures of high surface area powders and whiskers. Raw materials, TiN, AlN, and Al2O3, used to produce a titanium nitride/aluminum oxynitride (TiN/AlON) composite, were mixed in the turbomill, resulting in strength increases over samples prepared by dry ball milling. Using the turbomill as a leach vessel, it was found that 90.4 pct of the copper was extracted from the chalcopyrite during a 4-hour leach test in ferric sulfate versus conventional processing which involves either roasting of the ore for Cu recovery or leaching of the ore for several days.

  20. 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.

  1. The characteristics of void distribution in spalled high purity copper cylinder under sweeping detonation

    NASA Astrophysics Data System (ADS)

    Yang, Yang; Jiang, Zhi; Chen, Jixinog; Guo, Zhaoliang; Tang, Tiegang; Hu, Haibo

    2018-03-01

    The effects of different peak compression stresses (2-5 GPa) on the spallation behaviour of high purity copper cylinder during sweeping detonation were examined by Electron Backscatter Diffraction Microscopy, Doppler Pins System and Optical Microscopy techniques. The velocity history of inner surface and the characteristics of void distributions in spalled copper cylinder were investigated. The results indicated that the spall strength of copper in these experiments was less than that revealed in previous reports concerning plate impact loading. The geometry of cylindrical copper and the obliquity of incident shock during sweeping detonation may be the main reasons. Different loading stresses seemed to be responsible for the characteristics of the resultant damage fields, and the maximum damage degree increased with increasing shock stress. Spall planes in different cross-sections of sample loaded with the same shock stress of 3.29 GPa were found, and the distance from the initiation end has little effect on the maximum damage degree (the maximum damage range from 12 to 14%), which means that the spallation behaviour was stable along the direction parallel to the detonation propagation direction under the same shock stress.

  2. Preparative separation of sulfur-containing diketopiperazines from marine fungus Cladosporium sp. using high-speed counter-current chromatography in stepwise elution mode.

    PubMed

    Gu, Binbin; Zhang, Yanying; Ding, Lijian; He, Shan; Wu, Bin; Dong, Junde; Zhu, Peng; Chen, Juanjuan; Zhang, Jinrong; Yan, Xiaojun

    2015-01-09

    High-speed counter-current chromatography (HSCCC) was successively applied to the separation of three sulfur-containing diketopiperazines (DKPs) (including two new compounds cladosporin A (1) and cladosporin B (3), and a known compound haematocin (2)) from a marine fungus Cladosporium sp. The two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water at (1:1:1:1, v/v) and (2:1:2:1, v/v), in stepwise elution mode, was used for HSCCC. The preparative HSCCC separation was performed on 300 mg of crude sample yielding 26.7 mg of compound 3 at a purity of over 95%, 53.6 mg of a mixture of compounds 1 and 2, which was further separated by preparative-HPLC yielding 14.3 mg of compound 1 and 25.4 mg of compound 2 each at a purity of over 95%. Their structures were established by spectroscopic methods. The sulfur-containing DKPs suppressed the proliferation of hepatocellular carcinoma cell line HepG2. The present work represents the first application of HSCCC in the efficient preparation of marine fungal natural products.

  3. Preparative Separation of Sulfur-Containing Diketopiperazines from Marine Fungus Cladosporium sp. Using High-Speed Counter-Current Chromatography in Stepwise Elution Mode

    PubMed Central

    Gu, Binbin; Zhang, Yanying; Ding, Lijian; He, Shan; Wu, Bin; Dong, Junde; Zhu, Peng; Chen, Juanjuan; Zhang, Jinrong; Yan, Xiaojun

    2015-01-01

    High-speed counter-current chromatography (HSCCC) was successively applied to the separation of three sulfur-containing diketopiperazines (DKPs) (including two new compounds cladosporin A (1) and cladosporin B (3), and a known compound haematocin (2)) from a marine fungus Cladosporium sp. The two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water at (1:1:1:1, v/v) and (2:1:2:1, v/v), in stepwise elution mode, was used for HSCCC. The preparative HSCCC separation was performed on 300 mg of crude sample yielding 26.7 mg of compound 3 at a purity of over 95%, 53.6 mg of a mixture of compounds 1 and 2, which was further separated by preparative-HPLC yielding 14.3 mg of compound 1 and 25.4 mg of compound 2 each at a purity of over 95%. Their structures were established by spectroscopic methods. The sulfur-containing DKPs suppressed the proliferation of hepatocellular carcinoma cell line HepG2. The present work represents the first application of HSCCC in the efficient preparation of marine fungal natural products. PMID:25584683

  4. 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.%.

  5. Development of High-purity Certified Reference Materials for 17 Proteinogenic Amino Acids by Traceable Titration Methods.

    PubMed

    Kato, Megumi; Yamazaki, Taichi; Kato, Hisashi; Eyama, Sakae; Goto, Mari; Yoshioka, Mariko; Takatsu, Akiko

    2015-01-01

    To ensure the reliability of amino acid analyses, the National Metrology Institute of Japan of the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has developed high-purity certified reference materials (CRMs) for 17 proteinogenic amino acids. These CRMs are intended for use as primary reference materials to enable the traceable quantification of amino acids. The purity of the present CRMs was determined based on two traceable methods: nonaqueous acidimetric titration and nitrogen determination by the Kjeldahl method. Since neither method could distinguish compounds with similar structures, such as amino acid-related impurities, impurities were thoroughly quantified by combining several HPLC methods, and subtracted from the obtained purity of each method. The property value of each amino acid was calculated as a weighted mean of the corrected purities by the two methods. The uncertainty of the property value was obtained by combining measurement uncertainties of the two methods, a difference between the two methods, the uncertainty from the contribution of impurities, and the uncertainty derived from inhomogeneity. The uncertainty derived from instability was considered to be negligible based on stability monitoring of some CRMs. The certified value of each amino acid, property value with uncertainty, was given for both with or without enantiomeric separation.

  6. An electron trap related to phosphorus deficiency in high-purity InP grown by metalorganic chemical vapor deposition

    NASA Astrophysics Data System (ADS)

    Yamamoto, Norio; Uwai, Kunihiko; Takahei, Kenichiro

    1989-04-01

    Deep levels in high-purity InP crystal grown by metalorganic chemical vapor deposition (MOCVD) have been measured by deep level transient spectroscopy. While no electron traps are observed in the samples grown at 600 °C with a [PH3]/[In(C2H5)3] of 170, three electron traps with activation energies of 0.80, 0.44, and 0.24 eV were observed in the samples grown at 500 °C with the same [PH3]/[In(C2H5)3]. The 0.44-eV trap, whose capture cross section is 1.5×10-18 cm2, observed at a low [PH3]/[In(C2H5)3] shows a decrease in concentration as [PH3]/[In(C2H5)3] is increased, and becomes less than 5×1012 cm-3 at a [PH3]/[In(C2H5)3] of more than 170. The comparison of annealing behavior of this trap in MOCVD InP and that in liquid-encapsulated Czochralski InP suggests that the 0.44-eV trap is related to a complex formed from residual impurities and native defects related to a phosphorus deficiency such as phosphorus vacancies or indium interstitials. This trap is found to show configurational bistability similar to that observed for the trap in an Fe-doped InP, MFe center.

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

    Wang, Weiguo, E-mail: wang_weiguo@vip.163.com

    High purity (99.99%) iron samples were cold rolled with a thickness reduction of 87% followed by a annealing at 620 °C for 15 and 45 min, then the grain boundary plane distributions were characterized by electron backscatter diffraction and a stereology and statistics based five parameter analysis. The results showed that the grain boundary planes were mainly distributed on (1 0 0) and such distribution was enhanced obviously when the holding time of annealing increased from 15 to 45 min during which an extensive grain growth and a dramatic texture evolution took place. Further analysis indicated such distribution was largelymore » due to the rotation of grain boundary planes of the [1 0 0] misoriented grains. Additionally, it was also observed that some random boundaries of [1 0 0] misoriented grains were changing from asymmetrical tilt into (1 0 0)/(− 1 0 0) twist when annealing proceeded from 15 to 45 min. Based on the present work and the results reported by other investigators, it was suggested that the chemistry appeared to be critical in determining the grain boundary plane distribution in iron based materials. - Highlights: •Grain boundary (GB) plane distribution (GBPD) in a high purity (99.99%) was studied. •GB planes are mainly distributed on (1 0 0) in the cold rolled and annealed samples. •Such distribution is largely due to the rotation of GB planes of [100] misoriented grains. •Some [1 0 0] asymmetrical tilt boundaries are evolving into twist ones during annealing.« less

  8. Comparison of three methods of DNA extraction from peripheral blood mononuclear cells and lung fragments of equines.

    PubMed

    Santos, E M; Paula, J F R; Motta, P M C; Heinemann, M B; Leite, R C; Haddad, J P A; Del Puerto, H L; Reis, J K P

    2010-08-17

    We compared three different protocols for DNA extraction from horse peripheral blood mononuclear cells (PBMC) and lung fragments, determining average final DNA concentration, purity, percentage of PCR amplification using beta-actin, and cost. Thirty-four samples from PBMC, and 33 samples from lung fragments were submitted to DNA extraction by three different protocols. Protocol A consisted of a phenol-chloroform and isoamylic alcohol extraction, Protocol B used alkaline extraction with NaOH, and Protocol C used the DNAzol((R)) reagent kit. Protocol A was the best option for DNA extraction from lung fragments, producing high DNA concentrations, with high sensitivity in PCR amplification (100%), followed by Protocols C and B. On the other hand, for PBMC samples, Protocol B gave the highest sensitivity in PCR amplification (100%), followed by Protocols C and A. We conclude that Protocol A should be used for PCR diagnosis from lung fragment samples, while Protocol B should be used for PBMC.

  9. Oxygen production using solid-state zirconia electrolyte technology

    NASA Technical Reports Server (NTRS)

    Suitor, Jerry W.; Clark, Douglas J.

    1991-01-01

    High purity oxygen is required for a number of scientific, medical, and industrial applications. Traditionally, these needs have been met by cryogenic distillation or pressure swing adsorption systems designed to separate oxygen from air. Oxygen separation from air via solid-state zirconia electrolyte technology offers an alternative to these methods. The technology has several advantages over the traditional methods, including reliability, compactness, quiet operation, high purity output, and low power consumption.

  10. 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.

  11. 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.

  12. 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

  13. 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.

  14. 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.

  15. 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.

  16. 9 CFR 113.111 - Clostridium Perfringens Type C Toxoid and Bacterin-Toxoid.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... a prescribed test shall not be released. (a) Purity test. Final container samples of completed... § 113.26. (b) Safety test. Bulk or final container samples of completed product from each serial shall be tested for safety as provided in § 113.33(b). (c) Potency test. Bulk or final container samples of...

  17. 9 CFR 113.111 - Clostridium Perfringens Type C Toxoid and Bacterin-Toxoid.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... a prescribed test shall not be released. (a) Purity test. Final container samples of completed... § 113.26. (b) Safety test. Bulk or final container samples of completed product from each serial shall be tested for safety as provided in § 113.33(b). (c) Potency test. Bulk or final container samples of...

  18. 9 CFR 113.111 - Clostridium Perfringens Type C Toxoid and Bacterin-Toxoid.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... a prescribed test shall not be released. (a) Purity test. Final container samples of completed... § 113.26. (b) Safety test. Bulk or final container samples of completed product from each serial shall be tested for safety as provided in § 113.33(b). (c) Potency test. Bulk or final container samples of...

  19. Extraction and isotopic analysis of medium molecular weight hydrocarbons from Murchison using supercritical carbon dioxide

    NASA Technical Reports Server (NTRS)

    Gilmour, Iain; Pillinger, Colin

    1993-01-01

    The large variety of organic compounds present in carbonaceous chondrites poses particular problems in their analysis not the least of which is terrestrial contamination. Conventional analytical approaches employ simple chromatographic techniques to fractionate the extractable compounds into broad classes of similar chemical structure. However, the use of organic solvents and their subsequent removal by evaporation results in the depletion or loss of semi-volatile compounds as well as requiring considerable preparative work to assure solvent purity. Supercritical fluids have been shown to provide a powerful alternative to conventional liquid organic solvents used for analytical extractions. A sample of Murchison from the Field Museum was analyzed. Two interior fragments were used; the first (2.85 g) was crushed in an agate pestel and mortar to a grain size of ca. 50-100 micron, the second (1.80 g) was broken into chips 3-8 mm in size. Each sample was loaded into a stainless steel bomb and placed in the extraction chamber of an Isco supercritical fluid extractor maintained at 35 C. High purity (99.9995 percent) carbon dioxide was used and was pressurized using an Isco syringe pump. The samples were extracted dynamically by flowing CO2 under pressure through the bomb and venting via a 50 micron fused filica capillary into 5 mls of hexane used as a collection solvent. The hexane was maintained at a temperature of 0.5 C. A series of extractions were done on each sample using CO2 of increasing density. The principal components extracted in each fraction are summarized.

  20. Extraction and isotopic analysis of medium molecular weight hydrocarbons from Murchison using supercritical carbon dioxide

    NASA Astrophysics Data System (ADS)

    Gilmour, Iain; Pillinger, Colin

    1993-03-01

    The large variety of organic compounds present in carbonaceous chondrites poses particular problems in their analysis not the least of which is terrestrial contamination. Conventional analytical approaches employ simple chromatographic techniques to fractionate the extractable compounds into broad classes of similar chemical structure. However, the use of organic solvents and their subsequent removal by evaporation results in the depletion or loss of semi-volatile compounds as well as requiring considerable preparative work to assure solvent purity. Supercritical fluids have been shown to provide a powerful alternative to conventional liquid organic solvents used for analytical extractions. A sample of Murchison from the Field Museum was analyzed. Two interior fragments were used; the first (2.85 g) was crushed in an agate pestel and mortar to a grain size of ca. 50-100 micron, the second (1.80 g) was broken into chips 3-8 mm in size. Each sample was loaded into a stainless steel bomb and placed in the extraction chamber of an Isco supercritical fluid extractor maintained at 35 C. High purity (99.9995 percent) carbon dioxide was used and was pressurized using an Isco syringe pump. The samples were extracted dynamically by flowing CO2 under pressure through the bomb and venting via a 50 micron fused filica capillary into 5 mls of hexane used as a collection solvent. The hexane was maintained at a temperature of 0.5 C. A series of extractions were done on each sample using CO2 of increasing density. The principal components extracted in each fraction are summarized.

  1. Polarimetric imaging of biological tissues based on the indices of polarimetric purity.

    PubMed

    Van Eeckhout, Albert; Lizana, Angel; Garcia-Caurel, Enric; Gil, José J; Sansa, Adrià; Rodríguez, Carla; Estévez, Irene; González, Emilio; Escalera, Juan C; Moreno, Ignacio; Campos, Juan

    2018-04-01

    We highlight the interest of using the indices of polarimetric purity (IPPs) to the inspection of biological tissues. The IPPs were recently proposed in the literature and they result in a further synthetization of the depolarizing properties of samples. Compared with standard polarimetric images of biological samples, IPP-based images lead to larger image contrast of some biological structures and to a further physical interpretation of the depolarizing mechanisms inherent to the samples. In addition, unlike other methods, their calculation do not require advanced algebraic operations (as is the case of polar decompositions), and they result in 3 indicators of easy implementation. We also propose a pseudo-colored encoding of the IPP information that leads to an improved visualization of samples. This last technique opens the possibility of tailored adjustment of tissues contrast by using customized pseudo-colored images. The potential of the IPP approach is experimentally highlighted along the manuscript by studying 3 different ex-vivo samples. A significant image contrast enhancement is obtained by using the IPP-based methods, compared to standard polarimetric images. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. 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.

  3. 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.

  4. Thermal Diffusivity in Bone and Hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Calderón, A.; Peña Rodríguez, G.; Muñoz Hernández, R. A.; Díaz Gongora, J. A. I.; Mejia Barradas, C. M.

    2004-09-01

    We report thermal diffusivity measurements in bull bone and commercial hydroxyapatite (HA), both in powder form, in order to determinate the thermal compatibility between these materials. Besides this, we report a comparison between these measured values and those of metallic samples frequently used in implants, as high purity titanium and stainless steel. Our results show a good thermal compatibility (74%) between HA and bone, both in powder form. Finally, it was obtained a one order of magnitude difference between the thermal diffusivity values of metallic samples and those corresponding values to bone and HA being this difference greater in titanium than in stainless steel, which is important to consider in some biomedical and dental applications.

  5. Natural radioactivity measurements in building materials used in Samsun, Turkey.

    PubMed

    Tufan, M Çagatay; Disci, Tugba

    2013-01-01

    In this study, radioactivity levels of 35 different samples of 11 commonly used building materials in Samsun were measured by using a gamma spectrometry system. The analysis carried out with the high purity Germanium gamma spectrometry system. Radioactivity concentrations of (226)Ra, (232)Th and (40)K range from 6 to 54 Bq kg(-1), 5 to 88 Bq kg(-1) and 6 to 1070 Bq kg(-1), respectively. From these results, radium equivalent activities, gamma indexes, absorbed dose rates and annual effective doses were calculated for all samples. Obtained results were compared with the available data, and it was concluded that all the investigated materials did not have radiological risk.

  6. 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.

  7. Dielectric Constant Measurements of Solid 4He

    NASA Astrophysics Data System (ADS)

    Yin, L.; Xia, J. S.; Huan, C.; Sullivan, N. S.; Chan, M. H. W.

    2011-03-01

    Careful measurements of the dielectric properties of solid 4He have been carried out down to 35 mK, considerably lower than the temperature range of previous studies. The sample was prepared from high purity gas with 3He concentrations of the order of 200 ppb and were formed by the blocked capillary method. The molar volume of the sample was 20.30 cm3. The dielectric constant of the samples was found to be independent of temperature down to 120 mK before showing a continuous increase with decreasing temperature and saturating below 50 mK. The total increase in ɛ is 2 parts in 10-5. The temperature dependence of ɛ mimics the increase in the resonant frequency found in the torsional oscillator studies and also the increase found in the shear modulus measurements.

  8. Investigation of magnetic properties of superconductors Y0.98 - x Cax Co0.02 Ba2 Cu3O7 - δ

    NASA Astrophysics Data System (ADS)

    Pourasad, Sepideh; Shakeripour, Hamideh; Hosseini, SeyedSajad; Salamati, Hadi

    2018-06-01

    The effect of Co2+, 3+ and Ca2+ substitution in Y3+ site in YBa2Cu3O7-δ superconductor has been studied. The series of high temperature superconducting samples of Y1-y-xCoyCaxBa2Cu3O7-δ with 0 ≤ x ≤ 0.015 and y = 0.020 were prepared by solid-state reaction method. The samples were characterized for phase purity and lattice parameter variations by X-ray diffraction. The AC susceptibility curves, χ'(T), show that in reserving cobalt fixed sample with the optimum Tc, by substitution of divalent Ca2+ at the trivalent Y3+ site no sensitive increasing happen in the superconducting transition temperature.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. Effect of crystal orientation on conductivity and electron mobility in single-crystal alumina

    NASA Technical Reports Server (NTRS)

    Will, Fritz G.; Delorenzi, Horst G.; Janora, Kevin H.

    1992-01-01

    The electrical conductivity of high-purity, single-crystal alumina is determined parallel to and perpendicular to the c-axis. The mean conductivity of four samples of each orientation is a factor 3.3 higher parallel to the c-axis than perpendicular to it. The conductivity as a function of temperature is attributed to extrinsic electron conduction at temperatures from 400 to 900 C, and intrinsic semiconduction at temperatures from 900 to 1300 C. In the high-temperature regime, the slope on all eight specimens is 4.7 +/- 0.1 eV. Hence, the thermal bandgap at O K is 9.4 +/- 0.2 eV.

  14. 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.

  15. Analysis of Ethyl Acetate Extract of Enzymatic Hydrolysate from High Purity Oleuropein and DPPH Radical Scavenging Capacity

    NASA Astrophysics Data System (ADS)

    Yuan, Jiaojiao; Li, Bing; Qin, Frank G. F.; Tu, Junling

    2018-01-01

    High purify oleuropein (81.04% OL) was hydrolyzed by hemicellulase and phenols was existed in the ethyl acetate extract of enzymatic hydrolysate (EAE). The results presented that there were hydroxytyrosol (HT), tyrosol, caffeic acid, 3,4-dihydroxybenzoic acid, 3,4-dihydroxy phenylacetic acid in EAE by HPLC, and HT content was 19.36%. Antioxidant activities (DPPH radical scavenging capacity) were all added as the samples concentration increased, and dose-effect relationships also existed. HT possessed the highest DPPH radical scavenging capacity, followed by Vc, and eugenol, OL, caffeic acid, 3,4-dihydroxy phenylacetic acid and 3,4-dihydroxybenzoic acid.

  16. 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)

  17. 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.

  18. 9 CFR 113.110 - Clostridium Botulinum Type C Bacterin-Toxoid.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ..., safety, and potency as prescribed in this section. A serial found unsatisfactory by any prescribed test shall not be released. (a) Purity test. Final container samples of completed product from each serial... test. Bulk or final container samples of completed product from each serial shall be tested for safety...

  19. 9 CFR 113.110 - Clostridium Botulinum Type C Bacterin-Toxoid.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ..., safety, and potency as prescribed in this section. A serial found unsatisfactory by any prescribed test shall not be released. (a) Purity test. Final container samples of completed product from each serial... test. Bulk or final container samples of completed product from each serial shall be tested for safety...

  20. Comparison of Support Vector Machine, Neural Network, and CART Algorithms for the Land-Cover Classification Using Limited Training Data Points

    EPA Science Inventory

    Support vector machine (SVM) was applied for land-cover characterization using MODIS time-series data. Classification performance was examined with respect to training sample size, sample variability, and landscape homogeneity (purity). The results were compared to two convention...

  1. 9 CFR 114.17 - Rebottling of biological products.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... section. (a) All or part of a serial which has not left the licensed establishment may be aseptically returned to the mixing tank, thoroughly mixed, and rebottled in new final containers. (b) The rebottled...) Required purity tests for final container samples of the product shall be conducted on new samples selected...

  2. 9 CFR 114.17 - Rebottling of biological products.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... section. (a) All or part of a serial which has not left the licensed establishment may be aseptically returned to the mixing tank, thoroughly mixed, and rebottled in new final containers. (b) The rebottled...) Required purity tests for final container samples of the product shall be conducted on new samples selected...

  3. 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.

  4. Electrophoresis for the analysis of heparin purity and quality.

    PubMed

    Volpi, Nicola; Maccari, Francesca; Suwan, Jiraporn; Linhardt, Robert J

    2012-06-01

    The adulteration of raw heparin with oversulfated chondroitin sulfate (OSCS) in 2007-2008 produced a global crisis resulting in extensive revisions to the pharmacopeia monographs and prompting the FDA to recommend the development of additional methods for the analysis of heparin purity. As a consequence, a wide variety of innovative analytical approaches have been developed for the quality assurance and purity of unfractionated and low-molecular-weight heparins. This review discusses recent developments in electrophoresis techniques available for the sensitive separation, detection, and partial structural characterization of heparin contaminants. In particular, this review summarizes recent publications on heparin quality and related impurity analysis using electrophoretic separations such as capillary electrophoresis (CE) of intact polysaccharides and hexosamines derived from their acidic hydrolysis, and polyacrylamide gel electrophoresis (PAGE) for the separation of heparin samples without and in the presence of its relatively specific depolymerization process with nitrous acid treatment. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Electrophoresis for the analysis of heparin purity and quality

    PubMed Central

    Volpi, Nicola; Maccari, Francesca; Suwan, Jiraporn; Linhardt, Robert J.

    2012-01-01

    The adulteration of raw heparin with oversulfated chondroitin sulfate (OSCS) in 2007–2008 produced a global crisis resulting in extensive revisions to the pharmacopeia monographs and prompting the FDA to recommend the development of additional methods for the analysis of heparin purity. As a consequence, a wide variety of innovative analytical approaches have been developed for the quality assurance and purity of unfractionated and low-molecular-weight heparins. This review discusses recent developments in electrophoresis techniques available for the sensitive separation, detection, and partial structural characterization of heparin contaminants. In particular, this review summarizes recent publications on heparin quality and related impurity analysis using electrophoretic separations such as capillary electrophoresis (CE) of intact polysaccharides and hexosamines derived from their acidic hydrolysis, and polyacrylamide gel electrophoresis (PAGE) for the separation of heparin samples without and in the presence of its relatively specific depolymerization process with nitrous acid treatment. PMID:22736353

  6. Electrolytic production of high purity aluminum using inert anodes

    DOEpatents

    Ray, Siba P.; Liu, Xinghua; Weirauch, Jr., Douglas A.

    2001-01-01

    A method of producing commercial purity aluminum in an electrolytic reduction cell comprising inert anodes is disclosed. The method produces aluminum having acceptable levels of Fe, Cu and Ni impurities. The inert anodes used in the process preferably comprise a cermet material comprising ceramic oxide phase portions and metal phase portions.

  7. Fluorescence Properties of Fe2+- and Co2+-doped Hosts of CdMnTe Compositions as Potential Mid-Infrared Laser Materials

    DTIC Science & Technology

    2011-09-01

    composition also affects the Co2+ and Fe2+ dopant lifetimes and temperature dependencies. Crystal growth effort is underway in order to improve the...single-crystalline samples of Fe2+ or divalent cobalt ion (Co2+)-doped CMT crystals were produced by Brimrose Corporation using a modified vertical...Bridgman technique (18). The starting high purity ingredients Cd, Mn, and Te along with the dopants (Fe and Co) are placed in a pre-cleaned and baked

  8. 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

  9. 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.

  10. 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

  11. 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).

  12. 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.

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. Impact of South American heroin on the US heroin market 1993-2004.

    PubMed

    Ciccarone, Daniel; Unick, George J; Kraus, Allison

    2009-09-01

    The past two decades have seen an increase in heroin-related morbidity and mortality in the United States. We report on trends in US heroin retail price and purity, including the effect of entry of Colombian-sourced heroin on the US heroin market. The average standardized price ($/mg-pure) and purity (% by weight) of heroin from 1993 to 2004 was from obtained from US Drug Enforcement Agency retail purchase data for 20 metropolitan statistical areas. Univariate statistics, robust Ordinary Least Squares regression and mixed fixed and random effect growth curve models were used to predict the price and purity data in each metropolitan statistical area over time. Over the 12 study years, heroin price decreased 62%. The median percentage of all heroin samples that are of South American origin increased an absolute 7% per year. Multivariate models suggest percent South American heroin is a significant predictor of lower heroin price and higher purity adjusting for time and demographics. These analyses reveal trends to historically low-cost heroin in many US cities. These changes correspond to the entrance into and rapid domination of the US heroin market by Colombian-sourced heroin. The implications of these changes are discussed.

  18. Performance of Mercury Triple-Point Cells Made in Brazil

    NASA Astrophysics Data System (ADS)

    Petkovic, S. G.; Santiago, J. F. N.; Filho, R. R.; Teixeira, R. N.; Santos, P. R. F.

    2003-09-01

    Fixed-points cells are primary standards in ITS-90. They contain reference material with a purity of 99.999 % or more. The gallium in a melting-point cell, for example, can reach a purity of 99.99999 %. This level of purity is not easy to obtain. However, substances like water and mercury can be purified by means of distillation and chemical procedures. This paper presents the results of mercury triple-point cells made in Brazil that were directly compared to a mercury triple-point cell of 99.999% purity. This reference cell, made by Isotech (England), was previously compared to cells from CENAM (Mexico) and NRC (Canada) and the maximum deviation found was approximately 0.4 mK. The purification stage started with a sample of mercury 99.3 % pure, and the repeated use of both mechanical and chemical processes led to a purification grade considered good enough for calibration of standard platinum resistance thermometers. The purification procedures, the method of construction of the cell, the laboratory facilities, the comparison results and the budget of uncertainties are described in this paper. All of the cells tested have a triple-point temperature within 0.25 mK of the triple-point temperature of the Inmetro reference cell.

  19. Investigation of the shear response and geometrically necessary dislocation densities in shear localization in high-purity titanium

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

    Zhu, Chaoyi; Livescu, Veronica; Harrington, Tyler

    The influence of microstructural anisotropy on shear response of high-purity titanium was studied using the compact forced-simple-shear specimen (CFSS) loaded under quasi-static loading conditions. Post-mortem characterization reveals significant difference in shear response of different directions in the same material due to material crystallographic texture anisotropy. Shear bands are narrower in specimens in which the shear zone is aligned along the direction with a strong {0001} basal texture. Twinning was identified as an active mechanism to accommodate strains in the shear region in both orientations. This paper confirms the applicability of the CFSS design for the investigation of differences in themore » shear response of materials as a function of process-induced crystallographic texture. A detailed, systematic approach to quantifying shear band evolution by evaluating geometrically necessary dislocations (GND) associated with crystallographic anisotropy is presented. Finally, the results show that: i) line average GND density profiles, for Ti samples that possess a uniform equiaxed-grain structure, but with strong crystallographic anisotropy, exhibit significant differences in GND density close to the shear band center; ii) GND profiles decrease steadily away from the shear band as the plastic strain diminishes, in agreement with Ashby's theory of work hardening, where the higher GND density in the through-thickness (TT) orientation is a result of restricted < a > type slip in the shear band compared with in-plane (IP) samples; iii) the anisotropy in deformation response is derived from initial crystallographic texture of the materials, where GND density of < a > GNDs are higher adjacent to the shear band in the through-thickness sample oriented away from easy slip, but the density of < c+a > type GNDs are very similar in these two samples; and iv) the increase in grain average GND density was determined to have strong correlation to an increase in the Euler Φ angle of the grain average orientation, indicating an increased misorientation angle evolution.« less

  20. Investigation of the shear response and geometrically necessary dislocation densities in shear localization in high-purity titanium

    DOE PAGES

    Zhu, Chaoyi; Livescu, Veronica; Harrington, Tyler; ...

    2017-03-31

    The influence of microstructural anisotropy on shear response of high-purity titanium was studied using the compact forced-simple-shear specimen (CFSS) loaded under quasi-static loading conditions. Post-mortem characterization reveals significant difference in shear response of different directions in the same material due to material crystallographic texture anisotropy. Shear bands are narrower in specimens in which the shear zone is aligned along the direction with a strong {0001} basal texture. Twinning was identified as an active mechanism to accommodate strains in the shear region in both orientations. This paper confirms the applicability of the CFSS design for the investigation of differences in themore » shear response of materials as a function of process-induced crystallographic texture. A detailed, systematic approach to quantifying shear band evolution by evaluating geometrically necessary dislocations (GND) associated with crystallographic anisotropy is presented. Finally, the results show that: i) line average GND density profiles, for Ti samples that possess a uniform equiaxed-grain structure, but with strong crystallographic anisotropy, exhibit significant differences in GND density close to the shear band center; ii) GND profiles decrease steadily away from the shear band as the plastic strain diminishes, in agreement with Ashby's theory of work hardening, where the higher GND density in the through-thickness (TT) orientation is a result of restricted < a > type slip in the shear band compared with in-plane (IP) samples; iii) the anisotropy in deformation response is derived from initial crystallographic texture of the materials, where GND density of < a > GNDs are higher adjacent to the shear band in the through-thickness sample oriented away from easy slip, but the density of < c+a > type GNDs are very similar in these two samples; and iv) the increase in grain average GND density was determined to have strong correlation to an increase in the Euler Φ angle of the grain average orientation, indicating an increased misorientation angle evolution.« less

  1. Atmospheric deposition of {sup 7}Be by rain events, incentral Argentina

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

    Ayub, J. Juri; Velasco, H.; Rizzotto, M.

    2008-08-07

    Beryllium-7 is a natural radionuclide that enters into the ecosystems through wet and dry depositions and has numerous environmental applications in terrestrial and aquatic ecosystems. Atmospheric wet deposition of {sup 7}Be was measured in central Argentina. Rain traps were installed (1 m above ground) and individual rain events have been collected. Rain samples were filtered and analyzed by gamma spectrometry. The gamma counting was undertaken using a 40%-efficient p-type coaxial intrinsic high-purity natural germanium crystal built by Princeton Gamma-Tech. The cryostat was made from electroformed high-purity copper using ultralow-background technology. The detector was surrounded by 50 cm of lead bricksmore » to provide shielding against radioactive background. The detector gamma efficiency was determined using a water solution with known amounts of chemical compounds containing long-lived naturally occurring radioisotopes, {sup 176}Lu, {sup 138}La and {sup 40}K. Due to the geometry of the sample and its position close to the detector, the efficiency points from the {sup 176}Lu decay, had to be corrected for summing effects. The measured samples were 400 ml in size and were counted curing one day. The {sup 7}Be detection limit for the present measurements was as low as 0.2 Bq l{sup -1}. Thirty two rain events were sampled and analyzed (November 2006-May 2007). The measured values show that the events corresponding to low rainfall (<20 mm) are characterized by significantly higher activity concentrations (Bq l{sup -1}). The activity concentration of each individual event varied from 0.8 to 3.5 Bq l{sup -1}, while precipitations varied between 4 and 70 mm. The integrated activity by event of {sup 7}Be was fitted with a model that takes into account the precipitation amount and the elapsed time between two rain events. The integrated activities calculated with this model show a good agreement with experimental values.« less

  2. Low–Cost Bio-Based Carbon Fiber for High-Temperature Processing

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

    Naskar, Amit K.; Akato, Kokouvi M.; Tran, Chau D.

    GrafTech International Holdings Inc. (GTI), worked with Oak Ridge National Laboratory (ORNL) under CRADA No. NFE-15-05807 to develop lignin-based carbon fiber (LBCF) technology and to demonstrate LBCF performance in high-temperature products and applications. This work was unique and different from other reported LBCF work in that this study was application-focused and scalability-focused. Accordingly, the executed work was based on meeting criteria based on technology development, cost, and application suitability. The focus of this work was to demonstrate lab-scale LBCF from at least 4 different precursor feedstock sources that could meet the estimated production cost of $5.00/pound and have ash levelmore » of less than 500 ppm in the carbonized insulation-grade fiber. Accordingly, a preliminary cost model was developed based on publicly available information. The team demonstrated that 4 lignin samples met the cost criteria, as highlighted in Table 1. In addition, the ash level for the 4 carbonized lignin samples were below 500 ppm. Processing asreceived lignin to produce a high purity lignin fiber was a significant accomplishment in that most industrial lignin, prior to purification, had greater than 4X the ash level needed for this project, and prior to this work there was not a clear path of how to achieve the purity target. The lab scale development of LBCF was performed with a specific functional application in mind, specifically for high temperature rigid insulation. GTI is currently a consumer of foreignsourced pitch and rayon based carbon fibers for use in its high temperature insulation products, and the motivation was that LBCF had potential to decrease costs and increase product competitiveness in the marketplace through lowered raw material costs, lowered energy costs, and decreased environmental footprint. At the end of this project, the Technology Readiness Level (TRL) remained at 5 for LBCF in high temperature insulation.« less

  3. 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.

  4. 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.

  5. 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.

  6. Plasma membrane characterization, by scanning electron microscopy, of multipotent myoblasts-derived populations sorted using dielectrophoresis.

    PubMed

    Muratore, Massimo; Mitchell, Steve; Waterfall, Martin

    2013-09-06

    Multipotent progenitor cells have shown promise for use in biomedical applications and regenerative medicine. The implementation of such cells for clinical application requires a synchronized, phenotypically and/or genotypically, homogenous cell population. Here we have demonstrated the implementation of a biological tag-free dielectrophoretic device used for discrimination of multipotent myoblastic C2C12 model. The multipotent capabilities in differentiation, for these cells, diminishes with higher passage number, so for cultures above 70 passages only a small percentage of cells is able to differentiate into terminal myotubes. In this work we demonstrated that we could recover, above 96% purity, specific cell types from a mixed population of cells at high passage number without any biological tag using dielectrophoresis. The purity of the samples was confirmed by cytometric analysis using the cell specific marker embryonic myosin. To further investigate the dielectric properties of the cell plasma membrane we co-culture C2C12 with similar size, when in suspension, GFP-positive fibroblast as feeder layer. The level of separation between the cell types was above 98% purity which was confirmed by flow cytometry. These levels of separation are assumed to account for cell size and for the plasma membrane morphological differences between C2C12 and fibroblast unrelated to the stages of the cell cycle which was assessed by immunofluorescence staining. Plasma membrane conformational differences were further confirmed by scanning electron microscopy. Copyright © 2013 Elsevier Inc. All rights reserved.

  7. 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

  8. Genotyping of Single Nucleotide Polymorphisms in DNA Isolated from Serum Using Sequenom MassARRAY Technology.

    PubMed

    Clendenen, Tess V; Rendleman, Justin; Ge, Wenzhen; Koenig, Karen L; Wirgin, Isaac; Currie, Diane; Shore, Roy E; Kirchhoff, Tomas; Zeleniuch-Jacquotte, Anne

    2015-01-01

    Large epidemiologic studies have the potential to make valuable contributions to the assessment of gene-environment interactions because they prospectively collected detailed exposure data. Some of these studies, however, have only serum or plasma samples as a low quantity source of DNA. We examined whether DNA isolated from serum can be used to reliably and accurately genotype single nucleotide polymorphisms (SNPs) using Sequenom multiplex SNP genotyping technology. We genotyped 81 SNPs using samples from 158 participants in the NYU Women's Health Study. Each participant had DNA from serum and at least one paired DNA sample isolated from a high quality source of DNA, i.e. clots and/or cell precipitates, for comparison. We observed that 60 of the 81 SNPs (74%) had high call frequencies (≥95%) using DNA from serum, only slightly lower than the 85% of SNPs with high call frequencies in DNA from clots or cell precipitates. Of the 57 SNPs with high call frequencies for serum, clot, and cell precipitate DNA, 54 (95%) had highly concordant (>98%) genotype calls across all three sample types. High purity was not a critical factor to successful genotyping. Our results suggest that this multiplex SNP genotyping method can be used reliably on DNA from serum in large-scale epidemiologic studies.

  9. NMR Spectroscopy Using a Chiral Lanthanide Shift Reagent to Assess the Optical Purity of 1-Phenylethylamine

    NASA Astrophysics Data System (ADS)

    Viswanathan, Tito; Toland, Alan

    1995-10-01

    Enantiomeric forms of 1-phenylethylamine cannot be distinguished by 1H or 13C-NMR because the groups attached to the stereocenter are in an enantiopic environment. However, the chemical shifts of the protons in the groups attached to the stereocenter can be differentially altered to appear as distinct peaks in the NMR spectrum. This is accomplished by the use of a commercially available chiral lanthanide shift reagent, Yb(tfC)3. The NMR spectrum after the addition of a chiral shift reagent allows one to assess the optical purity of the sample.

  10. 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).

  11. Resolution of the carbon contamination problem in ion irradiation experiments

    NASA Astrophysics Data System (ADS)

    Was, G. S.; Taller, S.; Jiao, Z.; Monterrosa, A. M.; Woodley, D.; Jennings, D.; Kubley, T.; Naab, F.; Toader, O.; Uberseder, E.

    2017-12-01

    The widely experienced problem of carbon uptake in samples during ion irradiation was systematically investigated to identify the source of carbon and to develop mitigation techniques. Possible sources of carbon included carbon ions or neutrals incorporated into the ion beam, hydrocarbons in the vacuum system, and carbon species on the sample and fixture surfaces. Secondary ion mass spectrometry, atom probe tomography, elastic backscattering spectrometry, and principally, nuclear reaction analysis, were used to profile carbon in a variety of substrates prior to and following irradiation with Fe2+ ions at high temperature. Ion irradiation of high purity Si and Ni, and also of alloy 800H coated with a thin film of alumina eliminated the ion beam as the source of carbon. Hydrocarbons in the vacuum and/or on the sample and fixtures was the source of the carbon that became incorporated into the samples during irradiation. Plasma cleaning of the sample and sample stage, and incorporation of a liquid nitrogen cold trap both individually and especially in combination, completely eliminated the uptake of carbon during heavy ion irradiation. While less convenient, coating the sample with a thin film of alumina was also effective in eliminating carbon incorporation.

  12. Forensic discrimination of copper wire using trace element concentrations.

    PubMed

    Dettman, Joshua R; Cassabaum, Alyssa A; Saunders, Christopher P; Snyder, Deanna L; Buscaglia, JoAnn

    2014-08-19

    Copper may be recovered as evidence in high-profile cases such as thefts and improvised explosive device incidents; comparison of copper samples from the crime scene and those associated with the subject of an investigation can provide probative associative evidence and investigative support. A solution-based inductively coupled plasma mass spectrometry method for measuring trace element concentrations in high-purity copper was developed using standard reference materials. The method was evaluated for its ability to use trace element profiles to statistically discriminate between copper samples considering the precision of the measurement and manufacturing processes. The discriminating power was estimated by comparing samples chosen on the basis of the copper refining and production process to represent the within-source (samples expected to be similar) and between-source (samples expected to be different) variability using multivariate parametric- and empirical-based data simulation models with bootstrap resampling. If the false exclusion rate is set to 5%, >90% of the copper samples can be correctly determined to originate from different sources using a parametric-based model and >87% with an empirical-based approach. These results demonstrate the potential utility of the developed method for the comparison of copper samples encountered as forensic evidence.

  13. Dose estimation and dating of pottery from Turkey

    NASA Astrophysics Data System (ADS)

    Altay Atlıhan, M.; Şahiner, Eren; Soykal Alanyalı, Feriştah

    2012-06-01

    The luminescence method is a widely used technique for environmental dosimetry and dating archaeological, geological materials. In this study, equivalent dose (ED) and annual dose rate (AD) of an archaeological sample were measured. The age of the material was calculated by means of equivalent dose divided by the annual dose rate. The archaeological sample was taken from Antalya, Turkey. Samples were prepared by the fine grain technique and equivalent dose was found using multiple-aliquot-additive-dose (MAAD) and single aliquot regeneration (SAR) techniques. Also the short shine normalization-MAAD and long shine normalization-MAAD were applied and the results of the methods were compared with each other. The optimal preheat temperature was found to be 200 °C for 10 min. The annual doses of concentrations of the major radioactive isotopes were determined using a high-purity germanium detector and a low-level alpha counter. The age of the sample was found to be 510±40 years.

  14. Comparison of methods for the extraction of DNA from formalin-fixed, paraffin-embedded archival tissues.

    PubMed

    Sengüven, Burcu; Baris, Emre; Oygur, Tulin; Berktas, Mehmet

    2014-01-01

    Discussing a protocol involving xylene-ethanol deparaffinization on slides followed by a kit-based extraction that allows for the extraction of high quality DNA from FFPE tissues. DNA was extracted from the FFPE tissues of 16 randomly selected blocks. Methods involving deparaffinization on slides or tubes, enzyme digestion overnight or for 72 hours and isolation using phenol chloroform method or a silica-based commercial kit were compared in terms of yields, concentrations and the amplifiability. The highest yield of DNA was produced from the samples that were deparaffinized on slides, digested for 72 hours and isolated with a commercial kit. Samples isolated with the phenol-chloroform method produced DNA of lower purity than the samples that were purified with kit. The samples isolated with the commercial kit resulted in better PCR amplification. Silica-based commercial kits and deparaffinized on slides should be considered for DNA extraction from FFPE.

  15. Field analyses of (238)U and (226)Ra in two uranium mill tailings piles from Niger using portable HPGe detector.

    PubMed

    Déjeant, Adrien; Bourva, Ludovic; Sia, Radia; Galoisy, Laurence; Calas, Georges; Phrommavanh, Vannapha; Descostes, Michael

    2014-11-01

    The radioactivities of (238)U and (226)Ra in mill tailings from the U mines of COMINAK and SOMAÏR in Niger were measured and quantified using a portable High-Purity Germanium (HPGe) detector. The (238)U and (226)Ra activities were measured under field conditions on drilling cores with 600s measurements and without any sample preparation. Field results were compared with those obtained by Inductive Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and emanometry techniques. This comparison indicates that gamma-ray absorption by such geological samples does not cause significant deviations. This work shows the feasibility of using portable HPGe detector in the field as a preliminary method to observe variations of radionuclides concentration with the aim of identifying samples of interest. The HPGe is particularly useful for samples with strong secular disequilibrium such as mill tailings. Copyright © 2014 Elsevier Ltd. All rights reserved.

  16. 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.

  17. 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.

  18. 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...

  19. 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...

  20. Effect of purity on adsorption capacities of a Mars-like clay mineral at different pressures

    NASA Technical Reports Server (NTRS)

    Jenkins, Traci; Mcdoniel, Bridgett; Bustin, Roberta; Allton, Judith H.

    1992-01-01

    There has been considerable interest in adsorption of carbon dioxide on Marslike clay minerals. Some estimates of the carbon dioxide reservoir capacity of the martian regolith were calculated from the amount of carbon dioxide adsorbed on the ironrich smectite nontronite under martian conditions. The adsorption capacity of pure nontronite could place upper limits on the regolith carbon dioxide reservoir, both at present martian atmospheric pressure and at the postulated higher pressures required to permit liquid water on the surface. Adsorption of carbon dioxide on a Clay Mineral Society standard containing nontronite was studied over a wide range of pressures in the absence of water. Similar experiments were conducted on the pure nontronite extracted from the natural sample. Heating curves were obtained to help characterize and determine the purity of the clay sample.

  1. 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.

  2. 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.

  3. The moral foundations hypothesis does not replicate well in Black samples.

    PubMed

    Davis, Don E; Rice, Kenneth; Van Tongeren, Daryl R; Hook, Joshua N; DeBlaere, Cirleen; Worthington, Everett L; Choe, Elise

    2016-04-01

    The current study examined the generalizability of the moral foundations hypothesis (Graham, Haidt, & Nosek, 2009), which predicts that conservatism will be positively related to the binding foundations (i.e., virtues of ingroup/loyalty, authority/respect, and purity/sanctity). Religiosity has been consistently linked with the binding foundations in predominately White samples, but Black people in the United States are both more religious and more liberal than White people. In a sample of college students (N = 693; 58.3% Black, 41.7% White), examination of measurement invariance suggested metric, but not scalar invariance. The relationship between conservatism and the binding foundations-specifically, respect/authority and purity/sanctity-was weaker in Black people than in White people. These results were replicated in a second sample (N = 490; 63.5% Black, 36.5% White) using a 4-item measure of conservatism rather than a single item. Once again examination of measurement invariance suggested metric but not scalar invariance, and conservatism was more weakly related to the binding foundations in Black people than it was in White people. Implications for future theory and research are discussed. (c) 2016 APA, all rights reserved).

  4. 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.

  5. Bulk damage and absorption in fused silica due to high-power laser applications

    NASA Astrophysics Data System (ADS)

    Nürnberg, F.; Kühn, B.; Langner, A.; Altwein, M.; Schötz, G.; Takke, R.; Thomas, S.; Vydra, J.

    2015-11-01

    Laser fusion projects are heading for IR optics with high broadband transmission, high shock and temperature resistance, long laser durability, and best purity. For this application, fused silica is an excellent choice. The energy density threshold on IR laser optics is mainly influenced by the purity and homogeneity of the fused silica. The absorption behavior regarding the hydroxyl content was studied for various synthetic fused silica grades. The main absorption influenced by OH vibrational excitation leads to different IR attenuations for OH-rich and low-OH fused silica. Industrial laser systems aim for the maximum energy extraction possible. Heraeus Quarzglas developed an Yb-doped fused silica fiber to support this growing market. But the performance of laser welding and cutting systems is fundamentally limited by beam quality and stability of focus. Since absorption in the optical components of optical systems has a detrimental effect on the laser focus shift, the beam energy loss and the resulting heating has to be minimized both in the bulk materials and at the coated surfaces. In collaboration with a laser research institute, an optical finisher and end users, photo thermal absorption measurements on coated samples of different fused silica grades were performed to investigate the influence of basic material properties on the absorption level. High purity, synthetic fused silica is as well the material of choice for optical components designed for DUV applications (wavelength range 160 nm - 260 nm). For higher light intensities, e.g. provided by Excimer lasers, UV photons may generate defect centers that effect the optical properties during usage, resulting in an aging of the optical components (UV radiation damage). Powerful Excimer lasers require optical materials that can withstand photon energy close to the band gap and the high intensity of the short pulse length. The UV transmission loss is restricted to the DUV wavelength range below 300 nm and consists of three different absorption bands centered at 165 nm (peroxy radicals), 215 nm (E'-center), and 265 nm (non-bridging oxygen hole center (NBOH)), which change the transmission behavior of material.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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

  12. Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO₃ Ceramics Fabricated by Spark Plasma Sintering.

    PubMed

    Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

    2017-03-07

    Based on precursor powders with a size of 200-300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO₃ ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO₃ ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe 3+ to Fe 2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO₃ ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage.

  13. Synchrotron-induced X-ray fluorescence from rat bone and lumber vertebra of different age groups

    NASA Astrophysics Data System (ADS)

    Rao, Donepudi V.; Swapna, Medasani; Cesareo, Roberto; Brunetti, Antonio; Akatsuka, Tako; Yuasa, Tetsuya; Takeda, Tohoru; Tromba, Giuliana; Gigante, Giovanni E.

    2009-02-01

    The fluorescence spectra from rat bones of different age groups (8, 56 and 78 weeks) and lumber vertebra were measured with 8, 10 and 12 keV synchrotron X-rays. We have utilized the new hard X-ray micro-spectroscopy beamline facility, X27A, available at NSLS with a primary beam spot size of the order of ˜10 μm. With this spatial resolution and high flux throughput, X-ray fluorescent intensities for Ca and other trace elements were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. Regarding the lumber vertebra, we acquired the fluorescence spectra from the left, right and middle portions and calcium accumulation was evaluated and compared with the other samples. We have identified the major trace elements of Ca, Ni, Fe and Zn and minor trace elements of Ti, Cr and Mn in the sample. The percentage of scattered radiation and trace element contributions from these samples were highlighted at different energies.

  14. Method of extruding and packaging a thin sample of reactive material including forming the extrusion die

    DOEpatents

    Lewandowski, Edward F.; Peterson, Leroy L.

    1985-01-01

    This invention teaches a method of cutting a narrow slot in an extrusion die with an electrical discharge machine by first drilling spaced holes at the ends of where the slot will be, whereby the oil can flow through the holes and slot to flush the material eroded away as the slot is being cut. The invention further teaches a method of extruding a very thin ribbon of solid highly reactive material such as lithium or sodium through the die in an inert atmosphere of nitrogen, argon or the like as in a glovebox. The invention further teaches a method of stamping out sample discs from the ribbon and of packaging each disc by sandwiching it between two aluminum sheets and cold welding the sheets together along an annular seam beyond the outer periphery of the disc. This provides a sample of high purity reactive material that can have a long shelf life.

  15. Method of extruding and packaging a thin sample of reactive material, including forming the extrusion die

    DOEpatents

    Lewandowski, E.F.; Peterson, L.L.

    1981-11-30

    This invention teaches a method of cutting a narrow slot in an extrusion die with an electrical discharge machine by first drilling spaced holes at the ends of where the slot will be, whereby the oil can flow through the holes and slot to flush the material eroded away as the slot is being cut. The invention further teaches a method of extruding a very thin ribbon of solid highly reactive material such as lithium or sodium through the die in an inert atmosphere of nitrogen, argon, or the like as in a glovebox. The invention further teaches a method of stamping out sample discs from the ribbon and of packaging each disc by sandwiching it between two aluminum sheets and cold welding the sheets together along an annular seam beyond the outer periphery of the disc. This provides a sample of high purity reactive material that can have a long shelf life.

  16. Electrodrift purification of materials for room temperature radiation detectors

    DOEpatents

    James, R.B.; Van Scyoc, J.M. III; Schlesinger, T.E.

    1997-06-24

    A method of purifying nonmetallic, crystalline semiconducting materials useful for room temperature radiation detecting devices by applying an electric field across the material is disclosed. The present invention discloses a simple technology for producing purified ionic semiconducting materials, in particular PbI{sub 2} and preferably HgI{sub 2}, which produces high yields of purified product, requires minimal handling of the material thereby reducing the possibility of introducing or reintroducing impurities into the material, is easy to control, is highly selective for impurities, retains the stoichiometry of the material and employs neither high temperatures nor hazardous materials such as solvents or liquid metals. An electric field is applied to a bulk sample of the material causing impurities present in the sample to drift in a preferred direction. After all of the impurities have been transported to the ends of the sample the current flowing through the sample, a measure of the rate of transport of mobile impurities, falls to a low, steady state value, at which time the end sections of the sample where the impurities have concentrated are removed leaving a bulk sample of higher purity material. Because the method disclosed here only acts on the electrically active impurities, the stoichiometry of the host material remains substantially unaffected. 4 figs.

  17. Electrodrift purification of materials for room temperature radiation detectors

    DOEpatents

    James, Ralph B.; Van Scyoc, III, John M.; Schlesinger, Tuviah E.

    1997-06-24

    A method of purifying nonmetallic, crystalline semiconducting materials useful for room temperature radiation detecting devices by applying an electric field across the material. The present invention discloses a simple technology for producing purified ionic semiconducting materials, in particular PbI.sub.2 and preferably HgI.sub.2, which produces high yields of purified product, requires minimal handling of the material thereby reducing the possibility of introducing or reintroducing impurities into the material, is easy to control, is highly selective for impurities, retains the stoichiometry of the material and employs neither high temperatures nor hazardous materials such as solvents or liquid metals. An electric field is applied to a bulk sample of the material causing impurities present in the sample to drift in a preferred direction. After all of the impurities have been transported to the ends of the sample the current flowing through the sample, a measure of the rate of transport of mobile impurities, falls to a low, steady state value, at which time the end sections of the sample where the impurities have concentrated are removed leaving a bulk sample of higher purity material. Because the method disclosed here only acts on the electrically active impurities, the stoichiometry of the host material remains substantially unaffected.

  18. An automated synthesis-purification-sample-management platform for the accelerated generation of pharmaceutical candidates.

    PubMed

    Sutherland, J David; Tu, Noah P; Nemcek, Thomas A; Searle, Philip A; Hochlowski, Jill E; Djuric, Stevan W; Pan, Jeffrey Y

    2014-04-01

    A flexible and integrated flow-chemistry-synthesis-purification compound-generation and sample-management platform has been developed to accelerate the production of small-molecule organic-compound drug candidates in pharmaceutical research. Central to the integrated system is a Mitsubishi robot, which hands off samples throughout the process to the next station, including synthesis and purification, sample dispensing for purity and quantification analysis, dry-down, and aliquot generation.

  19. Sampled-data design for sliding mode control based on various robust specifications in open quantum system

    NASA Astrophysics Data System (ADS)

    Ji, Yinghua; Ju-Ju, Hu; Jian-Hua, Huang; Qiang, Ke

    Due to the influence of decoherence, the quantum state probably evolves from the initial pure state to the mixed state, resulting in loss of fidelity, coherence and purity, which is deteriorating for quantum information transmission. Thus, in quantum engineering, quantum control should not only realize the transfer and track of quantum states through manipulation of the external electromagnetic field but also enhance the robustness against decoherence. In this paper, we aim to design a control law to steer the system into the sliding mode domain and maintain it in that domain when bounded uncertainties exist in the system Hamiltonian. We first define the required control performance by fidelity, degree of coherence and purity in terms of the uncertainty of the Hamiltonian in Markovian open quantum system. By characterizing the required robustness using a sliding mode domain, a sampled-data design method is introduced for decoherence control in the quantum system. Furthermore, utilizing the sampled data, a control scheme has been designed on the basis of sliding mode control, and the choice of sampling operator and driving of quantum state during the sampling by the Lyapunov control method are discussed.

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. Development of a Small, Inexpensive, and Field-deployable Gas Chromatograph for the Automated Collection, Separation, and Analysis of Gas-phase Organic Compounds

    NASA Astrophysics Data System (ADS)

    Skog, K.; Xiong, F.; Gentner, D. R.

    2017-12-01

    The identification and quantification of gas-phase organic compounds, like volatile organic compounds (VOCs), in the atmosphere relies on separation of complex mixtures and sensitive detection. Gas chromatography (GC) is widely applied, but relies on the need for high-purity compressed gases for separation and, often for detection. We have developed a low-cost, compact GC-based system for the collection and quantitative chemical speciation of complex mixtures of common atmospheric VOCs without the need for compressed high-purity gases or expensive detectors. We present results of lab and field testing against a commercially-available GC system. At optimized linear velocities challenging VOC pairs of similar volatility were resolved within 30 minutes, including n- and i-pentane; n-pentane and isoprene; and ethylbenzene and m/p-xylene. For 5-30 minute samples, we observe ppt-level detection limits for common VOCs such as benzene, toluene, ethylbenzene, xylenes, alpha-pinene, and limonene. We also present results of in-field use for VOC measurements. In all, this instrument is accurate, precise, small, and inexpensive (<$2500). Its lack of compressed gas cylinders make it ideal for field deployment and has been demonstrated to produce similar quality data to available GC technology.

  5. Dislocation loops in ultra-high purity Fe(Cr) alloys after 7.2 MeV proton irradiation

    NASA Astrophysics Data System (ADS)

    Chen, J.; Duval, F.; Jung, P.; Schäublin, R.; Gao, N.; Barthe, M. F.

    2018-05-01

    Ultra-high purity Fe(Cr) alloys (from 0 wt% Cr to 14 wt% Cr) were 3D homogeneously irradiated by 0-7.2 MeV protons to 0.3 dpa at nominal temperatures from 270 °C to 500 °C. Microstructural changes were observed by transmission electron microscopy (TEM). The results showed that evolution of dislocation loops depends on the Cr content. Below 300 °C, large ½ a0 <111> loops are dominating. Above 300 °C, a0 <100> loops with a habit plane {100} appear. Loop sizes of both types are more or less the same. At temperatures from 310 °C to 400 °C, a0 <100> loops form clusters with the same {100} habit plane as the one of the loops forming them. This indicates that <100> loops of the same variant start gliding under mutual elastic interaction. At 500 °C, dislocation loops form disc shaped clusters about 1000 nm in diameter and sitting on {111} and/or {100} planes in the pure Fe samples. Based on these observations a quantitative analysis of the dislocation loops configurations and their temperature dependence is made, leading to an understanding of the basic mechanisms of formation of these loops.

  6. Effects of Tube Processing on the Fatigue Life of Nitinol

    NASA Astrophysics Data System (ADS)

    Adler, Paul; Frei, Rudolf; Kimiecik, Michael; Briant, Paul; James, Brad; Liu, Chuan

    2018-03-01

    Nitinol tubes were manufactured from Standard Grade VIM-VAR ingots using Tube Manufacturing method "TM-1." Diamond-shaped samples were laser cut, shape set, then fatigued at 37 °C to 107 cycles. The 50, 5, and 1% probabilities of fracture were calculated as a function of number of cycles to fracture and compared with probabilities determined for fatigue data published by Robertson et al. (J Mech Behav Biomater 51:119-131, 2015). Robertson tested similar diamonds made from the same standard grade of Nitinol as in the current study, two other standard grades of Nitinol, and two high-purity grades of Nitinol expressly designed to improve fatigue life. Robertson's tubes were manufactured using Tube Manufacturing method "TM-2." Fatigue performance of TM-1 and TM-2 diamonds were compared: At 107 cycles, strain amplitudes corresponding to the three probabilities of fracture of the TM-1 diamonds were 2-3 times those of the TM-2 diamonds made from the same grade of Nitinol, and comparable to TM-2 diamonds made from the higher-purity materials. This difference is likely a result of the differences in tube manufacturing techniques and effects on resulting microstructures. Microstructural analyses of samples revealed a correlation between the median probability of fracture and median inclusion diameter that follows an inverse power-law function of the form y ≈ x -1.

  7. 7 CFR 201.68 - Eligibility requirements for certification of varieties.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ...) Evidence supporting the identity of the variety, such as comparative yield data, insect and disease... genetic purity. (i) A sample of seed representative of the variety as marketed. [38 FR 25662, Sept. 14...

  8. 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

  9. 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.

  10. 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.

  11. 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.

  12. The Top-of-Instrument corrections for nuclei with AMS on the Space Station

    NASA Astrophysics Data System (ADS)

    Ferris, N. G.; Heil, M.

    2018-05-01

    The Alpha Magnetic Spectrometer (AMS) is a large acceptance, high precision magnetic spectrometer on the International Space Station (ISS). The top-of-instrument correction for nuclei flux measurements with AMS accounts for backgrounds due to the fragmentation of nuclei with higher charge. Upon entry in the detector, nuclei may interact with AMS materials and split into fragments of lower charge based on their cross-section. The redundancy of charge measurements along the particle trajectory with AMS allows for the determination of inelastic interactions and for the selection of high purity nuclei samples with small uncertainties. The top-of-instrument corrections for nuclei with 2 < Z ≤ 6 are presented.

  13. Acoustic levitation: recent developments and emerging opportunities in biomaterials research.

    PubMed

    Weber, Richard J K; Benmore, Chris J; Tumber, Sonia K; Tailor, Amit N; Rey, Charles A; Taylor, Lynne S; Byrn, Stephen R

    2012-04-01

    Containerless sample environments (levitation) are useful for study of nucleation, supercooling, and vitrification and for synthesis of new materials, often with non-equilibrium structures. Elimination of extrinsic nucleation by container walls extends access to supercooled and supersaturated liquids under high-purity conditions. Acoustic levitation is well suited to the study of liquids including aqueous solutions, organics, soft materials, polymers, and pharmaceuticals at around room temperature. This article briefly reviews recent developments and applications of acoustic levitation in materials R&D. Examples of experiments yielding amorphous pharmaceutical materials are presented. The implementation and results of experiments on supercooled and supersaturated liquids using an acoustic levitator at a high-energy X-ray beamline are described.

  14. XPS Investigation on Changes in UO 2 Speciation following Exposure to Humidity

    DOE PAGES

    Donald, Scott B.; Davisson, M. Lee; Nelson, Art J.

    2016-04-27

    High purity UO 2powder samples were subjected to accelerated aging under controlled conditions with relative humidity ranging from 34% to 98%. Characterization of the chemical speciation of the products was accomplished using X-ray photoelectron spectroscopy (XPS). A shift to higher uranium oxidation states was found to be directly correlated to increased relative humidity exposure. In addition, the relative abundance of O 2-, OH -, and H 2O was found to vary with exposure time. Therefore, it is expected that uranium oxide materials exposed to high relative humidity conditions during processing and storage would display a similar increase in average uraniummore » valence.« less

  15. Identifying and quantifying short-lived fission products from thermal fission of HEU using portable HPGe detectors

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

    Pierson, Bruce D.; Finn, Erin C.; Friese, Judah I.

    2013-03-01

    Due to the emerging potential for trafficking of special nuclear material, research programs are investigating current capabilities of commercially available portable gamma ray detection systems. Presented in this paper are the results of three different portable high-purity germanium (HPGe) detectors used to identify short-lived fission products generated from thermal neutron interrogation of small samples of highly enriched uranium. Samples were irradiated at the Washington State University (WSU) Nuclear Radiation Center’s 1MW TRIGA reactor. The three portable, HPGe detectors used were the ORTEC MicroDetective, the ORTEC Detective, and the Canberra Falcon. Canberra’s GENIE-2000 software was used to analyze the spectral datamore » collected from each detector. Ultimately, these three portable detectors were able to identify a large range of fission products showing potential for material discrimination.« less

  16. Comparative study of organosolv lignin extracted from prairie cordgrass, switchgrass and corn stover.

    PubMed

    Cybulska, Iwona; Brudecki, Grzegorz; Rosentrater, Kurt; Julson, James L; Lei, Hanwu

    2012-08-01

    Lignin extracted from prairie cordgrass, switchgrass, and corn stover (using ethyl acetate-ethanol-water organosolv pretreatment) was analyzed and characterized using several methods. These methods included analysis of purity (by determination of Klason lignin, carbohydrate, and ash contents), solubility (with several organic solvents), phenolic group analysis (ultraviolet ionization difference spectra, and nitrobenzene oxidation), and general functional group analysis (by (1)H NMR). Results showed that all the examined lignin samples were relatively pure (contained over 50% Klason lignin, less than 5% carbohydrate contamination, and less than 3% ash), but switchgrass-derived lignin was observed to be the purest. All the lignins were found to contain high amounts of phenolic groups, while switchgrass-derived lignin was the most phenolic, according to the ionization difference spectra. Nitrobenzene oxidation revealed that all the lignin samples contained available guaiacyl units in high amounts. Copyright © 2012 Elsevier Ltd. All rights reserved.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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

  2. 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.

  3. 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.

  4. 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.

  5. 7 CFR 160.202 - Fees generally for laboratory analysis and testing.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

  6. 7 CFR 160.202 - Fees generally for laboratory analysis and testing.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

  7. 7 CFR 160.202 - Fees generally for laboratory analysis and testing.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

  8. 7 CFR 160.202 - Fees generally for laboratory analysis and testing.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

  9. 7 CFR 160.202 - Fees generally for laboratory analysis and testing.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... turpentine. (See Note 3). (1) Comprehensive analysis to determine purity, specification compliance, or other... related to quality of utility. (i) Single Sample: (A) Rosin—$14.00. (B) Turpentine—$10.00. (ii) Two or more samples tested at same time: (A) Rosin—per sample—$10.00. (B) Turpentine—per sample—$8.00. Note 3...

  10. NIST-Traceable NMR Method to Determine Quantitative Weight Percentage Purity of Nitrogen Mustard HN-3 Feedstock Samples

    DTIC Science & Technology

    2013-08-01

    products . This report may not be cited for purposes of advertisement. This report has been approved for public release. Acknowledgments The...such as 0.01% ethylbenzene in deuterated acetone can be analyzed to check the signal response. The analysis of this sample can be done periodically as

  11. Impact of South American heroin on the US heroin market 1993–2004

    PubMed Central

    Ciccarone, Daniel; Unick, George J; Kraus, Allison

    2008-01-01

    Background The past two decades have seen an increase in heroin-related morbidity and mortality in the United States. We report on trends in US heroin retail price and purity, including the effect of entry of Colombian-sourced heroin on the US heroin market. Methods The average standardized price ($/mg-pure) and purity (% by weight) of heroin from 1993 to 2004 was from obtained from US Drug Enforcement Agency retail purchase data for 20 metropolitan statistical areas. Univariate statistics, robust Ordinary Least Squares regression and mixed fixed and random effect growth curve models were used to predict the price and purity data in each metropolitan statistical area over time. Results Over the 12 study years, heroin price decreased 62%. The median percentage of all heroin samples that are of South American origin increased an absolute 7% per year. Multivariate models suggest percent South American heroin is a significant predictor of lower heroin price and higher purity adjusting for time and demographics. Conclusion These analyses reveal trends to historically low-cost heroin in many US cities. These changes correspond to the entrance into and rapid domination of the US heroin market by Colombian-sourced heroin. The implications of these changes are discussed. PMID:19201184

  12. Use and qualification of primary and secondary standards employed in quantitative ¹H NMR spectroscopy of pharmaceuticals.

    PubMed

    Rundlöf, Torgny; McEwen, Ian; Johansson, Monika; Arvidsson, Torbjörn

    2014-05-01

    Standards are required in quantitative NMR (qNMR) to obtain accurate and precise results. In this study acetanilide was established and used as a primary standard. Six other chemicals were selected as secondary standards: 3,4,5-trichloropyridine, dimethylterephthalate, maleic acid, 3-sulfolene, 1,4-bis(trimethylsilyl)benzene, and 1,3,5-trimethoxybenzene. The secondary standards were quantified using the primary standard acetanilide. A protocol for qualification and periodic checks of these secondary standards was developed, and used for evaluation of the stability of the compounds. Periodic monitoring of purity was performed for several years. The purity was higher than 99% for all secondary standards. All standards maintained the initial purity during the time period of monitoring, with very small variations in purity (0.3-0.4%). The selected secondary standards were shown to be suitable qNMR standards and that periodic requalification of the standards by qNMR ensures reliable analytical results. These standards have been used in our laboratory for compliance testing of pharmaceutical active substances and approved medicinal products as well as for analysis of suspected illegal medicines. In total more than 1000 samples have been tested using both internal and external standardization and examples are given. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. 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.

  14. 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.

  15. Purity and Cleanness of Aeorgel as a Cosmic Dust Capture Medium

    NASA Technical Reports Server (NTRS)

    Tsou, P.; Fleming, R.; Lindley, P.; Craig, A.; Blake, D.

    1994-01-01

    The capability for capturing micrometeoroids intact through laboratory simulations [Tsou 1988] and in space [Tsou 1993] in passive underdense silica aerogel offers a valuable tool for cosmic dust research. The integrity of the sample handling medium can substantially modify the integrity of the sample. Intact capture is a violent hypervelocity event: the integrity of the capturing medium can cause even greater modification of the sample.

  16. Rapid purification of diastereoisomers from Piper kadsura using supercritical fluid chromatography with chiral stationary phases.

    PubMed

    Xin, Huaxia; Dai, Zhuoshun; Cai, Jianfeng; Ke, Yanxiong; Shi, Hui; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-08-04

    Supercritical fluid chromatography (SFC) with chiral stationary phases (CSPs) is an advanced solution for the separation of achiral compounds in Piper kadsura. Analogues and stereoisomers are abundant in natural products, but there are obstacles in separation using conventional method. In this paper, four lignan diastereoisomers, (-)-Galbelgin, (-)-Ganschisandrin, Galgravin and (-)-Veraguensin, from Piper kadsura were separated and purified by chiral SFC. Purification strategy was designed, considering of the compound enrichment, sample purity and purification throughput. Two-step achiral purification method on chiral preparative columns with stacked automated injections was developed. Unconventional mobile phase modifier dichloromethane (DCM) was applied to improve the sample solubility. Four diastereoisomers was prepared at the respective weight of 103.1mg, 10.0mg, 152.3mg and 178.6mg from 710mg extract with the purity of greater than 98%. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Automated centrifugal-microfluidic platform for DNA purification using laser burst valve and coriolis effect.

    PubMed

    Choi, Min-Seong; Yoo, Jae-Chern

    2015-04-01

    We report a fully automated DNA purification platform with a micropored membrane in the channel utilizing centrifugal microfluidics on a lab-on-a-disc (LOD). The microfluidic flow in the LOD, into which the reagents are injected for DNA purification, is controlled by a single motor and laser burst valve. The sample and reagents pass successively through the micropored membrane in the channel when each laser burst valve is opened. The Coriolis effect is used by rotating the LOD bi-directionally to increase the purity of the DNA, thereby preventing the mixing of the waste and elution solutions. The total process from the lysed sample injection into the LOD to obtaining the purified DNA was finished within 7 min with only one manual step. The experimental result for Salmonella shows that the proposed microfluidic platform is comparable to the existing devices in terms of the purity and yield of DNA.

  18. Luminescence (IRSL) dating of Yeni Rabat church in Artvin, Turkey

    NASA Astrophysics Data System (ADS)

    Şahiner, Eren; Meriç, Niyazi; Uygun, Selda

    2013-05-01

    Luminescence dating is a chronological method that has been used extensively in terrestrial materials. In this study, we present Infrared Stimulated Luminescence (IRSL) dating results obtained for sediment and pottery samples taken from Yeni Rabat Church, Ardanuç, Artvin, Turkey. For this purpose, equivalent dose (ED) and annual dose rate (AD) of samples were measured. For annual dose rate, concentrations of radioactive isotopes (U, Th, K) were determined by using a high-purity germanium detector. For the equivalent dose, polymineral fine grain SAR (Single Aliquot Regenerative Dose) and MAAD (Multiple Aliquot Additive Dose) procedures were used. The optimal preheat temperature was determined for sediment and pottery samples. Ages were calculated by Aitken's luminescence age calculation method, which found 710±190 years for the pottery sample and 1450±370 years, 1390±420 years, 1430±310 years, 2210±520 years and 1640±390 years for different sediment samples, respectively. These estimated age ranges support the theory that Yeni Rabat Church could have been constructed in medieval times.

  19. The deuterium depth profile in neutron-irradiated tungsten exposed to plasma

    NASA Astrophysics Data System (ADS)

    Shimada, Masashi; Cao, G.; Hatano, Y.; Oda, T.; Oya, Y.; Hara, M.; Calderoni, P.

    2011-12-01

    Tungsten samples (99.99% purity from A.L.M.T. Corp., 6 mm in diameter, 0.2 mm in thickness) were irradiated by high-flux neutrons at 50 °C to 0.025 dpa in the High Flux Isotope Reactor at Oak Ridge National Laboratory. Subsequently, the neutron-irradiated tungsten samples were exposed to high-flux deuterium plasmas (ion flux: 1021-1022 m-2 s-1, ion fluence: 1025-1026 m-2) in the Tritium Plasma Experiment at Idaho National Laboratory. This paper reports the results of deuterium depth profiling in neutron-irradiated tungsten exposed to plasmas at 100, 200 and 500 °C via nuclear reaction analysis (NRA). The NRA measurements show that a significant amount of deuterium (>0.1 at.% D/W) remains trapped in the bulk material (up to 5 μm) at 500 °C. Tritium Migration Analysis Program simulation results using the NRA profiles indicate that different trapping mechanisms exist for neutron-irradiated and unirradiated tungsten.

  20. Determinants of heroin retail prices in metropolitan France: Discounts, purity and local markets.

    PubMed

    Lahaie, Emmanuel; Janssen, Eric; Cadet-Taïrou, Agnès

    2016-09-01

    Field studies have indicated a recent increase in heroin availability and use in France, and yet very little is known about the mechanisms underlying heroin retail prices. This paper offers a first attempt at identifying the determinants of heroin pricing, to measure quantity discounts and assess the influence of purity on street prices, while controlling for a geographical effect. Data on heroin samples were collected during 2011 in seven urban areas of metropolitan France. Ordinary least squares regression was used to model the associations between price, quantity, purity and other independent variables. Quantity remains the most influential variable on heroin pricing. We estimate that a 10% increase in the size of a transaction leads to a 2.3% decrease in the unit price. Assessed purity proved to be significant, although in modest proportion. Sociodemographic characteristics, such as gender, users' experience and relationships with dealers, proved to be insignificant. Heroin retail prices vary according to a geographical gradient related to the routes of entry and distribution. As a credence good, heroin retail prices in France are affected by more than simply the traditional supply and demand relationship. The results of this study also underline the limitations of a quantitative framework and should be complemented by further ethnographic research to obtain an in-depth understanding of local markets. Policies should be designed to better take local disparities into account.[Lahaie E, Janssen E, Cadet-Taïrou A. Determinants of heroin retail prices in metropolitan France:Discounts, purity and local markets. Drug Alcohol Rev 2016;35:597-604]. © 2015 Australasian Professional Society on Alcohol and other Drugs.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. Laser-Induced Breakdown Spectroscopy Based Protein Assay for Cereal Samples.

    PubMed

    Sezer, Banu; Bilge, Gonca; Boyaci, Ismail Hakki

    2016-12-14

    Protein content is an important quality parameter in terms of price, nutritional value, and labeling of various cereal samples. However, conventional analysis methods, namely, Kjeldahl and Dumas, have major drawbacks such as long analysis time, titration mistakes, and carrier gas dependence with high purity. For this reason, there is an urgent need for rapid, reliable, and environmentally friendly technologies for protein analysis. The present study aims to develop a new method for protein analysis in wheat flour and whole meal by using laser-induced breakdown spectroscopy (LIBS), which is a multielemental, fast, and simple spectroscopic method. Unlike the Kjeldahl and Dumas methods, it has potential to analyze a high number of samples in considerably short time. In the study, nitrogen peaks in LIBS spectra of wheat flour and whole meal samples with different protein contents were correlated with results of the standard Dumas method with the aid of chemometric methods. A calibration graph showed good linearity with the protein content between 7.9 and 20.9% and a 0.992 coefficient of determination (R 2 ). The limit of detection was calculated as 0.26%. The results indicated that LIBS is a promising and reliable method with its high sensitivity for routine protein analysis in wheat flour and whole meal samples.

  6. Oxidation and Hydration of U 3O 8 Materials Following Controlled Exposure to Temperature and Humidity

    DOE PAGES

    Tamasi, Alison L.; Boland, Kevin S.; Czerwinski, Kenneth; ...

    2015-03-18

    Chemical signatures correlated with uranium oxide processing are of interest to forensic science for inferring sample provenance. Identification of temporal changes in chemical structures of process uranium materials as a function of controlled temperatures and relative humidities may provide additional information regarding sample history. In our study, a high-purity α-U 3O 8 sample and three other uranium oxide samples synthesized from reaction routes used in nuclear conversion processes were stored under controlled conditions over 2–3.5 years, and powder X-ray diffraction analysis and X-ray absorption spectroscopy were employed to characterize chemical speciation. We measured signatures from the α-U 3O 8 samplemore » indicated that the material oxidized and hydrated after storage under high humidity conditions over time. Impurities, such as uranyl fluoride or schoepites, were initially detectable in the other uranium oxide samples. After storage under controlled conditions, the analyses of the samples revealed oxidation over time, although the signature of the uranyl fluoride impurity diminished. The presence of schoepite phases in older uranium oxide material is likely indicative of storage under high humidity and should be taken into account for assessing sample history. Finally, the absence of a signature from a chemical impurity, such as uranyl fluoride hydrate, in an older material may not preclude its presence at the initial time of production.« less

  7. Oxidation and Hydration of U 3 O 8 Materials Following Controlled Exposure to Temperature and Humidity

    DOE PAGES

    Tamasi, Alison L.; Boland, Kevin S.; Czerwinski, Kenneth; ...

    2015-03-18

    Chemical signatures correlated with uranium oxide processing are of interest to forensic science for inferring sample provenance. Identification of temporal changes in chemical structures of process uranium materials as a function of controlled temperatures and relative humidities may provide additional information regarding sample history. In our study, a high-purity α-U 3O 8 sample and three other uranium oxide samples synthesized from reaction routes used in nuclear conversion processes were stored under controlled conditions over 2–3.5 years, and powder X-ray diffraction analysis and X-ray absorption spectroscopy were employed to characterize chemical speciation. We measured signatures from the α-U 3O 8 samplemore » indicated that the material oxidized and hydrated after storage under high humidity conditions over time. Impurities, such as uranyl fluoride or schoepites, were initially detectable in the other uranium oxide samples. After storage under controlled conditions, the analyses of the samples revealed oxidation over time, although the signature of the uranyl fluoride impurity diminished. The presence of schoepite phases in older uranium oxide material is likely indicative of storage under high humidity and should be taken into account for assessing sample history. Finally, the absence of a signature from a chemical impurity, such as uranyl fluoride hydrate, in an older material may not preclude its presence at the initial time of production. LA-UR-15-21495.« less

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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

  15. 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.

  16. Twin related domains in 3D microstructures of conventionally processed and grain boundary engineered materials

    DOE PAGES

    Lind, Jonathan; Li, Shiu Fai; Kumar, Mukul

    2016-05-20

    The concept of twin-limited microstructures has been explored in the literature as a crystallographically constrained grain boundary network connected via only coincident site lattice (CSL) boundaries. The advent of orientation imaging has made classification of twin-related domains (TRD) or any other orientation cluster experimentally accessible in 2D using EBSD. With the emergence of 3D orientation mapping, a comparison of TRDs in measured 3D microstructures is performed in this paper and compared against their 2D counterparts. The TRD analysis is performed on a conventionally processed (CP) and a grain boundary engineered (EM) high purity copper sample that have been subjected tomore » successive anneal procedures to promote grain growth. Finally, the EM sample shows extremely large TRDs which begin to approach that of a twin-limited microstructure, while the TRDs in the CP sample remain relatively small and remote.« less

  17. Microstructure and thermal characterization of dense bone and metals for biomedical use

    NASA Astrophysics Data System (ADS)

    Rodríguez, G. Peña; Calderón, A.; Hernández, R. A. Muñoz; Orea, A. Cruz; Méndez, M.; Sinencio, F. Sánchez

    2000-10-01

    We present a microstructural study and thermal diffusivity measurements at room temperature in two different sections of bull dense bone, bull bone and commercial hydroxyapatite, the last two in powder form. A comparison was realised between these measured values and those obtained from metallic samples frequently used in implants, as high purity titanium and 316L stainless steel. Our results show that the porosity and its orientation in the bone are two important factors for the heat flux through the bone. On the other hand, we obtained that the hydroxyapatite, in compact powder form, presents a thermal diffusivity value close to those obtained for the samples of bone which gives a good thermal agreement between these materials. Finally, it was obtained at one order of magnitude difference between the thermal diffusivity values of metallic samples and those corresponding values to bone and hydroxyapatite being this difference greater in titanium than in stainless steel.

  18. Effects of excess oxygen on the 4.5-6.3 eV absorption spectra of oxygen-rich high purity silica

    NASA Astrophysics Data System (ADS)

    Magruder, R. H.; Robinson, S. J.

    2016-05-01

    Type III silica samples were implanted with O using a multi-energy process that produced a layer of constant concentration to within ±5% beginning ∼80 nm from the surface and extending to ∼640 nm below the surfaces of the samples. The concentrations of excess oxygen in the layer ranged from 0.035 to ∼2.1at.%. In these samples we show that E‧ centers and NBOHCs, as well as the normal cadre of ODC (II) centers, were suppressed, and the optical absorption from 4.7 to 6.4 eV was primarily due to oxygen excess defects. Using Gaussian fitting techniques to examine the optical difference spectra, we have been able to identify four defect centers that are related to excess oxygen defect bands at 4.76 eV, 5.42 eV, 5.75 eV and 6.25 eV.

  19. 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.

  20. 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

  1. A novel method for the elaboration of hydroxyapatite with high purity by sol-gel using the albumin and comparison with the classical methods

    NASA Astrophysics Data System (ADS)

    Mohammed, Eddya; Bouazza, Tbib; Khalil, El-Hami

    2018-02-01

    In this paper, we report the first synthesis of hydroxyapatite (Hap) by sol-gel using the albumin (egg white) compared with the four classical elaboration methods such as co-precipitation, solid state, and solid-liquid samples of hydroxyapatite. We use a reference sample of hydroxyapatite bought from Fluka Chemika company (Lot and Filling code 385330/1 14599). All samples are characterized by X-ray diffraction (XRD), Uv-visible spectroscopy (Uv-Vis), and Fourier transforms infrared spectroscopy (FT-IR). The XRD study showed the existence of a Hexagonal phase for all our samples prepared in our laboratory and an orthorhombic phase for the Fulka Chemika sample of Hap (Lot and Filling code 385330/1 14599). The study by Uv-visible spectroscopy was performed to determine and compare the optical gap and the disorder of each sample of Hap. The FT-IR spectroscopy demonstrated that all our Hap samples had a similar mode of vibration of the chemical bonds (OH-) and (PO4)3-.

  2. Determination of radioactivity levels and heavy metal concentrations in seawater, sediment and anchovy (Engraulis encrasicolus) from the Black Sea in Rize, Turkey.

    PubMed

    Baltas, Hasan; Kiris, Erkan; Sirin, Murat

    2017-03-15

    Seawater, sediment and fish (anchovy) samples consumed in the Rize province of the Eastern Black Sea region of Turkey were collected from five different stations. The radioactivity levels ( 226 Ra, 232 Th, 40 K and 137 Cs) were determined in all the samples using a high-purity germanium detector. While 226 Ra, 232 Th and 40 K radionuclides were detected in all samples, the radionuclide concentration of 137 Cs, except for the sediment samples (mean activity is 9±1.4Bqkg -1 ), was not detected for the seawater and fish samples. The total annual effective dose rates from the ingestion of these radionuclides for fish were calculated using the measured activity concentrations in radionuclides and their ingested dose conversion factor. Also, the concentrations of some heavy metals in all the samples were determined. The activity and heavy metal concentration values that were determined for the seawater, sediment and fish samples were compared among the locations themselves and with literature values. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Natural radionuclide and radiological assessment of building materials in high background radiation areas of Ramsar, Iran.

    PubMed

    Bavarnegin, Elham; Moghaddam, Masoud Vahabi; Fathabadi, Nasrin

    2013-04-01

    Building materials, collected from different sites in Ramsar, a northern coastal city in Iran, were analyzed for their natural radionuclide contents. The measurements were carried out using a high resolution high purity Germanium (HPGe) gamma-ray spectrometer system. The activity concentration of (226)Ra, (232)Th, and (40)K content varied from below the minimum detection limit up to 86,400 Bqkg(-1), 187 Bqkg(-1), and 1350 Bqkg(-1), respectively. The radiological hazards incurred from the use of these building materials were estimated through various radiation hazard indices. The result of this survey shows that values obtained for some samples are more than the internationally accepted maximum limits and as such, the use of them as a building material pose significant radiation hazard to individuals.

  4. 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.

  5. Micro-quantity tissue digestion for metal measurements by use of a microwave acid-digestion bomb.

    PubMed

    Nicholson, J R; Savory, M G; Savory, J; Wills, M R

    1989-03-01

    We describe a simple and convenient method for processing small amounts of tissue samples for trace-metal measurements by atomic absorption spectrometry, by use of a modified Parr microwave digestion bomb. Digestion proceeds rapidly (less than or equal to 90 s) in a sealed Teflon-lined vessel that eliminates contamination or loss from volatilization. Small quantities of tissue (5-100 mg dry weight) are digested in high-purity nitric acid, yielding concentrations of analyte that can be measured directly without further sample manipulation. We analyzed National Institute of Standards and Technology bovine liver Standard Reference Material to verify the accuracy of the technique. We assessed the applicability of the technique to analysis for aluminum in bone by comparison with a dry ashing procedure.

  6. Effects of grain size on the corrosion resistance of pure magnesium by cooling rate-controlled solidification

    NASA Astrophysics Data System (ADS)

    Liu, Yichi; Liu, Debao; You, Chen; Chen, Minfang

    2015-09-01

    The aim of this study was to investigate the effect of grain size on the corrosion resistance of pure magnesium developed for biomedical applications. High-purity magnesium samples with different grain size were prepared by the cooling rate-controlled solidification. Electrochemical and immersion tests were employed to measure the corrosion resistance of pure magnesium with different grain size. The electrochemical polarization curves indicated that the corrosion susceptibility increased as the grain size decrease. However, the electrochemical impedance spectroscopy (EIS) and immersion tests indicated that the corrosion resistance of pure magnesium is improved as the grain size decreases. The improvement in the corrosion resistance is attributed to refine grain can produce more uniform and density film on the surface of sample.

  7. Preparative SDS PAGE as an Alternative to His-Tag Purification of Recombinant Amelogenin

    PubMed Central

    Gabe, Claire M.; Brookes, Steven J.; Kirkham, Jennifer

    2017-01-01

    Recombinant protein technology provides an invaluable source of proteins for use in structure-function studies, as immunogens, and in the development of therapeutics. Recombinant proteins are typically engineered with “tags” that allow the protein to be purified from crude host cell extracts using affinity based chromatography techniques. Amelogenin is the principal component of the developing enamel matrix and a frequent focus for biomineralization researchers. Several groups have reported the successful production of recombinant amelogenins but the production of recombinant amelogenin free of any tags, and at single band purity on silver stained SDS PAGE is technically challenging. This is important, as rigorous structure-function research frequently demands a high degree of protein purity and fidelity of protein sequence. Our aim was to generate His-tagged recombinant amelogenin at single band purity on silver stained SDS PAGE for use in functionality studies after His-tag cleavage. An acetic acid extraction technique (previously reported to produce recombinant amelogenin at 95% purity directly from E. coli) followed by repeated rounds of nickel column affinity chromatography, failed to generate recombinant amelogenin at single band purity. This was because following an initial round of nickel column affinity chromatography, subsequent cleavage of the His-tag was not 100% efficient. A second round of nickel column affinity chromatography, used in attempts to separate the cleaved His-tag free recombinant from uncleaved His-tagged contaminants, was still unsatisfactory as cleaved recombinant amelogenin exhibited significant affinity for the nickel column. To solve this problem, we used preparative SDS PAGE to successfully purify cleaved recombinant amelogenins to single band purity on silver stained SDS PAGE. The resolving power of preparative SDS PAGE was such that His-tag based purification of recombinant amelogenin becomes redundant. We suggest that acetic acid extraction of recombinant amelogenin and subsequent purification using preparative SDS PAGE provides a simple route to highly purified His-tag free amelogenin for use in structure-function experiments and beyond. PMID:28670287

  8. Factors influencing the purity of electronic grade phosphine delivered to MOCVD tools

    NASA Astrophysics Data System (ADS)

    Feng, Jun; Owens, Mitch; Raynor, Mark W.

    2010-04-01

    Increasing mobility of InP films with usage time of one PH 3 cylinder prompted an investigation into factors influencing the purity of delivered PH 3. The presence of hygroscopic H xPO y residues in a delivery system greatly increases the dry-down time compared to that of a clean system. Static delivery system tests show increasing H 2O concentration with time and twice the increase in PH 3 versus N 2 over 48 h indicating reaction of metal oxides in components with PH 3 to generate H 2O. Gas purity may also vary during cylinder usage. Depletion of a high-purity PH 3 cylinder shows consistently low gas phase H 2O levels before phase-break but increasing levels after phase-break, as the cylinder depressurizes. The results highlight the importance of using pure PH 3, employing rigorous cycle-purging procedures to prevent H xPO y contamination, switching out cylinders in good time and using purification technology to control H 2O.

  9. 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).

  10. Membrane-integrated fermentation system for improving the optical purity of D-lactic acid produced during continuous fermentation.

    PubMed

    Sawai, Hideki; Na, Kyungsu; Sasaki, Nanami; Mimitsuka, Takashi; Minegishi, Shin-ichi; Henmi, Masahiro; Yamada, Katsushige; Shimizu, Sakayu; Yonehara, Tetsu

    2011-01-01

    This report describes the production of highly optically pure D-lactic acid by the continuous fermentation of Sporolactobacillus laevolacticus and S. inulinus, using a membrane-integrated fermentation (MFR) system. The optical purity of D-lactic acid produced by the continuous fermentation system was greater than that produced by batch fermentation; the maximum value for the optical purity of D-lactic acid reached 99.8% enantiomeric excess by continuous fermentation when S. leavolacticus was used. The volumetric productivity of the optically pure D-lactic acid was about 12 g/L/h, this being approximately 11-fold higher than that obtained by batch fermentation. An enzymatic analysis indicated that both S. laevolacticus and S. inulinus could convert L-lactic acid to D-lactic acid by isomerization after the late-log phase. These results provide evidence for an effective bio-process to produce D-lactic acid of greater optical purity than has conventionally been achieved to date.

  11. High-purity and label-free isolation of circulating tumor cells (CTCs) in a microfluidic platform by using optically-induced-dielectrophoretic (ODEP) force.

    PubMed

    Huang, Song-Bin; Wu, Min-Hsien; Lin, Yen-Heng; Hsieh, Chia-Hsun; Yang, Chih-Liang; Lin, Hung-Chih; Tseng, Ching-Ping; Lee, Gwo-Bin

    2013-04-07

    Negative selection-based circulating tumor cell (CTC) isolation is believed valuable to harvest more native, and in particular all possible CTCs without biases relevant to the properties of surface antigens on the CTCs. Under such a cell isolation strategy, however, the CTC purity is normally compromised. To address this issue, this study reports the integration of optically-induced-dielectrophoretic (ODEP) force-based cell manipulation, and a laminar flow regime in a microfluidic platform for the isolation of untreated, and highly pure CTCs after conventional negative selection-based CTC isolation. In the design, six sections of moving light-bar screens were continuously and simultaneously exerted in two parallel laminar flows to concurrently separate the cancer cells from the leukocytes based on their size difference and electric properties. The separated cell populations were further partitioned, delivered, and collected through the two flows. With this approach, the cancer cells can be isolated in a continuous, effective, and efficient manner. In this study, the operating conditions of ODEP for the manipulation of prostate cancer (PC-3) and human oral cancer (OEC-M1) cells, and leukocytes with minor cell aggregation phenomenon were first characterized. Moreover, performances of the proposed method for the isolation of cancer cells were experimentally investigated. The results showed that the presented CTC isolation scheme was able to isolate PC-3 cells or OEC-M1 cells from a leukocyte background with high recovery rate (PC-3 cells: 76-83%, OEC-M1 cells: 61-68%), and high purity (PC-3 cells: 74-82%, OEC-M1 cells: 64-66%) (set flow rate: 0.1 μl min(-1) and sample volume: 1 μl). The latter is beyond what is currently possible in the conventional CTC isolations. Moreover, the viability of isolated cancer cells was evaluated to be as high as 94 ± 2%, and 95 ± 3% for the PC-3, and OEC-M1 cells, respectively. Furthermore, the isolated cancer cells were also shown to preserve their proliferative capability. As a whole, this study has presented an ODEP-based microfluidic platform that is capable of isolating CTCs in a continuous, label-free, cell-friendly, and particularly highly pure manner. All these traits are found particularly meaningful for exploiting the harvested CTCs for the subsequent cell-based, or biochemical assays.

  12. 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.

  13. Which Moral Foundations Predict Willingness to Make Lifestyle Changes to Avert Climate Change in the USA?

    PubMed Central

    Dickinson, Janis L.; McLeod, Poppy; Bloomfield, Robert; Allred, Shorna

    2016-01-01

    Jonathan Haidt’s Moral Foundations Theory identifies five moral axes that can influence human motivation to take action on vital problems like climate change. The theory focuses on five moral foundations, including compassion, fairness, purity, authority, and ingroup loyalty; these have been found to differ between liberals and conservatives as well as Democrats and Republicans. Here we show, based on the Cornell National Social Survey (USA), that valuations of compassion and fairness were strong, positive predictors of willingness to act on climate change, whereas purity had a non-significant tendency in the positive direction (p = 0.07). Ingroup loyalty and authority were not supported as important predictor variables using model selection (ΔAICc__). Compassion and fairness were more highly valued by liberals, whereas purity, authority, and in-group loyalty were more highly valued by conservatives. As in previous studies, participants who were younger, more liberal, and reported greater belief in climate change, also showed increased willingness to act on climate change. Our research supports the potential importance of moral foundations as drivers of intentions with respect to climate change action, and suggests that compassion, fairness, and to a lesser extent, purity, are potential moral pathways for personal action on climate change in the USA. PMID:27760207

  14. 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.

  15. A novel microfluidic platform for size and deformability based separation and the subsequent molecular characterization of viable circulating tumor cells.

    PubMed

    Hvichia, G E; Parveen, Z; Wagner, C; Janning, M; Quidde, J; Stein, A; Müller, V; Loges, S; Neves, R P L; Stoecklein, N H; Wikman, H; Riethdorf, S; Pantel, K; Gorges, T M

    2016-06-15

    Circulating tumor cells (CTCs) were introduced as biomarkers more than 10 years ago, but capture of viable CTCs at high purity from peripheral blood of cancer patients is still a major technical challenge. Here, we report a novel microfluidic platform designed for marker independent capture of CTCs. The Parsortix™ cell separation system provides size and deformability-based enrichment with automated staining for cell identification, and subsequent recovery (harvesting) of cells from the device. Using the Parsortix™ system, average cell capture inside the device ranged between 42% and 70%. Subsequent harvest of cells from the device ranged between 54% and 69% of cells captured. Most importantly, 99% of the isolated tumor cells were viable after processing in spiking experiments as well as after harvesting from patient samples and still functional for downstream molecular analysis as demonstrated by mRNA characterization and array-based comparative genomic hybridization. Analyzing clinical blood samples from metastatic (n = 20) and nonmetastatic (n = 6) cancer patients in parallel with CellSearch(®) system, we found that there was no statistically significant difference between the quantitative behavior of the two systems in this set of twenty six paired separations. In conclusion, the epitope independent Parsortix™ system enables the isolation of viable CTCs at a very high purity. Using this system, viable tumor cells are easily accessible and ready for molecular and functional analysis. The system's ability for enumeration and molecular characterization of EpCAM-negative CTCs will help to broaden research into the mechanisms of cancer as well as facilitating the use of CTCs as "liquid biopsies." © 2016 The Authors International Journal of Cancer published by John Wiley & Sons Ltd on behalf of UICC.

  16. 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.

  17. Crystals and tablets in the Spanish ecstasy market 2000-2014: Are they the same or different in terms of purity and adulteration?

    PubMed

    Vidal Giné, Claudio; Ventura Vilamala, Mireia; Fornís Espinosa, Iván; Gil Lladanosa, Cristina; Calzada Álvarez, Nú; Fitó Fruitós, Ariadna; Rodríguez Rodríguez, Joan; Domíngo Salvany, Antonia; de la Torre Fornell, Rafael

    2016-06-01

    Although 3,4-methylenedioxymethamphetamine (MDMA) has a long history in recreational settings, research on its composition (purity and adulteration) has focused only on tablets even though crystal format is readily available for users. Drug specimens collected between January 2000 and December 2014 were analyzed at Energy Control's facilities. All samples were voluntarily provided by drug users. Sample identification was made with thin layer chromatography and gas chromatography coupled to mass spectrometry, and quantification with ultraviolet spectrophotometry (only in unadulterated samples). Between January 2000 and December 2014, 6200 samples purchased as ecstasy by their users were analyzed. Crystals were the most frequent format (60.6%) followed by tablets (38.8%). During the study period, the proportion of samples containing only MDMA was higher in crystals than in tablets. Compared with tablets, adulterated crystal samples contained the same number of adulterants but more combinations of different substances. Although caffeine was commonly detected as adulterant both in crystals and tablets, other substances such as phenacetin, lidocaine, dextrometorphan or methamphetamine were detected almost exclusively in crystal samples. The amount of MDMA in crystal samples remained stable unlike tablets for which a huge increase in MDMA dose was observed since 2010. Crystal samples of ecstasy showed clear differences compared to ecstasy tablets and this must be taken into account both in research and harm reduction. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  18. 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.

  19. A solvent-extraction module for cyclotron production of high-purity technetium-99m.

    PubMed

    Martini, Petra; Boschi, Alessandra; Cicoria, Gianfranco; Uccelli, Licia; Pasquali, Micòl; Duatti, Adriano; Pupillo, Gaia; Marengo, Mario; Loriggiola, Massimo; Esposito, Juan

    2016-12-01

    The design and fabrication of a fully-automated, remotely controlled module for the extraction and purification of technetium-99m (Tc-99m), produced by proton bombardment of enriched Mo-100 molybdenum metallic targets in a low-energy medical cyclotron, is here described. After dissolution of the irradiated solid target in hydrogen peroxide, Tc-99m was obtained under the chemical form of 99m TcO 4 - , in high radionuclidic and radiochemical purity, by solvent extraction with methyl ethyl ketone (MEK). The extraction process was accomplished inside a glass column-shaped vial especially designed to allow for an easy automation of the whole procedure. Recovery yields were always >90% of the loaded activity. The final pertechnetate saline solution Na 99m TcO 4 , purified using the automated module here described, is within the Pharmacopoeia quality control parameters and is therefore a valid alternative to generator-produced 99m Tc. The resulting automated module is cost-effective and easily replicable for in-house production of high-purity Tc-99m by cyclotrons. Copyright © 2016 Elsevier Ltd. All rights reserved.

  20. 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.

  1. SABRE: Dark matter annual modulation detection in the northern and southern hemispheres

    NASA Astrophysics Data System (ADS)

    Tomei, C.

    2017-02-01

    SABRE (Sodium-iodide with Active Background REjection) is a new NaI(Tl) experiment designed to search for galactic Dark Matter through the annual modulation signature. SABRE will consist of highly pure NaI(Tl) crystals operated in an active liquid scintillator veto. The SABRE experiment will follow a two-phase approach. In the first phase, one high-purity NaI(Tl) crystal will be operated at LNGS in an active liquid scintillator veto with the goal of demonstrating backgrounds low enough for a sensitive test of the DAMA/LIBRA result. An unprecedented radio-purity for both the NaI powder and the crystal growth will be needed to achieve this goal. The second phase will consist in building two high-purity NaI(Tl) detector arrays, with a total mass of about 50 kg each, located at LNGS and in the Stawell Gold Mine in Australia. The operation of twin full-scale experiments in both the northern and the southern hemispheres will strengthen the reliability of the result against any possible seasonal systematic effect.

  2. Recovery of high-purity silver directly from dilute effluents by an emulsion liquid membrane-crystallization process.

    PubMed

    Tang, Bing; Yu, Guojun; Fang, Jianzhang; Shi, Taihong

    2010-05-15

    An emulsion liquid membrane (ELM)-crystallization process, using hypophosphorous acid as a reducing agent in the internal aqueous phase, has been developed for the purpose of recovering high-purity silver directly from dilute industrial effluents (waste rinse water). After pretreatment with HNO(3), silver in waste rinse water can be reliably recovered with high efficiency through the established process. The main parameters in the process of ELM-crystallization include the concentration of carrier in the membrane phase, the concentration of reducing agent in the internal aqueous phase, and the treatment ratio, which influence the recovery efficiency to various extents and must be controlled carefully. The results indicated that more than 99.5% (wt.) of the silver ions in the external aqueous phase were extracted by the ELM-crystallization process, with an average efficiency of recovery of 99.24% (wt.) and a purity of 99.92% (wt.). The membrane phase can be used repeatedly without loss of the efficiency of recovery. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  3. Standing wave design and experimental validation of a tandem simulated moving bed process for insulin purification.

    PubMed

    Xie, Yi; Mun, Sungyong; Kim, Jinhyun; Wang, Nien-Hwa Linda

    2002-01-01

    A tandem simulated moving bed (SMB) process for insulin purification has been proposed and validated experimentally. The mixture to be separated consists of insulin, high molecular weight proteins, and zinc chloride. A systematic approach based on the standing wave design, rate model simulations, and experiments was used to develop this multicomponent separation process. The standing wave design was applied to specify the SMB operating conditions of a lab-scale unit with 10 columns. The design was validated with rate model simulations prior to experiments. The experimental results show 99.9% purity and 99% yield, which closely agree with the model predictions and the standing wave design targets. The agreement proves that the standing wave design can ensure high purity and high yield for the tandem SMB process. Compared to a conventional batch SEC process, the tandem SMB has 10% higher yield, 400% higher throughput, and 72% lower eluant consumption. In contrast, a design that ignores the effects of mass transfer and nonideal flow cannot meet the purity requirement and gives less than 96% yield.

  4. Development of the protocol for purification of artemisinin based on combination of commercial and computationally designed adsorbents.

    PubMed

    Piletska, Elena V; Karim, Kal; Cutler, Malcolm; Piletsky, Sergey A

    2013-01-01

    A polymeric adsorbent for extraction of the antimalarial drug artemisinin from Artemisia annua L. was computationally designed. This polymer demonstrated a high capacity for artemisinin (120 mg g(-1) ), quantitative recovery (87%) and was found to be an effective material for purification of artemisinin from complex plant matrix. The artemisinin quantification was conducted using an optimised HPLC-MS protocol, which was characterised by high precision and linearity in the concentration range between 0.05 and 2 μg mL(-1) . Optimisation of the purification protocol also involved screening of commercial adsorbents for the removal of waxes and other interfering natural compounds, which inhibit the crystallisation of artemisinin. As a result of a two step-purification protocol crystals of artemisinin were obtained, and artemisinin purity was evaluated as 75%. By performing the second stage of purification twice, the purity of artemisinin can be further improved to 99%. The developed protocol produced high-purity artemisinin using only a few purification steps that makes it suitable for large scale industrial manufacturing process. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Catalyst evaluation for high-purity H2 production by sorption-enhanced steam-methane reforming coupled to a Ca/Cu process

    NASA Astrophysics Data System (ADS)

    Navarro, M. V.; López, J. M.; García, T.; Grasa, G.; Murillo, R.

    2017-09-01

    The operational limits of a commercial nickel-based catalyst under the conditions of a sorption-enhanced steam-methane reforming process coupled to a Ca/Cu chemical loop are investigated for high-purity H2 production in a cyclic operation. The performance of the reforming catalyst is tested by means of a high number of oxidation-reduction-reforming cycles. After 100 oxidation-reduction cycles, this catalyst retains its exceptional reforming activity. The methane conversion values are close to the thermodynamic equilibrium under very demanding conditions: temperature between 500 °C - 700 °C and mass hourly space velocity of 8.8 kgCH4 h-1 kgcat-1. After 200 cycles, the sample shows reduction in its reforming activity in line with a lower dispersion of the Ni species. Sintering of Ni nanocrystals is evidenced during the oxidation-reduction multi-cycles. The performance of the catalyst after 200 oxidation-reduction cycles mixed with a CaO-based CO2 sorbent is studied under optimal conditions calculated for the sorption-enhanced reforming process coupled to a Ca/Cu cycle (temperature of 650 °C, steam/methane ratio of 4, sorbent/catalyst ratio of 4 and space velocity of 0.75 kgCH4 h-1 kgcat-1). Remarkably, an equilibrium value over 92 vol.% H2 concentration is achieved, highlighting this catalyst as a promising candidate for the next steps of the process development.

  6. 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).

  7. On the accuracy of gamma spectrometric isotope ratio measurements of uranium

    NASA Astrophysics Data System (ADS)

    Ramebäck, H.; Lagerkvist, P.; Holmgren, S.; Jonsson, S.; Sandström, B.; Tovedal, A.; Vesterlund, A.; Vidmar, T.; Kastlander, J.

    2016-04-01

    The isotopic composition of uranium was measured using high resolution gamma spectrometry. Two acid solutions and two samples in the form of UO2 pellets were measured. The measurements were done in close geometries, i.e. directly on the endcap of the high purity germanium detector (HPGe). Applying no corrections for count losses due to true coincidence summing (TCS) resulted in up to about 40% deviation in the abundance of 235U from the results obtained with mass spectrometry. However, after correction for TCS, excellent agreement was achieved between the results obtained using two different measurement methods, or a certified value. Moreover, after corrections, the fitted relative response curves correlated excellently with simulated responses, for the different geometries, of the HPGe detector.

  8. Single step synthesis of high-purity CoO nanocrystals.

    PubMed

    Yang, Huaming; Ouyang, Jing; Tang, Aidong

    2007-07-19

    Both octahedral and slice-shaped cubic cobalt monoxide (CoO) nanocrystals with narrow size distributions have been successfully synthesized by a simple solvothermal route. It was found that conditions of the solvothermal treatment showed obvious effects on the formation and purity of the as-synthesized CoO nanocrystals, only when cobalt acetate was used as the cobalt source and when temperature reached 190 degrees C could CoO be produced; also, freeze-drying was necessary for obtaining pure CoO. Size of the CoO nanocrystals varied from 30 to 130 nm. Morphology of the products could be controlled by simply changing the type of surfactant in solvent, and the octahedral CoO nanocrystals showed rounded turns. Purity of the products was detected by intensive X-ray photoelectron spectroscopy (XPS) investigation and Fourier transform infrared spectroscopy (FTIR) combined with differential scanning calorimetry/thermal gravity (DSC/TG). The results indicated an absence of unexpected trivalence cobalt series on surface of the samples, thanks to the protection of the surface by trace amount of carbonate ions, adsorbed hydroxylation, and surfactant with a maximum thickness of 2 nm, which were proved by high-resolution transmission electron microscopy (HRTEM). The as-synthesized CoO nanoparticles were added into positive electrode of Ni/MH batteries, and discharge/charge cycling tests were performed under different rates from 0.1C to 5.0C. The results indicated that the specific capacities of batteries with addition of 5% octahedral or slice CoO nanocrystals at 0.1C were 393.3 and 318.1 mAh/g, respectively, which were higher than that without CoO (269.2mAh/g). Specific capacity of battery with addition of 5% octahedral CoO nanocrystals was 40% higher than that without CoO at 5.0C. Octahedral CoO nanocrystals show better electrochemical activity than slice CoO and indicate interesting potential in the field of electrochemical application.

  9. A Draft Test Protocol for Detecting Possible Biohazards in Martian Samples Returned to Earth

    NASA Technical Reports Server (NTRS)

    Rummel, John D. (Editor); Race, Margaret S.; DeVincenzi, Donald L.; Schad, P. Jackson; Stabekis, Pericles D.; Viso, Michel; Acevedo, Sara E.

    2002-01-01

    This document presents the first complete draft of a protocol for detecting possible biohazards in Mars samples returned to Earth: it is the final product of the Mars Sample Handling Protocol Workshop Series. convened in 2000-2001 by NASA's Planetary Protection Officer. The goal of the five-workshop Series vas to develop a comprehensive protocol by which returned martian sample materials could be assessed k r the presence of any biological hazard(s) while safeguarding the purity of the samples from possible terrestrial contamination.

  10. Dielectrophoretic focusing integrated pulsed laser activated cell sorting

    NASA Astrophysics Data System (ADS)

    Zhu, Xiongfeng; Kung, Yu-Chun; Wu, Ting-Hsiang; Teitell, Michael A.; Chiou, Pei-Yu

    2017-08-01

    We present a pulsed laser activated cell sorter (PLACS) integrated with novel sheathless size-independent dielectrophoretic (DEP) focusing. Microfluidic fluorescence activated cell sorting (μFACS) systems aim to provide a fully enclosed environment for sterile cell sorting and integration with upstream and downstream microfluidic modules. Among them, PLACS has shown a great potential in achieving comparable performance to commercial aerosol-based FACS (>90% purity at 25,000 cells sec-1). However conventional sheath flow focusing method suffers a severe sample dilution issue. Here we demonstrate a novel dielectrophoresis-integrated pulsed laser activated cell sorter (DEP-PLACS). It consists of a microfluidic channel with 3D electrodes laid out to provide a tunnel-shaped electric field profile along a 4cmlong channel for sheathlessly focusing microparticles/cells into a single stream in high-speed microfluidic flows. All focused particles pass through the fluorescence detection zone along the same streamline regardless of their sizes and types. Upon detection of target fluorescent particles, a nanosecond laser pulse is triggered and focused in a neighboring channel to generate a rapidly expanding cavitation bubble for precise sorting. DEP-PLACS has achieved a sorting purity of 91% for polystyrene beads at a throughput of 1,500 particle/sec.

  11. Glass dynamics and anomalous aging in a family of ionic liquids above the glass transition temperature.

    PubMed

    Shamim, Nabila; McKenna, Gregory B

    2010-12-09

    The present paper reports the results of a systematic rheological study of the dynamic moduli of 1-butyl 3-methylimidazolium tetrafluoroborate ([Bmim][BF(4)]), 1-butyl 3-methylimidazolium hexafluorophosphate ([Bmim][PF(6)]), and 1-ethyl 3-methylimidazolium ethylsulfate ([Emim][EtSO(4)]) in the vicinity of their respective glass transition temperatures. The results show an anomalous aging in that the dynamic and the low shear rate viscosities decrease with time at temperatures near to, but above, the glass transition temperature, and this is described. The samples that are aged into equilibrium obey the time-temperature superposition principle, and the shift factors and the viscosities follow classic super-Arrhenius behaviors with intermediate fragility values as the glass transition is approached. Similar experiments using a high-purity [Bmim][BF(4)] show that using a higher purity of the ionic liquid, while changing absolute values of the properties, does not eliminate the anomalous aging response. The data are also analyzed in a fashion similar to that used for polymer melts, and we find that these ionic liquids do not follow, for example, the Cox-Merz relationship between the steady shear viscosity and the dynamic viscosity.

  12. Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

    PubMed

    Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

    2015-06-01

    Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

  13. Comparison of Methods for the Extraction of DNA from Formalin-Fixed, Paraffin-Embedded Archival Tissues

    PubMed Central

    Sengüven, Burcu; Baris, Emre; Oygur, Tulin; Berktas, Mehmet

    2014-01-01

    Aim: Discussing a protocol involving xylene-ethanol deparaffinization on slides followed by a kit-based extraction that allows for the extraction of high quality DNA from FFPE tissues. Methods: DNA was extracted from the FFPE tissues of 16 randomly selected blocks. Methods involving deparaffinization on slides or tubes, enzyme digestion overnight or for 72 hours and isolation using phenol chloroform method or a silica-based commercial kit were compared in terms of yields, concentrations and the amplifiability. Results: The highest yield of DNA was produced from the samples that were deparaffinized on slides, digested for 72 hours and isolated with a commercial kit. Samples isolated with the phenol-chloroform method produced DNA of lower purity than the samples that were purified with kit. The samples isolated with the commercial kit resulted in better PCR amplification. Conclusion: Silica-based commercial kits and deparaffinized on slides should be considered for DNA extraction from FFPE. PMID:24688314

  14. 2016 NIST (133Xe) and Transfer (131mXe, 133mXe, 135Xe) Calibration Report

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

    Robinson, Troy A.

    A significantly improved calibration of the High Purity Germanium detectors used by the Idaho National Laboratory Noble Gas Laboratory was performed during the annual NIST calibration. New sample spacers provide reproducible and secure support of samples at distances of 4, 12, 24, 50 and 100 cm. Bean, 15mL and 50mL Schlenk tube geometries were calibrated. Also included in this year’s calibration was a correlation of detector dead-time with sample activity that can be used to predict the schedule of counting the samples at each distance for each geometry. This schedule prediction will help staff members set calendar reminders so thatmore » collection of calibration data at each geometry will not be missed. This report also correlates the counting efficiencies between detectors, so that if the counting efficiency on one detector is not known, it can be estimated from the same geometry on another detector.« less

  15. 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

  16. Large grain CBMM Nb ingot slices: An ideal test bed for exploring the microstructure-electromagnetic property relationships relevant to SRF

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

    Sung, Zu-Hawn, E-mail: ZSung@uss.com; Now at US-Steel, Pittsburgh, US; Lee, Peter J., E-mail: lee@asc.magnet.fsu.edu

    2015-12-04

    High purity (RRR > 200), large grain (> 5-10 cm) niobium ingot slices have been successfully used to fabricate radio frequency (RF) cavities for particle accelerators. They offer significantly reduced fabrication cost by eliminating processing steps and furthermore they provide the opportunity to study the influence of individual grain boundaries in SRF Nb. Here we summarize our measurements of grain boundary (GB) effects on the superconducting properties of large grain high purity niobium sheet manufactured by CBMM. We show by magneto-optical (MO) imaging that GBs allow premature flux penetration, but only when they are oriented close to the direction of themore » magnetic field. However, even low angle GBs produced by minor deformations commensurate with half-cell forming produce localized flux penetration. The transport properties of grain boundaries were investigated by direct transport across them and evidence for preferential vortex flow along the GBs of SRF Nb was observed for the first time. Using transmission electron microscopy (TEM) and micro crystallographic analysis with electron backscattered diffraction (EBSD), we were able to quantitatively characterize surface substructures that can lead to localized thermal breakdown of superconductivity. Important to these studies was the development of sample preparation techniques that made the cutout single, bi-crystal and tri-crystal Nb coupons as representative as possible of the surface properties of cavities manufactured by standard techniques.« less

  17. 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.

  18. Universal HPLC Detector for Hydrophilic Organic Compounds by Means of Total Organic Carbon Detection.

    PubMed

    Ohira, Shin-Ichi; Kaneda, Kyosuke; Matsuzaki, Toru; Mori, Shuta; Mori, Masanobu; Toda, Kei

    2018-06-05

    Most quantifications are achieved by comparison of the signals obtained with the sample to those from a standard. Thus, the purity and stability of the standard are key in chemical analysis. Furthermore, if an analyte standard cannot be obtained, quantification cannot be achieved, even if the chemical structures are identified by a qualification method (e.g., high-resolution mass spectrometry). Herein, we describe a universal and analyte standard-free detector for aqueous-eluent-based high-performance liquid chromatography. This universal carbon detector (UCD) was developed based on total organic carbon detection. Separated analytes were oxidized in-line and converted to carbon dioxide (CO 2 ). Generated CO 2 was transferred into the gas phase and collected into ultrapure water, which was followed by conductivity detection. The system can be applied as a HPLC detector that does not use an organic solvent as an eluent. The system can be calibrated with a primary standard of sodium bicarbonate for organic compounds. The universality and quantification were evaluated with organic compounds, including organic acids, sugars, and amino acids. Furthermore, the system was successfully applied to evaluation of the purity of formaldehyde in formalin solution, and determination of sugars in juices. The results show the universal carbon detector has good universality and can quantify many kinds of organic compounds with a single standard such as sodium bicarbonate.

  19. An experimental setup for the simultaneous measurement of thermoelectric power of two samples from 77 K to 500 K.

    PubMed

    Tripathi, T S; Bala, M; Asokan, K

    2014-08-01

    We report on an experimental setup for the simultaneous measurement of the thermoelectric power (TEP) of two samples in the temperature range from 77 K to 500 K using optimum electronic instruments. The setup consists of two rectangular copper bars in a bridge arrangement for sample mounting, two surface mount (SM) chip resistors for creating alternate temperature gradient, and a type E thermocouple in differential geometry for gradient temperature (ΔT) measurement across the samples. In addition, a diode arrangement has been made for the alternate heating of SM resistors using only one DC current source. The measurement accuracy of ΔT increases with the differential thermocouple arrangement. For the calibration of the setup, measurements of TEP on a high purity (99.99%) platinum wire and type K thermocouple wires Chromel and Alumel have been performed from 77 K to 500 K with respect to copper lead wires. Additionally, this setup can be utilized to calibrate an unknown sample against a sample of known absolute TEP.

  20. An experimental setup for the simultaneous measurement of thermoelectric power of two samples from 77 K to 500 K

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

    Tripathi, T. S.; Bala, M.; Asokan, K.

    2014-08-01

    We report on an experimental setup for the simultaneous measurement of the thermoelectric power (TEP) of two samples in the temperature range from 77 K to 500 K using optimum electronic instruments. The setup consists of two rectangular copper bars in a bridge arrangement for sample mounting, two surface mount (SM) chip resistors for creating alternate temperature gradient, and a type E thermocouple in differential geometry for gradient temperature (ΔT) measurement across the samples. In addition, a diode arrangement has been made for the alternate heating of SM resistors using only one DC current source. The measurement accuracy of ΔTmore » increases with the differential thermocouple arrangement. For the calibration of the setup, measurements of TEP on a high purity (99.99%) platinum wire and type K thermocouple wires Chromel and Alumel have been performed from 77 K to 500 K with respect to copper lead wires. Additionally, this setup can be utilized to calibrate an unknown sample against a sample of known absolute TEP.« less

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